CN106504829B - A kind of preparation method of high transmittance low resistance nano silver wire film - Google Patents
A kind of preparation method of high transmittance low resistance nano silver wire film Download PDFInfo
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- CN106504829B CN106504829B CN201610956482.7A CN201610956482A CN106504829B CN 106504829 B CN106504829 B CN 106504829B CN 201610956482 A CN201610956482 A CN 201610956482A CN 106504829 B CN106504829 B CN 106504829B
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 91
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 238000002834 transmittance Methods 0.000 title claims abstract description 21
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 48
- 230000001476 alcoholic effect Effects 0.000 claims abstract description 37
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 27
- 239000007788 liquid Substances 0.000 claims abstract description 23
- 239000000758 substrate Substances 0.000 claims abstract description 21
- 239000002270 dispersing agent Substances 0.000 claims abstract description 18
- 239000012452 mother liquor Substances 0.000 claims abstract description 18
- 239000000126 substance Substances 0.000 claims abstract description 18
- 208000011580 syndromic disease Diseases 0.000 claims abstract description 17
- 239000006185 dispersion Substances 0.000 claims abstract description 15
- 238000005119 centrifugation Methods 0.000 claims abstract description 11
- 239000004094 surface-active agent Substances 0.000 claims abstract description 10
- 239000011248 coating agent Substances 0.000 claims abstract description 9
- 238000000576 coating method Methods 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 150000005846 sugar alcohols Polymers 0.000 claims abstract description 8
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- 229910021645 metal ion Inorganic materials 0.000 claims abstract description 5
- 239000012535 impurity Substances 0.000 claims abstract description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 42
- 238000004528 spin coating Methods 0.000 claims description 17
- 238000003756 stirring Methods 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 8
- 229910052709 silver Inorganic materials 0.000 claims description 8
- 239000004332 silver Substances 0.000 claims description 8
- 238000010792 warming Methods 0.000 claims description 8
- 230000036571 hydration Effects 0.000 claims description 6
- 238000006703 hydration reaction Methods 0.000 claims description 6
- 239000002105 nanoparticle Substances 0.000 claims description 6
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 4
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 4
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 claims description 2
- 229910021380 Manganese Chloride Inorganic materials 0.000 claims description 2
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 claims description 2
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 claims description 2
- 229920003081 Povidone K 30 Polymers 0.000 claims description 2
- 229920003082 Povidone K 90 Polymers 0.000 claims description 2
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 239000003599 detergent Substances 0.000 claims description 2
- 235000011187 glycerol Nutrition 0.000 claims description 2
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 claims description 2
- 239000011565 manganese chloride Substances 0.000 claims description 2
- 235000002867 manganese chloride Nutrition 0.000 claims description 2
- 239000000463 material Substances 0.000 claims description 2
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical class Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 2
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 2
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 2
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 2
- ULWHHBHJGPPBCO-UHFFFAOYSA-N propane-1,1-diol Chemical class CCC(O)O ULWHHBHJGPPBCO-UHFFFAOYSA-N 0.000 claims description 2
- 239000011780 sodium chloride Substances 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 230000003213 activating effect Effects 0.000 claims 1
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims 1
- 229920006316 polyvinylpyrrolidine Polymers 0.000 claims 1
- 239000010408 film Substances 0.000 description 41
- 238000000034 method Methods 0.000 description 8
- 235000012149 noodles Nutrition 0.000 description 8
- 238000000926 separation method Methods 0.000 description 6
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 241000209094 Oryza Species 0.000 description 2
- 235000007164 Oryza sativa Nutrition 0.000 description 2
- 239000002042 Silver nanowire Substances 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000011031 large-scale manufacturing process Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 235000009566 rice Nutrition 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- MPMSMUBQXQALQI-UHFFFAOYSA-N cobalt phthalocyanine Chemical compound [Co+2].C12=CC=CC=C2C(N=C2[N-]C(C3=CC=CC=C32)=N2)=NC1=NC([C]1C=CC=CC1=1)=NC=1N=C1[C]3C=CC=CC3=C2[N-]1 MPMSMUBQXQALQI-UHFFFAOYSA-N 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000007970 homogeneous dispersion Substances 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- -1 polyethylene Pyrrolidones Polymers 0.000 description 1
- 238000003303 reheating Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
- H01B13/0026—Apparatus for manufacturing conducting or semi-conducting layers, e.g. deposition of metal
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
Abstract
The present invention discloses a kind of preparation method of high transmittance low resistance nano silver wire film, comprises the following steps：A) silver nitrate is dissolved in polyalcohol, well mixed by being ultrasonically treated, it is 0.1mol L to obtain amount of substance concentration‑1~0.5mol L‑1Silver nitrate alcoholic solution；B) surfactant is dissolved in polyalcohol, it is 0.05mol L to obtain substance withdrawl syndrome‑1~0.5mol L‑1Surfactant alcoholic solution；C) by silver nitrate alcoholic solution and surfactant alcoholic solution by volume 4:5 ratio mixing, adds Metal Ion Control Agents, then heats up, stands, and obtains nano silver wire mother liquor；D) to the washing of nano silver wire mother liquor, centrifugation made from step c, dispersant is used after going the removal of impurity, it is 0.2mgmL to obtain mass volume ratio‑1~20molL‑1Nano silver wire dispersion liquid, nano silver wire length be 80uM~200uM, a diameter of 40nM~100nm；E) clean substrate is inserted in spin coater, by nano silver wire dispersant liquid drop made from step d after the completion of substrate surface, coating, naturally dry obtains nano silver wire film.
Description
Technical field
The present invention relates to transparent conductive film manufacturing technology field, specifically a kind of high transmittance low resistance nano silver wire is thin
The preparation method of film.
Background technology
Transparent conductive film shows as a kind of important photoelectric function thin films in solar cell, Electronic Paper, flat liquid crystal
Show, the electronics and information industry field such as FED and touch-screen has a wide range of applications.With the development of science and technology, electronic device
Develop to flexibility and lighting direction, for the transparent conductive film with high transmittance, high conductivity and high-flexibility
The market demand is increasing.In recent years, based on the transparent conductive film of nano silver wire in optics, electricity and flexibility etc. table
The superperformance revealed is got the attention.
At this stage, the few of the method report of nano silver wire transparent conductive film is prepared.《A kind of mist degree adjustable flexibility is transparent
The preparation method of conductive film》（The A of publication number CN 102527621）Chinese patent disclosed in method, silver is made first and receives
Rice noodles ink, then film, reheating, pressurization, drying obtain sheet resistance and are less than 300 Ω/ on a flexible substrate, and transmitance is more than
85% nano silver wire transparent conductive film.《Flexible transparent conducting film and its manufacture method》（Publication number CN102693772 A）'s
In method disclosed in Chinese patent, nano-silver thread homogeneous dispersion is coated on another flexible transparent substrate surface and obtains Nano Silver
Line film, by hot pressing or transfer modes, the top layer that film transfer is adhered to transparent ink obtains flexible transparent conducting film, its
Sheet resistance is in 35~500 Ω/, and transmitance is 50%~80%.
The preparation process of existing nano silver wire transparent conductive film it is complicated, it is necessary to it is extraneous provide as inert gas shielding,
The conditions such as shading, high pressure, stirring, this certainly will add the complexity of technique, and inconvenience is brought for large-scale production.At present,
The biggest problem that nano silver wire transparent conductive film faces is still that sheet resistance is too big, and transmitance is undesirable.
The content of the invention
It is an object of the invention to provide a kind of preparation method of high transmittance low resistance nano silver wire film, this method work
Skill is simple, can prepare high transmittance, low resistance, has the nano silver wire transparent conductive film of excellent photoelectric properties.
The technical solution adopted for the present invention to solve the technical problems is：
A kind of preparation method of high transmittance low resistance nano silver wire film, comprises the following steps：
A) silver nitrate is dissolved in polyalcohol, and it is well mixed by being ultrasonically treated, and obtaining substance withdrawl syndrome is
0.1mol•L-1~0.5mol L-1Silver nitrate alcoholic solution；
B) surfactant is dissolved in polyalcohol, it is 0.05mol L to obtain substance withdrawl syndrome-1~0.5mol L-1Surfactant alcoholic solution；
C) by the silver nitrate alcoholic solution and surfactant alcoholic solution by volume 4:5 ratio mixing, stirs
The amount for adding material afterwards is 1 × 10-6Mol~5 × 10-5Mol Metal Ion Control Agents, then 80 DEG C~110 DEG C are warming up to, it is quiet
2h~12h is put, obtains nano silver wire mother liquor；
D) to nano silver wire mother liquor washing made from step c, centrifuge, after going the removal of impurity, using dispersant by its point
Intersperse among and preserve in brown bottle；The mass volume ratio of nano silver wire and dispersant is 0.2mgmL-1~20 mgm L-1；Silver
Nano silver wire length is 80um~200um, a diameter of 40nm~100nm in nanowire dispersion；
E) clean substrate is inserted in spin coater, by nano silver wire dispersant liquid drop made from step d in substrate surface,
After the completion of coating, naturally dry obtains nano silver wire film.
Further, the polyalcohol uses ethylene glycol, propane diols, glycerine or isopropanol.
Further, the Metal Ion Control Agents using Iron(III) chloride hexahydrate, sodium chloride, four hydration Nickel Chlorides,
Six hydration manganous chloride or six hydration cobaltous dichlorides.
Further, the surfactant is using PVP K30, polyvinylpyrrolidone K45, polyethylene
Pyrrolidones K60 or PVP K90.
Further, the washing in the step d is washed using absolute ethyl alcohol, acetone or deionized water as detergent
Number 6~10 times；Described centrifuge uses centrifuge, and centrifugal rotational speed 2000rpm~8000rpm, centrifugation time 10min~
40min。
Further, the dispersant in step d is absolute ethyl alcohol, isopropanol, one kind in ethylene glycol monomethyl ether or any two
The mixed liquor of kind.
Further, spin speed is 500r/min~5000r/min in step e, and spin-coating time is 20s~90s, spin coating
Number is 2 times~20 times.
The invention has the advantages that length is first prepared as 80um~200um, a diameter of 40nm~100nm long silver
Nano wire；It is used into dispersant again, prepares the Yin Na of low resistance high transmission by way of spin coating plated film on substrate
Rice noodles transparent conductive film.The preparation of long nano silver wire causes the negligible amounts of silver wire in film surface unit area, so as to have
Beneficial to the visible light transmissivity for improving film；Meanwhile nano silver wire is longer, section that film surface unit area interior lines are intersected with line
Count less, cause resistance to increase because nano silver wire connection is loose at node, and less nodes effectively reduce film
Resistance, so as to improve the electric conductivity of film.In addition, the selection of dispersant and suitable nano silver wire dispersion liquid concentration are really
One of fixed and obtained low resistance high transmission nano silver wire transparent conductive film key technology.Present invention process is simple, repeatability
Height, stability is good, film mode is simple, easily realizes large-scale production.
Embodiment
Embodiment one
The present invention provides a kind of preparation method of high transmittance low resistance nano silver wire film, comprises the following steps：
A) 0.8g silver nitrates are dissolved in 40mL ethylene glycol, the ultrasonic 30min in the ultrasonic wave that ultrasonic power is 100W,
It is 0.1mol L to obtain substance withdrawl syndrome-1Silver nitrate alcoholic solution；
B) 0.68gPVP- K90 are weighed to be dissolved in 50mL ethylene glycol, are placed in three-necked flask, stirring fills it
Divide dissolving, it is 0.05mol L to obtain substance withdrawl syndrome-1PVP- K90 alcoholic solutions；
C) by the silver nitrate alcoholic solution and PVP- K90 alcoholic solutions by volume 4:5 ratio mixing, stirs 5min, adds
Enter 5 × 10-6molFeCl3·6H2O, then 80 DEG C are warming up to, 2h is stood, obtains nano silver wire mother liquor；
D) nano silver wire mother liquor made from step c is washed 6 times with absolute ethyl alcohol, centrifuge separation, centrifugal rotational speed
2000rpm, centrifugation time 10min, and disperseed using absolute ethyl alcohol, it is 0.5mgmL to obtain mass volume ratio-1Yin Na
Rice noodles dispersion liquid；Nano silver wire length is 80 in nano silver wire alcoholic solutionuM, a diameter of 40nm；
E) clean substrate is inserted in spin coater, by nano silver wire dispersant liquid drop made from step d in substrate surface,
Spin speed is 500r/min, and spin-coating time 20s, spin coating number is 2 times, and after the completion of coating, naturally dry obtains Yin Na
Rice noodles film.
Embodiment two
The present invention provides a kind of preparation method of high transmittance low resistance nano silver wire film, comprises the following steps：
A) 1g silver nitrates are dissolved in 40mL ethylene glycol, the ultrasonic 30min in the ultrasonic wave that ultrasonic power is 100W, obtained
It is 0.25mol L to substance withdrawl syndrome-1Silver nitrate alcoholic solution；
B) 0.8gPVP- K90 are weighed to be dissolved in 50mL ethylene glycol, are placed in three-necked flask, stirring makes its abundant
Dissolving, it is 0.1mol L to obtain substance withdrawl syndrome-1PVP- K90 alcoholic solutions；
C) by the silver nitrate alcoholic solution and PVP- K90 alcoholic solutions by volume 4:5 ratio mixing, stirs 5min, adds
Enter 7.5 × 10-6molFeCl3·6H2O, then 110 DEG C are warming up to, 4h is stood, obtains nano silver wire mother liquor；
D) nano silver wire mother liquor made from step c is washed with deionized 6 times, centrifuge separation, centrifugal rotational speed
3000rpm, centrifugation time 15min, and use absolute ethyl alcohol to be disperseed to obtain mass volume ratio for 1mgmL-1Silver nanoparticle
Line dispersion liquid；Nano silver wire length is 100 in nano silver wire dispersion liquiduM, a diameter of 50nm；
E) clean substrate is inserted in spin coater, by nano silver wire dispersant liquid drop made from step d in substrate surface,
Spin speed is 1000r/min, and spin-coating time 30s, spin coating number is 4 times, and after the completion of coating, naturally dry obtains Yin Na
Rice noodles film.
Embodiment three
The present invention provides a kind of preparation method of high transmittance low resistance nano silver wire film, comprises the following steps：
A) 1g silver nitrates are dissolved in 40mL ethylene glycol, the ultrasonic 30min in the ultrasonic wave that ultrasonic power is 100W, obtained
It is 0.25mol L to substance withdrawl syndrome-1Silver nitrate alcoholic solution；
B) 0.98gPVP- K90 are weighed to be dissolved in 50mL ethylene glycol, are placed in three-necked flask, stirring fills it
Divide dissolving, it is 0.15mol L to obtain substance withdrawl syndrome-1PVP- K90 alcoholic solutions；
C) by the silver nitrate alcoholic solution and PVP- K90 alcoholic solutions by volume 4:5 ratio mixing, stirs 5min, adds
Enter 2 × 10-5molFeCl3·6H2O, then 110 DEG C are warming up to, 12h is stood, obtains nano silver wire mother liquor；
D) nano silver wire mother liquor made from step c is washed with deionized 6 times, centrifuge separation, centrifugal rotational speed
4000rpm, centrifugation time 20min, and use absolute ethyl alcohol to be disperseed to obtain mass volume ratio for 4mgmL-1Silver nanoparticle
Line dispersion liquid；Nano silver wire length is 110 in nano silver wire dispersion liquiduM, a diameter of 60nm；
E) clean substrate is inserted in spin coater, by nano silver wire dispersant liquid drop made from step d in substrate surface,
Spin speed is 1000r/min, and spin-coating time 30s, spin coating number is 6 times, and after the completion of coating, naturally dry obtains Yin Na
Rice noodles film.
Example IV
The present invention provides a kind of preparation method of high transmittance low resistance nano silver wire film, comprises the following steps：
A) 1g silver nitrates are dissolved in 40mL ethylene glycol, the ultrasonic 30min in the ultrasonic wave that ultrasonic power is 100W, obtained
It is 0.25mol L to substance withdrawl syndrome-1Silver nitrate alcoholic solution；
B) 1.1430gPVP- K90 are weighed to be dissolved in 50mL ethylene glycol, are placed in three-necked flask, stirring makes it
Fully dissolving, it is 0.3mol L to obtain substance withdrawl syndrome-1PVP- K90 alcoholic solutions；
C) by the silver nitrate alcoholic solution and PVP- K90 alcoholic solutions by volume 4:5 ratio mixing, stirs 5min, adds
Enter 2.5 × 10-5molFeCl3·6H2O, then 110 DEG C are warming up to, 6h is stood, obtains nano silver wire mother liquor；
D) nano silver wire mother liquor made from step c is washed with deionized 6 times, centrifuge separation, centrifugal rotational speed
8000rpm, centrifugation time 40min, and use absolute ethyl alcohol to be disperseed to obtain mass volume ratio for 2mgmL-1Silver nanoparticle
Line dispersion liquid；Nano silver wire length is 200 in nano silver wire dispersion liquiduM, a diameter of 100nm；
E) clean substrate is inserted in spin coater, by nano silver wire dispersant liquid drop made from step d in substrate surface,
Spin speed is 1500r/min, and spin-coating time 30s, spin coating number is 8 times, and after the completion of coating, naturally dry obtains Yin Na
Rice noodles film.
Embodiment five
The present invention provides a kind of preparation method of high transmittance low resistance nano silver wire film, comprises the following steps：
A) 1g silver nitrates are dissolved in 50mL ethylene glycol, the ultrasonic 30min in the ultrasonic wave that ultrasonic power is 100W, obtained
It is 0.2mol L to substance withdrawl syndrome-1Silver nitrate alcoholic solution；
B) 1.3070gPVP- K90 are weighed to be dissolved in 50mL ethylene glycol, are placed in three-necked flask, stirring makes it
Fully dissolving, it is 0.3mol L to obtain substance withdrawl syndrome-1PVP- K90 alcoholic solutions；
C) by the silver nitrate alcoholic solution and PVP- K90 alcoholic solutions by volume 4:5 ratio mixing, stirs 5min, adds
Enter 1.5 × 10-5molFeCl3·6H2O, then 130 DEG C are warming up to, 8h is stood, obtains nano silver wire mother liquor；
D) nano silver wire mother liquor made from step c is washed with deionized 6 times, centrifuge separation, centrifugal rotational speed
8000rpm, centrifugation time 40min, and use absolute ethyl alcohol to be disperseed to obtain mass volume ratio for 6mgmL-1Silver nanoparticle
Line dispersion liquid；Nano silver wire length is 180 in nano silver wire dispersion liquiduM, a diameter of 100nm；
E) clean substrate is inserted in spin coater, by nano silver wire dispersant liquid drop made from step d in substrate surface,
Spin speed is 2000r/min, and spin-coating time 30s, spin coating number is 6 times, and after the completion of coating, naturally dry obtains Yin Na
Rice noodles film.
Embodiment six
The present invention provides a kind of preparation method of high transmittance low resistance nano silver wire film, comprises the following steps：
A) 1g silver nitrates are dissolved in 50mL ethylene glycol, the ultrasonic 30min in the ultrasonic wave that ultrasonic power is 100W, obtained
It is 0.2mol L to substance withdrawl syndrome-1Silver nitrate alcoholic solution；
B) 0.98gPVP- K90 are weighed to be dissolved in 50mL ethylene glycol, are placed in three-necked flask, stirring fills it
Divide dissolving, it is 0.3mol L to obtain substance withdrawl syndrome-1PVP- K90 alcoholic solutions；
C) by the silver nitrate alcoholic solution and PVP- K90 alcoholic solutions by volume 4:5 ratio mixing, stirs 5min, adds
Enter 2 × 10-5molFeCl3·6H2O, then 100 DEG C are warming up to, 10h is stood, obtains nano silver wire mother liquor；
D) nano silver wire mother liquor made from step c is washed with deionized 6 times, centrifuge separation, centrifugal rotational speed
8000rpm, centrifugation time 30min, and use absolute ethyl alcohol to be disperseed to obtain mass volume ratio for 8mgmL-1Silver nanoparticle
Line dispersion liquid；Nano silver wire length is 150 in nano silver wire dispersion liquiduM, a diameter of 100nm；
E) clean substrate is inserted in spin coater, by nano silver wire dispersant liquid drop made from step d in substrate surface,
Spin speed is 3000r/min, and spin-coating time 40s, spin coating number is 10 times, and after the completion of coating, naturally dry obtains silver
Nano wire film.
The above described is only a preferred embodiment of the present invention, any formal limitation not is made to the present invention；Appoint
What those skilled in the art, without departing from the scope of the technical proposal of the invention, all using the side of the disclosure above
Method and technology contents make many possible changes and modifications to technical solution of the present invention, or are revised as the equivalent reality of equivalent variations
Apply example.Therefore, every content without departing from technical solution of the present invention, the technical spirit according to the present invention are done to above example
Any simple modification, equivalent substitution, equivalence changes and modification, still fall within the range of technical solution of the present invention protects.
Claims (7)
1. a kind of preparation method of high transmittance low resistance nano silver wire film, it is characterised in that comprise the following steps：
A) silver nitrate is dissolved in polyalcohol, and it is well mixed by being ultrasonically treated, and it is 0.1mol L to obtain substance withdrawl syndrome-1~0.5mol L-1Silver nitrate alcoholic solution；
B) surfactant is dissolved in polyalcohol, it is 0.05mol L to obtain substance withdrawl syndrome-1~0.5mol L-1Table
Face activating agent alcoholic solution；
C) by the silver nitrate alcoholic solution and surfactant alcoholic solution by volume 4:5 ratio mixing, adds after stirring
The amount for entering material is 1 × 10-6Mol~5 × 10-5Mol Metal Ion Control Agents, then 80 DEG C~110 DEG C are warming up to, stand 2h
~12h, obtain nano silver wire mother liquor；
D) to the washing of nano silver wire mother liquor, centrifugation made from step c, after going the removal of impurity, disperseed to put using dispersant
Preserved in brown bottle；The mass volume ratio of nano silver wire and dispersant is 0.2mgmL-1~20 mgm L-1；Silver nanoparticle
Nano silver wire length is 80um~200um, a diameter of 40nm~100nm in line dispersion liquid；
E) clean substrate is inserted in spin coater, by nano silver wire dispersant liquid drop made from step d in substrate surface, coating
After the completion of, naturally dry obtains nano silver wire film.
A kind of 2. preparation method of high transmittance low resistance nano silver wire film according to claim 1, it is characterised in that
The polyalcohol uses ethylene glycol, propane diols, glycerine or isopropanol.
3. a kind of preparation method of high transmittance low resistance nano silver wire film according to claim 1 or 2, its feature exist
In the Metal Ion Control Agents are using Iron(III) chloride hexahydrate, sodium chloride, four hydration Nickel Chlorides, six hydration manganous chloride
Or six hydration cobaltous dichloride.
4. a kind of preparation method of high transmittance low resistance nano silver wire film according to claim 1 or 2, its feature exist
In, the surfactant using PVP K30, polyvinylpyrrolidone K45, polyvinylpyrrolidone K60 or
PVP K90.
5. a kind of preparation method of high transmittance low resistance nano silver wire film according to claim 1 or 2, its feature exist
In the washing in the step d is using absolute ethyl alcohol, acetone or deionized water as detergent, washing times 6~10 times；Institute
State centrifugation and use centrifuge, centrifugal rotational speed 2000rpm~8000rpm, centrifugation time 10min~40min.
6. a kind of preparation method of high transmittance low resistance nano silver wire film according to claim 1 or 2, its feature exist
In the dispersant in step d is absolute ethyl alcohol, isopropanol, one kind in ethylene glycol monomethyl ether or any two kinds of mixed liquor.
7. a kind of preparation method of high transmittance low resistance nano silver wire film according to claim 1 or 2, its feature exist
In spin speed is 500r/min~5000r/min in step e, and spin-coating time is 20s~90s, and spin coating number is 2 times~20
It is secondary.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610956482.7A CN106504829B (en) | 2016-10-27 | 2016-10-27 | A kind of preparation method of high transmittance low resistance nano silver wire film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201610956482.7A CN106504829B (en) | 2016-10-27 | 2016-10-27 | A kind of preparation method of high transmittance low resistance nano silver wire film |
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| CN108057899B (en) * | 2017-12-07 | 2020-07-21 | 深圳大学 | C, N-doped AgPd nanowire and preparation method thereof |
| CN108627267A (en) * | 2018-05-10 | 2018-10-09 | 北京工业大学 | A kind of temperature sensor based on nano silver wire network |
| CN108971510A (en) * | 2018-07-26 | 2018-12-11 | 深圳清华大学研究院 | Silver nanowires and preparation method thereof, silver nanowires film and laminated film |
| CN110875098A (en) * | 2018-08-29 | 2020-03-10 | 天津大学 | Nano silver wire conductive ink sintered film based on hot-pressing sintering and preparation method and application thereof |
| CN110875100A (en) * | 2018-08-29 | 2020-03-10 | 天津大学 | Nano silver wire conductive ink sintered film based on sodium chloride hot-pressing sintering and preparation method and application thereof |
| CN109346242B (en) * | 2018-09-29 | 2020-04-28 | 华南理工大学 | Transparent electrode based on silver nanowires and preparation method thereof |
| CN112008181A (en) * | 2019-05-31 | 2020-12-01 | 天津大学 | Process for welding silver nanowires |
| CN111879230A (en) * | 2020-06-18 | 2020-11-03 | 山东师范大学 | Method for preparing polylactic acid flexible strain sensor of silver nanowires and application thereof |
| CN111909570B (en) * | 2020-06-19 | 2022-10-21 | 世大新材料(深圳)有限公司 | Synthesis method of silver nanowire ink and preparation method of flexible conductive film |
| CN112971725B (en) * | 2021-02-10 | 2023-12-26 | 武汉理工大学 | Preparation of electromagnetic radiation resistant nanocellulose/silver nanowire flexible sensor |
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