CN104575869A - Patterning etching method of transparent conducting electrode and patterning transparent conducting electrode - Google Patents
Patterning etching method of transparent conducting electrode and patterning transparent conducting electrode Download PDFInfo
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- CN104575869A CN104575869A CN201510013392.XA CN201510013392A CN104575869A CN 104575869 A CN104575869 A CN 104575869A CN 201510013392 A CN201510013392 A CN 201510013392A CN 104575869 A CN104575869 A CN 104575869A
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Abstract
The invention discloses patterning etching method of a transparent conducting electrode and a patterning transparent conducting electrode. The method comprises the steps that an electrode to be patterned is manufactured; a patterning protecting layer is prepared on the electrode; the electrode is placed in etching liquid or gas for etching; and the electrode is placed in washing liquid, and etching products and the protecting layer are washed off. The method is used for carrying out latticed patterning on metal nanowires, and the latticed patterning transparent conducting electrode is manufactured. Metal or a metal nanowire film is subjected to quick, low-cost, safe and low-toxic chemical etching through gas or low-concentration etching liquid, complete etching can be achieved, shadowless etching can be achieved, safety and low-toxic performance are achieved, etching speed is high, and effect is obvious in practical application. A prepared latticed patterning transparent conducting electrode comprehensive nanowire and a nanometer lattice transparent electrode have the advantages that under the premise that conductivity loss is very small, transparency is greatly improved, and performance is good.
Description
Technical field
The invention belongs to transparency conductive electrode field, relate to metal, metal grill or metal nanometer line transparency conductive electrode, particularly relate to a kind of patterning lithographic method and patterned transparent conductive electrode of transparency conductive electrode.
Background technology
At present, the material of transparency electrode mainly comprises ITO (tin indium oxide), carbon nano-tube, Graphene, conducting polymer, metal grill, metal nanometer line etc.Ito transparent electrode relies on its high grade of transparency and high conductivity to occupy the most market share.But ITO electrode needs the method preparation using vacuum vapor deposition, and containing rare element indium, thus cost is higher, and ITO enbrittles, and cannot use in flexible device.Thus people start to find other transparent electrode materials, and metal nanometer line is due to its lower cost, higher performance, gain great popularity to the adaptability of flexible device.Although thicker metal film is opaque, if carried out waffle-like pattern to make it to become metal grill, then can want with metal nanometer line the transparency conductive electrode that matches in excellence or beauty by becoming.
In the practical application in the fields such as liquid crystal display, OLED (organic electroluminescent), touch-screen, solar cell, usually need the transparency conductive electrode of patterning to complete various function.For metal, metal grill and metal nanowire thin-films transparency conductive electrode, prior art has multiple patterns method, comprises non-chemically lithographic method and the chemical etching method based on etching liquids such as acid etching solutions such as laser ablation.Non-chemically lithographic method requires higher to instrument and equipment, and cost is wayward.Existing chemical etching method relative toxicity is higher, and often cannot etch micron, nano level fine structure due to etching liquid and protective layer wettability deficiency.
Summary of the invention
In order to overcome above-mentioned the deficiencies in the prior art, the invention provides a kind of patterning lithographic method of transparency conductive electrode, in turn including the following steps:
Metallic film, metal grill film or metal nanowire thin-films are prepared on transparent substrates by 1.1, make electrode to be patterned;
Prepare the protective layer of patterning on 1.2 electrodes to be patterned described in step 1.1, make electrode to be etched;
Electrode to be etched described in step 1.2 to be placed in solution, the gaseous halogen simple substance of halogen simple substance or to etch containing organic solution that is amino and halogen group by 1.3; The metal that order does not have protected seam to cover or metal nanometer line no longer conduct electricity, and make electrode to be cleaned;
If employ the solution of halogen simple substance or gaseous halogen simple substance etching electrode in 1.4 steps 1.3, then first electrode to be cleaned described in step 1.3 is placed in organic solvent and removes protective layer, then be placed on and remove etch product containing in amino organic solution; If employ the organic solution etches electrode containing amino and halogen group in step 1.3, then only electrode to be cleaned described in step 1.3 is placed in organic solvent and removes protective layer; Finishing patternsization etches, and makes patterned transparent conductive electrode.
In the patterning lithographic method of above-mentioned preparation transparency conductive electrode, metallic film described in step 1.1 is a kind of or wherein several laminated film in silver, copper and mickel; Described metal grill film is a kind of or wherein several composite gridding film in silver-colored grid, copper mesh and nickel screen lattice; Described metal nanowire thin-films is a kind of or wherein several composite nano-line film in nano silver wire, copper nano-wire and nickel nano wire; Described transparent substrates is glass or transparent plastic.
In the patterning lithographic method of above-mentioned preparation transparency conductive electrode, when using solution or the gaseous halogen simple substance etching of halogen simple substance in step 1.3, the part that is etched after patterning completes disappears completely, is thorough patterning; When using the organic solution etches containing amino and halogen group, though patterning is etched after completing, part is no longer conducted electricity, and macro morphology is constant, is without shadow patterning.
As one embodiment of the present invention, the metallic film in step 1.1, metal grill film or metal nanowire thin-films are prepared on transparent substrates by ways such as spin coating, spraying, printing, self assembly, vapour deposition, liquid deposition or plating.
As one embodiment of the present invention, step 1.2 prepares the protective layer of patterning especially by methods such as photoetching development, silk screen printing or seal transfer printings on electrode to be patterned, makes electrode to be etched; Wherein photoetching development method in turn includes the following steps:
2.1 prepare photoresist on electrode to be patterned, make electrode to be exposed;
The mask plate that on 2.2 electrodes to be exposed described in step 2.1, covering design is good, and carry out uv-exposure, make electrode to be developed;
2.3, by treating described in step 2.2 that development electrode is placed in developer solution and develops, wash away the part being subject to UV-irradiation, make electrode to be etched.
The present invention is directed to patterning lithographic method that metal, metal grill and metal nanometer line prepare transparency conductive electrode both can to have realized being etched the thorough patterning that part disappears completely, the part macro morphology that can also realize being etched substantially constant without shadow patterning, be the fast and patterned transparent conductive electrode preparation method of low cost of a kind of safety and low toxicity, etching speed.
By above-mentioned patterning lithographic method, waffle-like pattern is carried out to conduction monodimension nanometer material, can be made into a kind of patterned transparent conductive electrode.Described conduction monodimension nanometer material, through patterning, forms the fenestral fabric with micron order hole.Described conduction monodimension nanometer material can be metal nanometer line or carbon nano-tube.
As one embodiment of the present invention, the present invention also provides a kind of and carries out waffle-like pattern via above-mentioned patterning lithographic method to metal nanometer line, and be prepared into the method for patterned transparent conductive electrode, its preparation process is:
Metal nanowire thin-films is prepared on transparent substrates by 3.1, makes electrode to be patterned;
Prepare the protective layer of micron order waffle-like pattern on 3.2 electrodes to be patterned described in step 3.1, make electrode to be etched;
Electrode to be etched described in step 3.2 to be placed in the solution of halogen simple substance or gaseous halogen simple substance etches by 3.3; The metal nanometer line that order does not have protected seam to cover and halogen simple substance react, and make electrode to be cleaned;
Electrode to be cleaned described in step 3.3 is placed in organic solvent by 3.4 removes protective layer, then is placed on and removes etch product containing in amino organic solution, completes waffle-like patternization and thoroughly etches, make the transparency conductive electrode of waffle-like pattern.
Compared with prior art, the invention has the beneficial effects as follows:
The patterning lithographic method of transparency conductive electrode provided by the invention to be realized metal or metal nanowire thin-films fast by the etching liquid of gas or low concentration, low cost and the chemical etching of safety and low toxicity, and both can realize the thorough etching removing virgin metal or metal nanowire thin-films after etching completely, and also can realize etching rear virgin metal or substantially constant the etching without shadow of metal nanowire thin-films macro morphology.Compared with the conventional method, there is the advantages such as with low cost, safety and low toxicity, etching speed are fast, Be very effective in actual applications.
The invention provides a kind of novel transparent conductive electrode, be made up of the conduction monodimension nanometer material of waffle-like pattern.By by one-dimensional metal nano wire transparency electrode waffle-like pattern, under the prerequisite of substantially not losing macroscopical conductivity, significantly improve electrode transparency.In addition, compared with conventional metals grid electrode, there is not periodically complete lighttight region in novel transparent electrode of the present invention, inhibits the possibility occurring Moire fringe during application of electrode.Novel transparent conductive electrode provided by the invention combines the advantage of metal nanometer line and nanometer grid transparency electrode, functional.
Accompanying drawing explanation
Fig. 1 is patterning lithographic method flow chart provided by the invention.
Fig. 2 is the optical microscope photograph of embodiment one when using the nano silver wire sample of thorough lithographic method patterning also not wash away etch product, and wherein, " PKU " printed words inside is nano silver wire, and printed words outside is etch product.
Fig. 3 is scanning electron microscopy (SEM) photo of nano silver wire and gaseous iodine product (i.e. etch product) in embodiment one.
Fig. 4 is the optical microscope photograph using the nano silver wire sample of thorough lithographic method patterning final in embodiment one, and wherein, " PKU " printed words inside is nano silver wire, and printed words are outside without nano silver wire.
Fig. 5 is scanning electron microscopy (SEM) photo used in embodiment two without the not protected part of nano silver wire sample of shadow lithographic method patterning.
Fig. 6 is scanning electron microscopy (SEM) photo of waffle-like pattern nano silver wire transparency electrode prepared by embodiment three.
Embodiment
Below in conjunction with accompanying drawing, further describe the present invention by embodiment, but the scope do not limited the present invention in any way.
Embodiment one:
First, the aqueous dispersions of blade coating nano silver wire in substrate of glass, makes nano silver wire film, as electrode to be patterned.Then prepare business photoresist film by method of spin coating thereon, and dry process after carrying out the even glue of 100 DEG C, continue 1.5 minutes, make electrode to be exposed.After cooling, the mask plate of " PKU " shape pattern is covered thereon, carry out uv-exposure, continue 2min, make electrode to be developed.Immersed after completing in the NaOH aqueous solution of 1% and develop 10 seconds, and rinse with clear water, nitrogen dries up, and makes electrode to be etched.Inserted after drying up in iodine cylinder and seal, make itself and gaseous iodine react 1 minute, after taking-up, it is washed away photoresist in acetone, and rinse with clear water, nitrogen dries up.Fig. 2 is optical microscope photograph when using the nano silver wire sample of thorough lithographic method patterning also not wash away etch product; " PKU " printed words inside is nano silver wire; printed words outside is etch product; in nano silver wire sample now, not protected part completely and Iod R; thus no longer conduct electricity, be illustrated in figure 3 scanning electron microscopy (SEM) photo of nano silver wire and gaseous iodine product (i.e. etch product).To be immersed in the amine terminated polyether aqueous isopropanol of 20% 30 seconds again to remove etch product, and rinse with clear water, nitrogen dries up.Wash away etch product and protective layer completely; finally obtain the nano silver wire sample with thorough lithographic method patterning; Fig. 4 is the optical microscope photograph using the nano silver wire sample of thorough lithographic method patterning final, and " PKU " printed words inside is nano silver wire, and printed words are outside without nano silver wire.
In above process, only need be replaced by the mask plate of designed shape, just can obtain the patterned electrodes of corresponding pattern.
Embodiment two:
First, in substrate of glass, the isopropyl alcohol dispersion liquid of spin coating nano silver wire, makes nano silver wire film, as electrode to be patterned.Then prepare business photoresist film by method of spin coating thereon, and dry process after carrying out the even glue of 100 DEG C, continue 1.5 minutes, make electrode to be exposed.After cooling, mask plate is covered thereon, carry out uv-exposure, continue 2min, make electrode to be developed.Immersed after completing in the NaOH aqueous solution of 1% and develop 10 seconds, and rinse with clear water, nitrogen dries up, and makes electrode to be etched.After immersed the iodate methylamine (CH of 1.2mg/mL
3nH
3i) etch 5 minutes in aqueous isopropanol, and rinse with clear water, nitrogen dries up.After drying up, it is washed away photoresist in acetone, and rinse with clear water, nitrogen dries up.Finally obtain by the transparency conductive electrode without shadow lithographic method patterning, see Fig. 5, wherein the nano silver wire of visible not protected part has been partly cut thus has no longer conducted electricity, and macro morphology is almost constant.
Embodiment three:
First, in substrate of glass, spray the isopropyl alcohol dispersion liquid of nano silver wire, make nano silver wire film, as electrode to be patterned.Then prepare business photoresist film by method of spin coating thereon, and dry process after carrying out the even glue of 100 DEG C, continue 1.5min, make electrode to be exposed.After cooling, the mask plate of waffle-like pattern is covered thereon, carry out uv-exposure, continue 2min, make electrode to be developed.Immersed after completing in the NaOH aqueous solution of 1% and develop 10 seconds, and rinse with clear water, nitrogen dries up, and makes electrode to be etched.After inserted in iodine cylinder and sealed, make itself and gaseous iodine react 1 minute, after taking-up, it is washed away photoresist in acetone, and rinse with clear water, nitrogen dries up.To be immersed in the amine terminated polyether aqueous isopropanol of 20% 30 seconds again to remove etch product, and rinse with clear water, nitrogen dries up.Wash away etch product and protective layer completely, finally obtain the novel transparent conductive electrode of thorough patterning, Fig. 6 is scanning electron microscopy (SEM) photo of the waffle-like pattern nano silver wire transparency electrode that the present embodiment prepares.
It should be noted that the object publicizing and implementing example is to help to understand the present invention further, but it will be appreciated by those skilled in the art that: in the spirit and scope not departing from the present invention and claims, various substitutions and modifications are all possible.Therefore, the present invention should not be limited to the content disclosed in embodiment, and the scope that the scope of protection of present invention defines with claims is as the criterion.
Claims (10)
1. a patterning lithographic method for transparency conductive electrode, in turn includes the following steps:
Metallic film, metal grill film or metal nanowire thin-films are prepared on transparent substrates by 1.1, make electrode to be patterned;
Prepare the protective layer of patterning on 1.2 electrodes to be patterned described in step 1.1, make electrode to be etched;
Electrode to be etched described in step 1.2 to be placed in solution, the gaseous halogen simple substance of halogen simple substance or to etch containing organic solution that is amino and halogen group by 1.3; The metal that order does not have protected seam to cover or metal nanometer line no longer conduct electricity, and make electrode to be cleaned;
If employ the solution of halogen simple substance or gaseous halogen simple substance etching electrode in 1.4 steps 1.3, then first electrode to be cleaned described in step 1.3 is placed in organic solvent and removes protective layer, then be placed on and remove etch product containing in amino organic solution; If employ the organic solution etches electrode containing amino and halogen group in step 1.3, then only electrode to be cleaned described in step 1.3 is placed in organic solvent and removes protective layer; Finishing patternsization etches, and makes patterned transparent conductive electrode.
2. patterning lithographic method as claimed in claim 1, is characterized in that, metallic film described in step 1.1 is a kind of or wherein several laminated film in silver, copper and mickel.
3. patterning lithographic method as claimed in claim 1, it is characterized in that, metal grill film described in step 1.1 is a kind of or wherein several composite gridding film in silver-colored grid, copper mesh and nickel screen lattice.
4. patterning lithographic method as claimed in claim 1, it is characterized in that, metal nanowire thin-films described in step 1.1 is a kind of or wherein several composite nano-line film in nano silver wire, copper nano-wire and nickel nano wire.
5. patterning lithographic method as claimed in claim 1, it is characterized in that, transparent substrates described in step 1.1 is glass or transparent plastic.
6. patterning lithographic method as claimed in claim 1, it is characterized in that, described in step 1.1, metallic film, metal grill film or metal nanowire thin-films are prepared on transparent substrates particular by spin coating, spraying, printing, self assembly, vapour deposition, liquid deposition or plating way.
7. patterning lithographic method as claimed in claim 1, is characterized in that, makes electrode to be etched particular by photoetching development, silk screen printing or the preparation of seal printing transferring method described in step 1.2 on electrode to be patterned.
8. patterning lithographic method as claimed in claim 1, is characterized in that, the solution or the gaseous halogen simple substance etching that described in step 1.3, electrode to be etched are placed in halogen simple substance are thorough patterning lithographic method; The described organic solution etching be placed in by electrode to be etched containing amino and halogen group is without shadow patterning method.
9. utilize patterning lithographic method described in claim 1 to carry out to conduction monodimension nanometer material a kind of patterned transparent conductive electrode that waffle-like pattern is prepared into.
10. patterned transparent conductive electrode as claimed in claim 9, it is characterized in that, described conduction monodimension nanometer material is metal nanometer line or carbon nano-tube.
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| CN108526486A (en) * | 2018-05-28 | 2018-09-14 | 五邑大学 | A kind of latticed nano wire and preparation method thereof |
| CN110718337A (en) * | 2019-10-24 | 2020-01-21 | 宁波石墨烯创新中心有限公司 | Composite conductive film and patterning method thereof |
| CN111197153A (en) * | 2018-11-16 | 2020-05-26 | 南昌欧菲光科技有限公司 | Preparation method of metal grid and metal grid sheet |
| CN112908520A (en) * | 2018-10-30 | 2021-06-04 | 苏州诺菲纳米科技有限公司 | Etching method of silver nanowire, transparent conductive electrode and preparation method of transparent conductive electrode |
| CN113921192A (en) * | 2021-09-22 | 2022-01-11 | 香港城市大学成都研究院 | Preparation method of high-precision patternable micro-nano silver nanowire transparent electrode |
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