CN104882224A - Preparation of transparent conducting film based on nano-silver wires and caboxylated carbon nano-materials - Google Patents
Preparation of transparent conducting film based on nano-silver wires and caboxylated carbon nano-materials Download PDFInfo
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Abstract
The invention belongs to the technical field of preparation of conducting materials, and specifically discloses preparation of a transparent conducting film based on nano-silver wires and caboxylated carbon nano-materials. The nano-silver wires can be well dispersed in solvents such as water and alcohols, carbon nano-materials are insoluble and difficult to disperse in water or an organic solvent, after being carboxylated, the carbon nano-materials can be well dispersed in the solvents and are used to prepare a mixed solution together with the nano-silver wires, and thus addition of auxiliaries such as dispersing agents, which makes post-treatment complex, can be effectively avoided. Surfaces of the nano-silver wires have electrophilic characteristics, and thus can be coordinated with atoms rich in electrons through coordination. Carboxyl groups in the prepared carbon nano-materials can be combined with the nano-silver wires, thereby enabling the nano-materials to better contact with the nano-silver wires and eliminating contact resistance to the greatest extent. Influences of the nano-silver wires and the carbon nano-mateirals in the aspect of light transmission are different, and mutual complementation can be realized, thereby enabling light transmission and electrical conductivity to be improved.
Description
Technical field
The invention belongs to the preparing technical field of electric conducting material, especially a kind of flexible transparent conductive film technology of preparing, be specifically related to a kind of preparation of the transparent conductive film based on nano-silver thread and carboxylated carbon nanomaterial.
Background technology
Transparent conductive film refer to 80% be greater than to the transmitance of the visible ray of wave-length coverage between 380 to 780nm, resistivity is lower than 10
-3the film of Ω cm.The transparent conductive film of current own extensive use is mainly prepared on the hard backing material such as pottery, glass using ITO as electric conducting material, but because these materials also exist the crisp defect such as frangible, not yielding of matter, therefore limit the application of transparent conductive film to a great extent.In addition, although ITO successfully uses as nesa coating reached for six more than ten years in optoelectronic devices, because its flex capability is very poor, be not suitable as prepare flexible transparent conductive film material completely.
Silver nano material have the unexistent optical property of silver-colored simple substance this make the purposes of silver nano material more extensive in numerous nano materials also attention.Nano silver wire, except having 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 thin-film solar cells.In addition due to the big L/D ratio effect of nano silver wire, make, in its application in conducting resinl, heat-conducting glue etc., also there is outstanding advantage.
Carbon nanomaterial has that electron mobility is at room temperature high, electric conductivity is excellent, transmitance in visible ray and near infrared range is high, the chemical property that excellent heat conductivility is stable, in addition, carbon nanomaterial also has and bends characteristic preferably, and these excellent performances make carbon nanomaterial also have good application preparing in flexible transparent conductive film.
Therefore nano-silver thread and carbon nanomaterial are considered to be the most possible material substituting conventional I TO transparency electrode, provide possibility for realizing flexibility, bent LED display, touch-screen etc.
Summary of the invention
For solving the deficiency of the preparation of existing transparent conductive film complicated and conductivity and light transmission, the present invention proposes a kind of preparation method of the transparent conductive film based on nano-silver thread and carboxylated carbon nanomaterial.
For achieving the above object, the present invention adopts following technical scheme:
Based on a preparation method for the transparent conductive film of nano-silver thread and carboxylated carbon nanomaterial, comprise following steps:
(1) carbon nanomaterial is carboxylated: joined by 1 ~ 10g carbon nanomaterial in the mixed acid containing 15 ~ 100mL 60wt% red fuming nitric acid (RFNA) and 0 ~ 100mL 98wt% concentrated sulfuric acid, after ultrasonic disperse, adding thermal agitation and reacting under counterflow condition; After reaction terminates, suction filtration, with deionized water cyclic washing repeatedly to neutral, namely vacuumize obtain carboxylated carbon nanomaterial;
(2) carboxylated carbon nanomaterial and nano-silver thread are mixed with compound transparent electricity conductive film: get the obtained carboxylated carbon nanomaterial of a certain amount of step (1) and to add in solvent then ultrasonic disperse, leave standstill afterwards or centrifugal removing sediment, add the ethanolic solution of a certain amount of nano-silver thread again, after ultrasonic disperse, obtain the mixed solution of nano-silver thread and carboxylated carbon nanomaterial; The ratio of the solid content of the nano-silver thread wherein in the quality of carboxylated carbon nanomaterial and the ethanolic solution of nano-silver thread is 5 ~ 20:5 ~ 30;
The mixed solution getting a certain amount of nano-silver thread and carboxylated carbon nanomaterial carries out film on transparent base, then carries out annealing in process, obtains described transparent conductive film.
Carbon nanomaterial described in step (1) is preferably at least one in carbon nano-tube, Graphene, carbon nano-fiber, nano carbon microsphere and fullerene etc.
Reaction temperature described in step (1) is 110 ~ 130 DEG C, and the reaction time is 24 ~ 48h.
The condition of the ultrasonic disperse described in step (1) is that 50 ~ 250W disperses 10 ~ 60min.
Solvent described in step (2) is preferably at least one in water, methyl alcohol, ethanol and propyl alcohol etc.
Carboxylated carbon nanomaterial described in step (2) concentration is in a solvent 0.1 ~ 3mg/mL.
Time of repose described in step (2) is 12 ~ 48h; Centrifugal rotational speed described in step (2) is 2000 ~ 8000r/min.
In the ethanolic solution of nano-silver thread described in step (2), the concentration of nano-silver thread is 0.1 ~ 10mg/mL; Diameter 30 ~ the 150nm of described nano-silver thread, length is 4 ~ 50 μm.
The condition that carboxylated carbon nanomaterial described in step (2) adds ultrasonic disperse in solvent is that 50 ~ 250W disperses 10 ~ 60min, and the ultrasonic disperse condition after the ethanolic solution of nano-silver thread that adds is that 50 ~ 100W disperses 10 ~ 60s.
Coating method described in step (2) is spraying process, spin-coating method, suction filtration membrane formation process or scrape embrane method etc.; Annealing temperature described in step (2) is 100 ~ 200 DEG C.
The present invention prepares transparent conductive film by carboxylated carbon nanomaterial and nano-silver thread mixed solution, and bi-material can disperse in the solution well, can mutually supplement in film forming procedure simultaneously.
Experimental principle of the present invention is:
Nano-silver thread can well disperse in water and alcohols equal solvent, and insoluble, the difficult dispersion of carbon nanomaterial in water or organic solvent, therefore after it is carboxylated can well in these solvents dispersion can prepare mixed solution together with nano-silver thread simultaneously, can effectively avoid like this making reprocessing loaded down with trivial details by adding the auxiliary agents such as dispersant.Therefore nano-silver thread surface has close electrical characteristics can carry out coordination by coordination and the atom being rich in electronics.Carboxyl in carbon nanomaterial prepared in the present invention can combine with nano-silver thread thus carbon nanomaterial is better contacted with nano-silver thread eliminates contact resistance as far as possible.In addition nano-silver thread and carbon nanomaterial affect and differently therefore can realize mutually supplementing light transmission and conductivity are promoted all to some extent in printing opacity.
In the present invention, the film after annealing process on transparent base of the mixing dispersion soln of nano-silver thread and carboxylated carbon nanomaterial realizes electrically conducting transparent.
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 vegetation transparent conductive films such as nano-silver thread, nano-Ag particles (or other nano metal material), carbon nanomaterials at present, but conductivity and the transparency are also not bery desirable.The mixed solution that the present invention is based on nano-silver thread and carboxylated carbon nanomaterial prepares transparent conductive film.There is following characteristics: (1) nano-silver thread and carboxylated carbon nanomaterial can disperse well in partial solvent; (2) carbon nanomaterial due to surface carboxyl can better and nano-silver thread combine; (3) effect in light transmission of nano-silver thread and carbon nanomaterial different therefore can mutually supplement make the transparency and conductivity better.
Accompanying drawing explanation
Fig. 1 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 transparent conductive film based on nano-silver thread and carboxylated carbon nanomaterial, comprise following steps:
(1) in the mono-neck round-bottomed flask of the 250mL that magnetic stir bar is housed, add the single armed carbon nano-tube of 3g drying and the mixed acid of 15mL 60wt% red fuming nitric acid (RFNA) and the 45mL 98wt% concentrated sulfuric acid, spherical condensating tube and tail gas absorption pipe is loaded onto with after 150W ultrasonic wave process 30min, be heated to 120 DEG C, stir and reflux down and react 2h; After reaction terminates, with the dilution of 800mL deionized water, with little 0.22 μm of mixed fine miillpore filter suction filtration, with deionized water cyclic washing repeatedly to neutral, 60 DEG C of vacuumize 24h obtain carboxylated carbon nanomaterial;
(2) in the beaker of a 150mL, add the carboxylated carbon nanomaterial of the preparation in 20mg step (1), then 50mL ethanol is added, 150W ultrasonic disperse 10 minutes, leave standstill and remove bottom precipitation after 12 hours, in dispersion liquid, add the ethanolic solution of the 1mg/mL nano-silver thread of 50mL afterwards, then obtain the mixed solution of nano-silver thread and carboxylated carbon nanomaterial at the ultrasonic 30s of 50W;
The mixed solution of nano-silver thread and carboxylated carbon nanomaterial is carried out spin-coating film on transparent base, rotating speed 1500 ~ 3000r/min, heat 20min by the film 120 ~ 200 DEG C made, obtain described transparent conductive film.The performance test results of obtained transparent conductive film is as shown in table 1.
Fig. 1 is the image (multiplication factor is 400 times) of the transparent conductive film that under microscope, embodiment 1 is obtained.
Embodiment 2
Prepare transparent conductive film based on nano-silver thread and carboxylated carbon nanomaterial, comprise following steps:
(1) in the mono-neck round-bottomed flask of the 100mL that magnetic stir bar is housed, add the Graphene of 2g drying and the mixed acid of 10mL 60wt% red fuming nitric acid (RFNA) and the 30mL 98wt% concentrated sulfuric acid, spherical condensating tube and tail gas absorption pipe is loaded onto with after 100W ultrasonic wave process 40min, be heated to 120 DEG C, stir and reflux down and react 4h; After reaction terminates, with the dilution of 400mL deionized water, with little 0.22 μm of mixed fine miillpore filter suction filtration, with deionized water cyclic washing repeatedly to neutral, 60 DEG C of vacuumize 24h obtain carboxylated carbon nanomaterial;
(2) in the beaker of a 150mL, add the carboxylated carbon nanomaterial of the preparation in 10mg step (1), then 50mL ethanol is added, 150W ultrasonic disperse 10 minutes, leave standstill and remove bottom precipitation after 12 hours, in dispersion liquid, add the ethanolic solution of 50mL 5mg/mL nano-silver thread afterwards, then at the ultrasonic 30s of 50W, obtain the mixed solution of nano-silver thread and carboxylated carbon nanomaterial;
With film rod by the mixed solution film on the glass sheet of nano-silver thread and carboxylated carbon nanomaterial, the thickness of solution film is 4 ~ 60 μm, heats 30min, obtain described transparent conductive film after drying by the film 120 ~ 200 DEG C made.The performance test results of obtained transparent conductive film is as shown in table 1.
Embodiment 3
Prepare transparent conductive film based on nano-silver thread and carboxylated carbon nanomaterial, comprise following steps:
(1) in the mono-neck round-bottomed flask of the 250mL that magnetic stir bar is housed, add the multi-arm carbon nano-tube of 3g drying and the mixed acid of 15mL 60wt% red fuming nitric acid (RFNA) and the 45mL 98wt% concentrated sulfuric acid, spherical condensating tube and tail gas absorption pipe is loaded onto with after 150W ultrasonic wave process 30min, be heated to 120 DEG C, stir and reflux down and react 24h, after reaction terminates, dilute with 800mL deionized water, with little 0.22 μm of mixed fine miillpore filter suction filtration, with deionized water cyclic washing repeatedly to neutral, 60 DEG C of vacuumize 24h obtain carboxylated carbon nanomaterial;
(2) in the beaker of a 150mL, add the carboxylated carbon nanomaterial of the preparation in 15mg (1) step, then 50mL ethanol is added, 150W ultrasonic disperse 10 minutes, leave standstill and remove bottom precipitation after 12 hours, in the dispersion liquid of upper strata, add the ethanolic solution of 50mL 5mg/mL nano-silver thread afterwards, then at the ultrasonic 30s of 50W, obtain the mixed solution of nano-silver thread and carboxylated carbon nanomaterial;
The mixed solution of nano-silver thread and carboxylated carbon nanomaterial is sprayed film forming on transparent base, sprays fast 1mL/h, heat 30min at the film 120 ~ 200 DEG C of one-tenth, obtain described transparent conductive film.The performance test results of obtained transparent conductive film is as shown in table 1.
Embodiment 4
Prepare transparent conductive film based on nano-silver thread and carboxylated carbon nanomaterial, comprise following steps:
(1) in the mono-neck round-bottomed flask of the 250mL that magnetic stir bar is housed, add the fullerene of 3g drying and the mixed acid of 15mL 60wt% red fuming nitric acid (RFNA) and the 45mL 98wt% concentrated sulfuric acid, spherical condensating tube and tail gas absorption pipe is loaded onto with after 150W ultrasonic wave process 30min, be heated to 120 DEG C, stir and reflux down and react 24h, after reaction terminates, dilute with 800mL deionized water, with little 0.22 μm of mixed fine miillpore filter suction filtration, with deionized water cyclic washing repeatedly to neutral, 60 DEG C of vacuumize 24h obtain carboxylated carbon nanomaterial;
(2) in the beaker of a 150mL, add the carboxylated carbon nanomaterial of the preparation in 10mg step (1), then 50mL ethanol is added, 150W ultrasonic disperse 10 minutes, leave standstill and remove bottom precipitation after 12 hours, in dispersion liquid, add the ethanolic solution of 50mL 5mg/mL nano-silver thread afterwards, then at the ultrasonic 30s of 50W, obtain the mixed solution of nano-silver thread and carboxylated carbon nanomaterial;
The mixed solution of nano-silver thread and carboxylated carbon nanomaterial is carried out spin-coating film on transparent base, rotating speed 2000r/min, heat 40min by the film 140 ~ 200 DEG C made, obtain described transparent conductive film.The performance test results of obtained transparent conductive film is as shown in table 1.
Embodiment 5
Prepare transparent conductive film based on nano-silver thread and carboxylated carbon nanomaterial, comprise following steps:
(1) carboxylated carbon nanomaterial is prepared according to the method for step (1) in embodiment 2;
(2) in the beaker of a 150mL, 50mL ethanol is added after adding the carboxylated carbon nanomaterial of the preparation in 50mg step (1), 150W ultrasonic disperse 30 minutes, leave standstill and remove bottom precipitation after 12 hours, the ethanolic solution of 50mL 1mg/mL nano-silver thread is added afterwards in dispersion liquid, then at the ultrasonic 30s of 50W, the mixed solution of nano-silver thread and carboxylated carbon nanomaterial is obtained;
The mixed solution of nano-silver thread and carboxylated carbon nanomaterial is carried out spin-coating film on transparent base, rotating speed 1500r/min, heat 30min by the film 160 ~ 200 DEG C made, obtain described transparent conductive film.The performance test results of obtained transparent conductive film is as shown in table 1.
Embodiment 6
Prepare transparent conductive film based on nano-silver thread and carboxylated carbon nanomaterial, comprise following steps:
(1) carboxylated carbon nanomaterial is prepared according to the method for step (1) in embodiment 1;
(2) in the beaker of a 150mL, 50mL ethanol is added after adding the carboxylated carbon nanomaterial of the preparation in 10mg step (1), 150W ultrasonic disperse 10 minutes, leave standstill and remove bottom precipitation after 12 hours, the ethanolic solution of 50mL 5mg/mL nano-silver thread is added afterwards in dispersion liquid, then at the ultrasonic 30s of 50W, the mixed solution of nano-silver thread and carboxylated carbon nanomaterial is obtained;
The mixed solution of nano-silver thread and carboxylated carbon nanomaterial is carried out blade coating film forming on transparent base, wet-film thickness 20um, heat 30min by the film 150 ~ 200 DEG C made, obtain described transparent conductive film.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.
Nano-silver thread and carbon nanomaterial have feature separately preparing in transparent conductive film: it is poorer than carbon nanomaterial that nano-silver thread is prepared in conductive film light transmission and mist degree, but electric conductivity is better than carbon nanomaterial, therefore the present invention utilizes respective advantage mutually to supplement.The dispersive property of bi-material is optimized and makes it can form a kind of mixed dispersion liquid by the present invention, and both can reach good electric conductivity when preparing transparent conductive film like this, light transmission is also very good.
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., based on a preparation method for the transparent conductive film of nano-silver thread and carboxylated carbon nanomaterial, it is characterized in that, comprise following steps:
(1) 1 ~ 10g carbon nanomaterial is joined in the mixed acid containing 15 ~ 100mL 60wt% red fuming nitric acid (RFNA) and 0 ~ 100mL98wt% concentrated sulfuric acid, after ultrasonic disperse, adding thermal agitation and reacting under counterflow condition; After reaction terminates, suction filtration, with deionized water cyclic washing repeatedly to neutral, vacuumize obtains carboxylated carbon nanomaterial;
(2) get the obtained carboxylated carbon nanomaterial of a certain amount of step (1) and to add in solvent then ultrasonic disperse, leave standstill afterwards or centrifugal removing sediment, add the ethanolic solution of a certain amount of nano-silver thread again, after ultrasonic disperse, obtain the mixed solution of nano-silver thread and carboxylated carbon nanomaterial; The ratio of the solid content of the nano-silver thread wherein in the quality of carboxylated carbon nanomaterial and the ethanolic solution of nano-silver thread is 5 ~ 20:5 ~ 30;
The mixed solution getting a certain amount of nano-silver thread and carboxylated carbon nanomaterial carries out film on transparent base, then carries out annealing in process, obtains described transparent conductive film.
2. the preparation method of a kind of transparent conductive film based on nano-silver thread and carboxylated carbon nanomaterial according to claim 1, it is characterized in that, the carbon nanomaterial described in step (1) is at least one in carbon nano-tube, Graphene, carbon nano-fiber, nano carbon microsphere and fullerene.
3. the preparation method of a kind of transparent conductive film based on nano-silver thread and carboxylated carbon nanomaterial according to claim 1, it is characterized in that, the reaction temperature described in step (1) is 110 ~ 130 DEG C, and the reaction time is 24 ~ 48h.
4. the preparation method of a kind of transparent conductive film based on nano-silver thread and carboxylated carbon nanomaterial according to claim 1, is characterized in that, the condition of the ultrasonic disperse described in step (1) is that 50 ~ 250W disperses 10 ~ 60min.
5. the preparation method of a kind of transparent conductive film based on nano-silver thread and carboxylated carbon nanomaterial according to claim 1, it is characterized in that, the solvent described in step (2) is at least one in water, methyl alcohol, ethanol and propyl alcohol.
6. the preparation method of a kind of transparent conductive film based on nano-silver thread and carboxylated carbon nanomaterial according to claim 1, it is characterized in that, the concentration in a solvent of the carboxylated carbon nanomaterial described in step (2) is 0.1 ~ 3mg/mL.
7. the preparation method of a kind of transparent conductive film based on nano-silver thread and carboxylated carbon nanomaterial according to claim 1, it is characterized in that, the time of repose described in step (2) is 12 ~ 48h; Centrifugal rotational speed described in step (2) is 2000 ~ 8000r/min.
8. the preparation method of a kind of transparent conductive film based on nano-silver thread and carboxylated carbon nanomaterial according to claim 1, it is characterized in that, in the ethanolic solution of nano-silver thread described in step (2), the concentration of nano-silver thread is 0.1 ~ 10mg/mL; Diameter 30 ~ the 150nm of described nano-silver thread, length is 4 ~ 50 μm.
9. the preparation method of a kind of transparent conductive film based on nano-silver thread and carboxylated carbon nanomaterial according to claim 1, it is characterized in that, the condition that carboxylated carbon nanomaterial described in step (2) adds ultrasonic disperse in solvent is that 50 ~ 250W disperses 10 ~ 60min, and the ultrasonic disperse condition after the ethanolic solution of nano-silver thread that adds is that 50 ~ 100W disperses 10 ~ 60s.
10. the preparation method of a kind of transparent conductive film based on nano-silver thread and carboxylated carbon nanomaterial according to claim 1, 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; Annealing temperature described in step (2) is 100 ~ 200 DEG C.
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Application publication date: 20150902 |