CN105139964A - Uniform-performance silver nanowire transparent conductive thin-film preparation method by means of dynamic infrared heating - Google Patents
Uniform-performance silver nanowire transparent conductive thin-film preparation method by means of dynamic infrared heating Download PDFInfo
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- CN105139964A CN105139964A CN201510428706.2A CN201510428706A CN105139964A CN 105139964 A CN105139964 A CN 105139964A CN 201510428706 A CN201510428706 A CN 201510428706A CN 105139964 A CN105139964 A CN 105139964A
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Abstract
The invention provides a uniform-performance silver nanowire transparent conductive thin-film preparation method by means of dynamic infrared heating so that uniformity of the optical and electrical properties of the thin-film is ensured to be better than that of ITO and other similar products. A wet film on which silver nanowire dispersion liquid is coated is uniformly heated and dried by adopting a dynamic infrared heating method so that the silver nanowire transparent conductive thin-film with uniform electrical performance and optical performance is obtained. The silver nanowire transparent conductive thin-film of which average square resistance is lower than 35ohm/square, resistance non-uniformity is less than 7% in two-dimensional space and transmittance can be more than 95% can be obtained by utilizing the method.
Description
Technical field
The present invention relates to the preparation field of transparent conductive film, particularly the preparation of nano silver wire transparent conductive film.
Background technology
Nano silver wire transparent conductive film is because of its good optical transmission and excellent electric conductivity and have benefited from the flexible bent characteristic of nano silver wire, in photoelectric device is as touch-screen, organic solar batteries, display particularly flexible electronic device of new generation, have important application prospect.The uniformity of film is the problem that various transparent conductive film must solve in the application, is directly connected to the yield of product.The method of silver coating nano wire transparent conductive film has a lot, such as drop-coating, vacuum filtration method, spraying process, spin-coating method and knife coating etc.It is poor that the dispersion liquid that spraying coating process sprays due to nozzle can produce at substrate the uniformity of film that uneven distribution causes it to prepare; And spin coating proceeding utilizes to rotate the centrifugal action produced and come dispersing nanowires and then film forming, this just causes the orientation of nano silver wire to have certain directivity and the dispersion of nano silver wire has certain selectivity, so the uniformity of film is poor.From the simplification of equipment, we have selected the method for blade coating to prepare nano silver wire transparent conductive film, and this method is simple, the more important thing is can prepare large-area transparent conductive film, be conducive to business large-scale production preparation; But there is a lot of influencing factor can cause the inhomogeneities of film in doctor blade process, the deployment conditions of the uniformity such as heated and nano silver wire dispersion liquid and the thickness of wet film etc.
The report adopting Dynamic IR heating means to prepare unevenness to be less than the nano silver wire transparent conductive film of 10% performance index is there is no in document and patent.
Summary of the invention
The invention provides a kind of preparation method of simple and easy to do nano silver wire transparent conductive film, ensure that the uniformity of Film Optics and electrology characteristic is better than the like products such as ITO.The present invention adopts the method for Dynamic IR heating to carry out homogeneous heating oven dry to the wet film being coated with nano silver wire dispersion liquid, obtains electric property and the homogeneous nano silver wire transparent conductive film of optical property.Utilize the method can obtain average square resistance lower than 35 Ω/, resistance in two-dimensional space unevenness lower than 7%, transmitance can reach more than 95% nano silver wire transparent conductive film.The uniformity of nano silver wire transparent conductive film performance prepared by the method has exceeded commercial tin indium oxide (ITO) film to the requirement of this index.
The technical solution used in the present invention is as follows:
Utilize Dynamic IR to heat the method for the homogeneous nano silver wire transparent conductive film of processability, it is characterized in that, comprise the following steps:
(1) precursor liquid is prepared
A, required dispersant is dissolved in the mixed solution of deionized water and alcohols solvent, the volume ratio of deionized water and alcohols solvent is (0 ~ 5): 1, the concentration of dispersant can control between 0.01wt%-0.2wt%, then leave standstill 12 ~ 24h after stirring 8 ~ 15h again and obtain the mixed solvent being dissolved with dispersant, stand-by;
B, nano silver wire is scattered in prepared by step (a) be dissolved with in the mixed solvent of dispersant, be made into the dispersion liquid that nano silver wire solid content is 0.1-0.3mg/ml, namely obtain coating precursor liquid;
(2) apply
By the precursor liquid drop of preparation on transparent substrates surface, the height utilizing the siphonage of the coated tools such as glass bar and dispersion liquid to control coated tool distance film is 0.05-0.07mm; Then blade coating is carried out, according to first laterally longitudinal again order blade coating precursor liquid (right-angled intersection coating), repeat 2-4 time, precursor liquid is made evenly to be coated in transparent substrates surface, uniformity of film index: the square resistance unevenness of nano silver wire transparent conductive film is lower than 10%, and transmitance unevenness is lower than 1%;
(3) heat drying film
After each blade coating, adopt the method heat drying film of infrared lamp dynamic heat, 1-6 power is adopted to be the arrangement of 200W-1500W lamp tube array, the speed of substrate with 0.5cm/s-5cm/s under infrared lamp irradiation being coated with nano silver wire precursor liquid is at the uniform velocity passed through irradiation zone, come and go twice, nano silver wire transparent conductive film can be obtained.
The described method utilizing Dynamic IR to heat the homogeneous nano silver wire transparent conductive film of processability, is characterized in that: described dispersant is selected from hydroxypropyl methylcellulose (HPMC), polyvinylpyrrolidone (PVP), Hydroxypropyl ethyl cellulose, lauryl sodium sulfate, Macrogol Ester etc. at interior one or more; Described alcohols solvent be selected from ethanol, normal propyl alcohol, isopropyl alcohol, ethylene glycol, glycerol one or more.
The described Dynamic IR that utilizes heats the method for the homogeneous nano silver wire transparent conductive film of processability, it is characterized in that: the length of the nano silver wire described in step (1) is 75 μm, diameter is 40nm.
The described Dynamic IR that utilizes heats the method for the homogeneous nano silver wire transparent conductive film of processability, it is characterized in that: in the dispersion liquid described in step (1), the mass fraction of dispersant is 0.05%-0.2%.
the present invention has following characteristics:
The method that the present invention utilizes Dynamic IR to heat, namely fix the position of infrared surface heating source and realize dynamic homogeneous heating with substrate level, at the uniform velocity moving substrate, in precursor liquid, add dispersant disperse nano silver wire and obtain conductivity and transmitance be better than the ito thin film of the same terms and the transparent conductive film of unevenness within 10%, for the large-scale application of nano silver wire transparent conductive film is laid a solid foundation by controlling the thickness of wet film.Concrete advantage:
1, the equal control of transparent substrates temperature can be realized by Dynamic IR heating;
2, in precursor liquid, add dispersant and can disperse nano silver wire well, and the adhesion of silver-colored line film on substrate can be increased;
3, infrared heating effectively can reduce the junction resistance of nano silver wire transparent conductive film;
4, the method can prepare large-area transparent conductive film;
5, the method can prepare electric property and the homogeneous transparent conductive film of optical property;
6, this method is simple, cost is low, can produce in batches.
figure of description
Fig. 1 is that Dynamic IR heating is schemed with static base reservoir temperature profiles versus;
Fig. 2 is the layer resistance cloth point situation of case study on implementation 1;
Fig. 3 is the scanning electron microscope (SEM) photograph of case study on implementation 1;
Fig. 4 is the layer resistance cloth point situation of case study on implementation 2;
Fig. 5 is the scanning electron microscope (SEM) photograph of case study on implementation 2.
Embodiment
Device therefor: infrared heater, glass plate, glass bar, 3M adhesive tape, PET film.
case study on implementation 1:
1, be scattered in by nano silver wire in the solvent containing 75vol% ethanol, 12.5vol% water and 12.5vol% isopropyl alcohol, containing mass fraction in solvent is the HPMC of 0.05%, and preparation nano silver wire concentration is the dispersion liquid of 0.2mg/ml, is mixed;
2, atmospheric pressure is utilized also to be fixed fixing for PET film with 3M adhesive tape on a glass, for the PET film of 10cm*10cm area, get 1ml dispersion liquid in pet sheet face, the height utilizing the siphonage of glass bar and dispersion liquid to control glass bar distance film is 0.06mm at every turn;
3, the dispersion liquid for instillation pet sheet face carries out blade coating, according to the dispersion liquid on first laterally longitudinal again order blade coating PET film surface, repeat 2 times, homogeneous dispersion is made to be coated in PET film surface, after each blade coating, open infrared heater, then allow film with the speed of 0.05m/s by below heater, come and go twice, nano silver wire transparent conductive film can be obtained.
By this programme, we can obtain that square resistance is 35 Ω/, unevenness is 7%, transmitance is the transparent conductive film of 96%.
case study on implementation 2:
1, be scattered in by nano silver wire in the solvent containing 75vol% ethanol, 12.5vol% water and 12.5vol% isopropyl alcohol, containing mass fraction in solvent is the HPMC of 0.05%, and compound concentration is the dispersion liquid of 0.1mg/ml, is mixed;
2, atmospheric pressure is utilized also to be fixed fixing for PET film with 3M adhesive tape on a glass, for the PET film of 10cm*10cm area, get 1ml dispersion liquid in pet sheet face, the height utilizing the siphonage of glass bar and dispersion liquid to control glass bar distance film is 0.06mm at every turn;
3, the dispersion liquid for instillation pet sheet face carries out blade coating, according to the dispersion liquid on first laterally longitudinal again order blade coating PET film surface, repeat 6 times, homogeneous dispersion is made to be coated in PET film surface, after each blade coating, open infrared heater, then allow film with the speed of 0.05m/s by below heater, come and go twice, nano silver wire transparent conductive film can be obtained.
By this programme, we can obtain that square resistance is 21 Ω/, unevenness is 7%, transmitance is the transparent conductive film of 95%.
Claims (4)
1. utilize Dynamic IR to heat the method for the homogeneous nano silver wire transparent conductive film of processability, it is characterized in that, comprise the following steps:
(1) precursor liquid is prepared
A, required dispersant is dissolved in the mixed solution of deionized water and alcohols solvent, the volume ratio of deionized water and alcohols solvent is (0 ~ 5): 1, the concentration of dispersant can control between 0.01wt%-0.2wt%, then leave standstill 12 ~ 24h after stirring 8 ~ 15h again and obtain the mixed solvent being dissolved with dispersant, stand-by;
B, nano silver wire is scattered in prepared by step (a) be dissolved with in the mixed solvent of dispersant, be made into the dispersion liquid that nano silver wire solid content is 0.1-1.2mg/ml, namely obtain coating precursor liquid;
(2) apply
By the precursor liquid drop of preparation on transparent substrates surface, the height utilizing the siphonage of the coated tools such as glass bar and dispersion liquid to control coated tool distance film is 0.05-0.07mm; Then blade coating is carried out, according to first laterally longitudinal again order blade coating precursor liquid (right-angled intersection coating), repeat 2-4 time, precursor liquid is made evenly to be coated in transparent substrates surface, uniformity of film index: the square resistance unevenness of nano silver wire transparent conductive film is lower than 10%, and transmitance unevenness is lower than 1%;
(3) heat drying film
After each blade coating, adopt the method heat drying film of infrared lamp dynamic heat, 1-6 power is adopted to be the arrangement of 200W-1500W lamp tube array, the speed of substrate with 0.5cm/s-5cm/s under infrared lamp irradiation being coated with nano silver wire precursor liquid is at the uniform velocity passed through irradiation zone, come and go twice, nano silver wire transparent conductive film can be obtained.
2. the method utilizing Dynamic IR to heat processability homogeneous nano silver wire transparent conductive film according to claim 1, is characterized in that: described dispersant is selected from hydroxypropyl methylcellulose (HPMC), polyvinylpyrrolidone (PVP), Hydroxypropyl ethyl cellulose, lauryl sodium sulfate, Macrogol Ester etc. at interior one or more; Described alcohols solvent be selected from ethanol, normal propyl alcohol, isopropyl alcohol, ethylene glycol, glycerol one or more.
3. the method utilizing Dynamic IR to heat the homogeneous nano silver wire transparent conductive film of processability according to claim 1, is characterized in that: the length of the nano silver wire described in step (1) is 75 μm, diameter is 40nm.
4. the method utilizing Dynamic IR to heat the homogeneous nano silver wire transparent conductive film of processability according to claim 1, is characterized in that: in the dispersion liquid described in step (1), the mass fraction of dispersant is 0.05%-0.2%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112008181A (en) * | 2019-05-31 | 2020-12-01 | 天津大学 | Process for welding silver nanowires |
| CN116410627A (en) * | 2023-04-04 | 2023-07-11 | 北京航空航天大学 | Preparation method of transparent conductive coating based on evaporation self-driving and transparent conductive coating |
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| US20040036993A1 (en) * | 2002-05-17 | 2004-02-26 | Tin Hla Ngwe | Transparent heat mirror for solar and heat gain and methods of making |
| CN102324462A (en) * | 2006-10-12 | 2012-01-18 | 凯博瑞奥斯技术公司 | Transparent conductor and application thereof based on nano wire |
| CN104021840A (en) * | 2014-06-18 | 2014-09-03 | 中南大学 | Low-temperature curing high-conductive silver paste, preparation method of low-temperature curing high-conductive silver paste, conductive film and preparation method of conductive film |
| CN104347191A (en) * | 2014-02-28 | 2015-02-11 | 深圳市骏达光电股份有限公司 | Transparent conducting film shrinking method |
| CN104952551A (en) * | 2015-06-16 | 2015-09-30 | 北京石油化工学院 | Method and equipment for preparing flexible substrate silver nanowire transparent conducting thin film |
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- 2015-07-17 CN CN201510428706.2A patent/CN105139964A/en active Pending
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| US20040036993A1 (en) * | 2002-05-17 | 2004-02-26 | Tin Hla Ngwe | Transparent heat mirror for solar and heat gain and methods of making |
| CN102324462A (en) * | 2006-10-12 | 2012-01-18 | 凯博瑞奥斯技术公司 | Transparent conductor and application thereof based on nano wire |
| CN104347191A (en) * | 2014-02-28 | 2015-02-11 | 深圳市骏达光电股份有限公司 | Transparent conducting film shrinking method |
| CN104021840A (en) * | 2014-06-18 | 2014-09-03 | 中南大学 | Low-temperature curing high-conductive silver paste, preparation method of low-temperature curing high-conductive silver paste, conductive film and preparation method of conductive film |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112008181A (en) * | 2019-05-31 | 2020-12-01 | 天津大学 | Process for welding silver nanowires |
| CN116410627A (en) * | 2023-04-04 | 2023-07-11 | 北京航空航天大学 | Preparation method of transparent conductive coating based on evaporation self-driving and transparent conductive coating |
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