CN104934137A - Method for preparing transparent conductive film based on nano-silver welding - Google Patents
Method for preparing transparent conductive film based on nano-silver welding Download PDFInfo
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- CN104934137A CN104934137A CN201510210263.XA CN201510210263A CN104934137A CN 104934137 A CN104934137 A CN 104934137A CN 201510210263 A CN201510210263 A CN 201510210263A CN 104934137 A CN104934137 A CN 104934137A
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Abstract
The invention discloses a method for preparing a transparent conductive film based on nano-silver welding When a nanometer granular conducting material is used to prepare the transparent conductive film, the nanometer conductive material generates great contact resistance when particles make contact in the conductive process. Silver carboxylate is heated to generate Nano-silver particles, the nano-silver particle generating process includes decomposition of silver carboxylate and dissolution of nano-silver, and thus, part of the nanometer conductive material is welded. The nano-silver particles generated by decomposition of the silver carboxylate are used to realize welding of the nanometer conductive material, welding enables that contact between the nanometer conductive materials to be ohmic contact, contact resistance is effectively eliminated, and the conductive film has high conductivity.
Description
Technical field
The invention belongs to electric conducting material field, be specifically related to a kind of method preparing transparent conductive film based on Nano Silver welding.
Background technology
In recent years, electronic product development is maked rapid progress, to touch-screen, solar cell etc. rapidly universal the and demand of speed constantly increase, for transparent conductive film provides huge opportunity and development space.Current ITO is widely used in opto-electronic device as transparent conductive film, but differs from the features such as frangible because ITO is flexible, is restricted when preparing transparent conductive membrane material.A lot of research in recent years shows that utilizing nano-carbon material and nano metal material on transparent base, prepare transparent conductive film has prospect well.
The electric conducting material such as nano silver wire and carbon nanomaterial has the excellent conductivity of silver, due to the dimensional effect of Nano grade, has excellent light transmission, flexible resistance.Nano-silver thread (AgNW) transparent conductive film has the bending of best conductivity, preferably transmitance and excellence because of it, and existing large quantifier elimination is applied to the electronic product such as thin-film solar cells and touch-screen.
Sukang Bae, HyeongkeunKim etc. (Nature Nanotechnology, 5 (2010), 574) report and utilize Graphene on transparent base, to prepare flexible transparent conductive film by roll-to-roll.30 inch clear conductive films have been prepared by the method, sheet resistance 125 Ω/ light transmittance 97.4% in article.
Hyeon-Gyun Im etc. (Nanoscale, 6 (2013), 711) report and by spraying method, Nano Silver have been prepared high stability transparent conductive film on transparent base, sheet resistance 22 Ω/ light transmittance 85%.
Carbon nano-tube, Graphene, nano-silver thread etc. show excellent performance preparing in flexible transparent conductive film.But these materials contact resistance when preparing transparent conductive material becomes the key factor affecting electric conductivity.
Summary of the invention
For solving the shortcoming and defect part of prior art, the object of the present invention is to provide a kind of method preparing transparent conductive film based on Nano Silver welding.
For achieving the above object, the present invention adopts following technical scheme:
Prepare a method for transparent conductive film based on Nano Silver welding, comprise following steps:
(1) preparation of silver carboxylate micella: by the organic acid of the carboxyl moles such as a certain amount of sodium hydroxide solution joins with methyl alcohol or organic acid in the solution of ethanol, at room temperature stir 30 ~ 60min and obtain reaction solution; Liquor argenti nitratis ophthalmicus is joined in reaction solution the flocculent deposit generating white silver carboxylate, cross leaching precipitation, washing, vacuumize, can obtain pure silver carboxylate; Obtained silver carboxylate is dissolved in organic solvent, obtained silver carboxylate micella; NaOH wherein in sodium hydroxide solution is identical with the silver nitrate mole in liquor argenti nitratis ophthalmicus;
(2) nano-Ag particles welding nanometer conductive material prepare transparent conductive film: by nanometer conductive material in a solvent ultrasonic disperse obtain certain density nanometer conductive material dispersion liquid; Ultrasonic disperse after silver carboxylate micella step (1) prepared mixes with nanometer conductive material dispersion liquid, then carries out film on transparent base, and 150 ~ 200 DEG C of annealing in process after dry, can obtain described transparent conductive film.
At least one in the preferred n-caproic acid of organic acid described in step (1), neodecanoic acid, 12 carbon carboxylic acids, 14 carbon carboxylic acids, 16 carbon carboxylic acids and 18 carbon carboxylic acids etc.
Organic solvent described in step (1) can be one or more in toluene, dimethylbenzene, ethanol, methyl alcohol, isopropyl alcohol etc.
Washing described in step (1) refers to uses distilled water and methyl alcohol or ethanol to wash in turn, removes impurity.
Solvent described in step (2) is preferably at least one in paraxylene, toluene, oxolane, carrene, chloroform, isopropyl alcohol, propyl alcohol, dimethyl sulfoxide (DMSO) and 1-METHYLPYRROLIDONE.
Nanometer conductive material described in step (2) is preferably at least one in carbon nano-tube, Graphene, nano-silver thread and carbon nano-fiber etc.
In nanometer conductive material dispersion liquid described in step (2), the concentration of nanometer conductive material is 0.1 ~ 10mg/mL.
The condition of the ultrasonic disperse described in step (2) is that 50 ~ 250W disperses 1 ~ 60min.
One in the preferred PET of transparent base (PETG), glass or dimethyl silicone polymer etc. described in step (2).
Coating method described in step (2) is spraying process, spin-coating method, suction filtration membrane formation process or scrape embrane method etc.
This produces nano-Ag particles by the heating of Nano Silver micella and realizes the preparation that welding nanometer conductive material elimination contact resistance realizes highly conductive, transparent conductive film.
Experimental principle of the present invention is:
Nanoparticle conductive material (such as carbon nano-tube, Graphene, nano-silver thread etc.) when preparing transparent conductive film, due to this kind of nanometer conductive material realize conducting process particle contact time can produce very large contact resistance.The present invention utilizes silver carboxylate micella to heat and produces nano-Ag particles, and producing in nano-Ag particles process is that a silver carboxylate decomposes and therefore can realize the welding to part nanometer conductive material with the melting process of Nano Silver.The present invention utilizes silver carboxylate to decompose the nano-Ag particles produced and realizes the welding of nanometer conductive material, and this welding makes the contact between nanometer conductive material be that thus ohmic contact well eliminates contact resistance and make conductive film have good conductivity.Because this welding can not realize when all nano-Ag particles contact, therefore want further annealing in process, annealing in process also can make the further melting of nano-Ag particles, and continued operation is carried out on the basis that annealing in process only need be decomposed at silver carboxylate.
The present invention has following advantage and effect relative to prior art:
At present both at home and abroad obtained transparent conductive film major part or based on ITO electro-conductive glass, the maximum shortcoming of ITO can not bend and frangible exactly, and the price comparison of ITO transparent conducting glass is expensive in addition; Also have portioned product to be with transparent conductive films such as nano-silver thread, nano-Ag particles (or other nano metal material), carbon nanomaterials at present, but the transparency and conductivity aspect are difficult to carry out coordinating to make both to reach very desirable state.The present invention obtains nano-Ag particles process implementation welding nanometer conductive material by silver carboxylate micella and prepares the method for transparent conductive film.Have following characteristics: silver carboxylate decomposes the nano-Ag particles produced and realizes the welding of nanometer conductive material, this welding makes the contact between nanometer conductive material be that thus ohmic contact well eliminates contact resistance and make conductive film have good conductivity.
Accompanying drawing explanation
Fig. 1 is Nano Silver welding process schematic diagram in embodiment 1.
Fig. 2 is embodiment 1 nano silver wire scanning electron microscope (SEM) photograph used.
Fig. 3 is the image (multiplication factor is 400 times) of the transparent conductive film that under microscope, embodiment 1 is obtained.
Embodiment
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention are not limited thereto.
Embodiment 1
Prepare a method for transparent conductive film based on Nano Silver welding, comprise following steps:
(1) by NaOH (0.50g, 0.0125mo1) be dissolved in 10mL distilled water, then joining in the solution of n-caproic acid (1.45g, 0.0125mo1) and methyl alcohol (10mL) and at room temperature stir 30 minutes slowly; 10.6mL liquor argenti nitratis ophthalmicus (0.20g/mL) is joined in above-mentioned solution the flocculent deposit generating white, the precipitation obtained after filtration, by distilled water and methanol wash 6 times, remove unreacted reactant, then drying can obtain n-caproic acid silver in a vacuum;
N-caproic acid silver obtained for 0.5g is dissolved in 10mL oxolane, obtained silver carboxylate micella;
(2) nano-silver thread is added ultrasonic disperse 1min in 10mL propyl alcohol, in dispersion liquid, nano-silver thread concentration is 1mg/mL; Silver carboxylate micella prepared by 0.5mL step (1) is mixed ultrasonic 1min with nano-silver thread dispersion liquid, then spin-coating film on clear glass matrix, rotating speed 500r/min, heats 100min by the film made at 150 ~ 200 DEG C, can obtain transparent conductive film.The performance test results of obtained transparent conductive film is as shown in table 1.
Fig. 1 is for embodiment 1, Nano Silver welding process schematic diagram.
Fig. 2 is embodiment 1 nano silver wire scanning electron microscope (SEM) photograph used.
Fig. 3 is the image (multiplication factor is 400 times) of embodiment 1 transparent conductive film under microscope.
Embodiment 2
Prepare a method for transparent conductive film based on Nano Silver welding, comprise following steps:
(1) NaOH (1.0g, 0.025mo1) is dissolved in 10mL distilled water, then joining in the solution of neodecanoic acid (4.3g, 0.025mo1) and methyl alcohol (10mL) and at room temperature stir 30 minutes slowly; 21.2mL liquor argenti nitratis ophthalmicus (0.20g/mL) is joined in above-mentioned solution the flocculent deposit generating white, the precipitation obtained after filtration, by distilled water and methanol wash 6 times, remove unreacted reactant, then drying can obtain neodecanoic acid silver in a vacuum;
Obtained neodecanoic acid silver 0.5g is dissolved in 10mL toluene, silver carboxylate micella can be obtained;
(2) carbon nano-tube is added ultrasonic disperse 1h in 20mL toluene, in dispersion liquid, carbon nanotube concentration is 0.5mg/mL; Silver carboxylate micella prepared by 0.5mL step (1) is mixed ultrasonic 1min with carbon nano tube dispersion liquid, then on transparent PET matrix, film forming is sprayed, spray speed is 1mL/30min, the film made is heated 100min at 150 ~ 200 DEG C, can obtain transparent conductive film.The performance test results of obtained transparent conductive film is as shown in table 1.
Embodiment 3
Prepare a method for transparent conductive film based on Nano Silver welding, comprise following steps:
(1) by NaOH (0.50g, 0.0125mo1) be dissolved in 10mL distilled water, then joining in the solution of 14 carbon carboxylic acids (2.85g, 0.0125mo1) and methyl alcohol (10mL) and at room temperature stir 30 minutes slowly; 10.6mL liquor argenti nitratis ophthalmicus (0.20g/mL) is joined in above-mentioned solution the flocculent deposit generating white, the precipitation obtained after filtration, by distilled water and methanol wash 6 times, remove unreacted reactant, then drying can obtain tetradecanoic acid silver in a vacuum;
Obtained tetradecanoic acid silver 0.5g is dissolved in 10mL 1-METHYLPYRROLIDONE, silver carboxylate micella can be obtained;
(2) Graphene is added ultrasonic disperse 30min in 10mLN-methyl pyrrolidone, in dispersion liquid, Graphene concentration is 0.5mg/mL; Silver carboxylate micellar solution prepared by 0.5mL step (1) is mixed ultrasonic 1min with graphene dispersing solution, then on clear glass matrix, uses blade applicator blade coating film forming, wet-film thickness 15 μm; At 150 ~ 200 DEG C, heat 90min by after the film drying of making, can transparent conductive film be obtained.The performance test results of obtained transparent conductive film is as shown in table 1.
Embodiment 4
Prepare a method for transparent conductive film based on Nano Silver welding, comprise following steps:
(1) by NaOH (2.0g, 0.05mo1) be dissolved in 10mL distilled water, then joining in the solution of 18 carbon carboxylic acids (14.2g, 0.05mo1) and methyl alcohol (10mL) and at room temperature stir 30 minutes slowly; 10.6mL liquor argenti nitratis ophthalmicus (0.80g/mL) is joined in above-mentioned solution the flocculent deposit generating white, the precipitation obtained after filtration, wash 6 times with distilled water and ethanol, remove unreacted reactant, then drying can obtain octadecanoid acid silver in a vacuum;
Obtained octadecanoid acid 0.5g is dissolved in 10mL oxolane, silver carboxylate micella can be obtained;
(2) nano-silver thread is added ultrasonic disperse 1min in 10mL isopropyl alcohol, in dispersion liquid, nano-silver thread concentration is 1mg/mL; Silver carboxylate micellar solution prepared by 1mL step (1) is mixed ultrasonic 1min with nano-silver thread dispersion liquid, then on clear glass matrix, film forming is sprayed, spray speed is 1mL/40min, the film made is heated 100min at 150 ~ 200 DEG C, can obtain transparent conductive film.The performance test results of obtained transparent conductive film is as shown in table 1.
Embodiment 5
Prepare a method for transparent conductive film based on Nano Silver welding, comprise following steps:
(1) silver carboxylate micella is prepared according to the method for the step (1) in embodiment 1;
(2) Graphene is added ultrasonic disperse 30min in 10mL 1-METHYLPYRROLIDONE, in dispersion liquid, Graphene concentration is 1mg/mL; Silver carboxylate micellar solution 0.5mL prepared by step (1) is mixed ultrasonic 10min with graphene dispersing solution, then spin-coating film on clear glass matrix, rotating speed 1500r/min, heats 90min by the film made at 150 ~ 200 DEG C, can obtain transparent conductive film.The performance test results of obtained transparent conductive film is as shown in table 1.
Embodiment 6
Prepare a method for transparent conductive film based on Nano Silver welding, comprise following steps:
(1) silver carboxylate micella is prepared according to the method for the step (1) in embodiment 2;
(2) nano-silver thread is added ultrasonic disperse 1min in 10mL isopropyl alcohol, in dispersion liquid, nano-silver thread concentration is 1mg/mL; Silver carboxylate micellar solution 0.5mL prepared by step (1) is mixed ultrasonic 1min with nano-silver thread dispersion liquid, then on clear glass matrix, film forming is sprayed, spray fast 1mL/30min, the film made is heated 100min at 150 ~ 200 DEG C, can transparent conductive film be obtained.The performance test results of obtained transparent conductive film is as shown in table 1.
The performance test of the transparent conductive film that table 1 embodiment 1 ~ 6 is obtained
In table 1, light transmittance is tested: taking matrix as contrast, is the light transmittance of 550 ~ 650nm place conductive film at wavelength.
The present invention adds solubility carboxyl silver in the dispersion liquids such as carbon nano-tube, Graphene, nano-silver thread, and carboxyl silver can be assembled into nanometer ping-pong ball in the solution, these nanometer ping-pong balls can become discharge nano-Ag particles when heating, low can being easy to of the nano-Ag particles fusing point discharged is welded electric conducting materials such as carbon nano-tube, Graphene, nano-silver threads, and these welding well improve conductivity.
Above-described embodiment is the present invention's preferably execution mode; but embodiments of the present invention are not restricted to the described embodiments; change, the modification done under other any does not deviate from Spirit Essence of the present invention and principle, substitute, combine, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (10)
1. prepare a method for transparent conductive film based on Nano Silver welding, it is characterized in that, comprise following steps:
(1) by the organic acid of the carboxyl moles such as a certain amount of sodium hydroxide solution joins with methyl alcohol or organic acid in the mixed solution of ethanol, at room temperature stir 30 ~ 60min and obtain reaction solution; Liquor argenti nitratis ophthalmicus is joined in reaction solution the flocculent deposit generating white silver carboxylate, cross leaching precipitation, washing, vacuumize, can obtain pure silver carboxylate; Obtained silver carboxylate is dissolved in organic solvent, obtained silver carboxylate micella; NaOH wherein in sodium hydroxide solution is identical with the silver nitrate mole in liquor argenti nitratis ophthalmicus;
(2) by nanometer conductive material in a solvent ultrasonic disperse obtain certain density nanometer conductive material dispersion liquid; Ultrasonic disperse after silver carboxylate micella step (1) prepared mixes with nanometer conductive material dispersion liquid, then carries out film on transparent base, and 150 ~ 200 DEG C of annealing in process after dry, namely obtain described transparent conductive film.
2. a kind of method preparing transparent conductive film based on Nano Silver welding according to claim 1, it is characterized in that, the organic acid described in step (1) is at least one in n-caproic acid, neodecanoic acid, 12 carbon carboxylic acids, 14 carbon carboxylic acids, 16 carbon carboxylic acids and 18 carbon carboxylic acids.
3. a kind of method preparing transparent conductive film based on Nano Silver welding according to claim 1, it is characterized in that, the organic solvent described in step (1) is at least one in toluene, dimethylbenzene, ethanol, methyl alcohol and isopropyl alcohol.
4. a kind of method preparing transparent conductive film based on Nano Silver welding according to claim 1, is characterized in that, the washing described in step (1) refers to uses distilled water and methyl alcohol or ethanol to wash in turn.
5. a kind of method preparing transparent conductive film based on Nano Silver welding according to claim 1, it is characterized in that, the solvent described in step (2) is at least one in paraxylene, toluene, oxolane, carrene, chloroform, isopropyl alcohol, propyl alcohol, dimethyl sulfoxide (DMSO) and 1-METHYLPYRROLIDONE.
6. a kind of method preparing transparent conductive film based on Nano Silver welding according to claim 1, it is characterized in that, the nanometer conductive material described in step (2) is at least one in carbon nano-tube, Graphene, nano-silver thread and carbon nano-fiber.
7. a kind of method preparing transparent conductive film based on Nano Silver welding according to claim 1, it is characterized in that, in the nanometer conductive material dispersion liquid described in step (2), the concentration of nanometer conductive material is 0.1 ~ 10mg/mL.
8. a kind of method preparing transparent conductive film based on Nano Silver welding according to claim 1, is characterized in that, the condition of the ultrasonic disperse described in step (2) is that 50 ~ 250W disperses 1 ~ 60min.
9. a kind of method preparing transparent conductive film based on Nano Silver welding according to claim 1, it is characterized in that, the transparent base described in step (2) is the one in PET, glass or dimethyl silicone polymer.
10. according to claim 1ly a kind ofly prepare the method for transparent conductive film based on Nano Silver welding, it is characterized in that, the coating method described in step (2) is spraying process, spin-coating method, suction filtration membrane formation process or scrape embrane method.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105702381A (en) * | 2016-01-11 | 2016-06-22 | 合肥微晶材料科技有限公司 | Packaging and manufacturing method of highly stable silver nano-wire composite film |
| CN107602898A (en) * | 2017-10-10 | 2018-01-19 | 深圳大学 | A kind of antibiotic plastic and preparation method |
| CN108406169A (en) * | 2018-02-02 | 2018-08-17 | 北京交通大学 | A kind of welding point and welding method of the low resistance yttrium system high-temperature superconducting body based on nanometer silver solder |
| CN108733243A (en) * | 2017-04-17 | 2018-11-02 | 蓝思科技（长沙）有限公司 | A kind of production method of the touch screen based on nano silver film |
| CN112837847A (en) * | 2019-11-22 | 2021-05-25 | 重庆神华薄膜太阳能科技有限公司 | Preparation method and application of conductive film |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105702381A (en) * | 2016-01-11 | 2016-06-22 | 合肥微晶材料科技有限公司 | Packaging and manufacturing method of highly stable silver nano-wire composite film |
| CN108733243A (en) * | 2017-04-17 | 2018-11-02 | 蓝思科技（长沙）有限公司 | A kind of production method of the touch screen based on nano silver film |
| CN108733243B (en) * | 2017-04-17 | 2021-11-02 | 蓝思科技（长沙）有限公司 | Method for manufacturing touch screen based on nano silver film |
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| CN108406169A (en) * | 2018-02-02 | 2018-08-17 | 北京交通大学 | A kind of welding point and welding method of the low resistance yttrium system high-temperature superconducting body based on nanometer silver solder |
| CN112837847A (en) * | 2019-11-22 | 2021-05-25 | 重庆神华薄膜太阳能科技有限公司 | Preparation method and application of conductive film |
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Application publication date: 20150923 |