CN108376587A - A kind of high-performance stablizes the preparation method of copper nano-wire flexible transparent conductive film - Google Patents
A kind of high-performance stablizes the preparation method of copper nano-wire flexible transparent conductive film Download PDFInfo
- Publication number
- CN108376587A CN108376587A CN201810188525.0A CN201810188525A CN108376587A CN 108376587 A CN108376587 A CN 108376587A CN 201810188525 A CN201810188525 A CN 201810188525A CN 108376587 A CN108376587 A CN 108376587A
- Authority
- CN
- China
- Prior art keywords
- preparation
- copper nano
- wire
- conductive film
- transparent conductive
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
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
Abstract
A kind of high-performance stablizes the preparation method of copper nano-wire flexible transparent conductive film, it include the preparation of copper nano-wire, the preparation of CuNWsTCF 1, the preparation of CuNWsTCF 2, the preparation of CuNWsTCF 3 and etc. be made.A kind of high-performance of the present invention stablizes copper nano-wire flexible transparent conductive film, product preparation process copper wire is not in clustering phenomena, film surface is not in particle, the case where fusing will not occur in preparation process, the phenomenon that flavescence greening will not occur, finished product transmitance is high, electric conductivity is excellent, its transmitance is up to 86% or more, sheet resistance is less than 25 Ω/sq, it is used to prepare display equipment, the good visual effect of its touch screen, the picture of presentation is all the image quality for more having a sense of hierarchy more high definition exquisiteness, color seems to compare natural reality, and transmitance height is also smaller to the injury of eyes, finished product stability is good, it can preferably be preserved in conventional environment and adverse circumstances, preparation method simple possible, marketing application is made.
Description
Technical field
The invention belongs to transparent conductive film technical fields, and in particular to a kind of high-performance stabilization copper nano-wire flexible and transparent
The preparation method of conductive film.
Background technology
Transparent conductive film (TCF) is a kind of material having both translucency and electric conductivity, is widely used in touch screen, has
The fields such as machine light emitting diode, solar cell, flat-panel screens and intelligent glass.In recent years, with electronic device flexibility,
Lightening direction is developed, and tin indium oxide (ITO) is since it is expensive and the frangible property of material itself cannot meet
The needs of flexible electronic, accordingly, it is desirable to find a kind of material substituting ITO, copper nano-wire (Cu NWs) is excellent because of its
Electric conductivity, optical property and abundant reserves become the material for being most expected to substitute ITO.
Currently, mainly preparing copper nano-wire transparent conductive film by the methods of vacuum filtration method, roll coating process and spray coating method.
Since the copper nano-wire surface of synthesis has coated remaining organic matter and oxide layer, line resistance is increased, is received to reduce copper
The electric conductivity of rice noodles transparent conductive film hinders its application in the opto-electronic device.Existing frequently-used method is in hydrogen gas
Lower 300 DEG C of atmosphere is annealed to improve the electric conductivity of copper nano-wire film.However, due to the flexible substrates such as PET non-refractory (＜ 180
DEG C), this method is not suitable for copper nano-wire fexible film, therefore finds a kind of effective low temperature post-processing approach removing copper nanometer
The oxide layer and residual organic matter on line surface are very crucial for application of the copper nano-wire in flexible electronic device.Another party
Face, the aerial copper nano-wire of exposure, oxide layer can be spontaneously formed on its surface.Even if in solution, because in solution
Dissolved oxygen can also form oxide layer.Therefore inhibit copper nano-wire oxidation and its be applied to transparent electrode required for solve
One of critical issue.In terms of the anti-oxidant research of copper nano-wire transparent electrode, carbon coating copper nano-wire and nickel coated copper nanometer
Line is currently used two methods.Although both methods significantly improves the stability of copper nano-wire transparent electrode,
More photoelectric properties are sacrificed, therefore a kind of in the photoelectricity for not sacrificing or sacrificing less copper nano-wire transparent electrode there is an urgent need for finding
Under the premise of performance, the effective ways of its stability are significantly improved.At present apparently, copper is still remained in copper nano-wire preparation process
The case where the phenomenon that line is susceptible to clustering phenomena, film surface is susceptible to particle, preparation process are susceptible to fusing easily goes out
Phenomena such as now flavescence greening, finished product be oxidizable, transmitance, sheet resistance etc. are not satisfactory and leads to the technical problems such as application range limitation
Urgent need to resolve.
Invention content
The purpose of the present invention is to provide the preparation methods that a kind of high-performance stablizes copper nano-wire flexible transparent conductive film.
The purpose of the present invention is what is realized by following technical measures：
A kind of high-performance stablizes the preparation method of copper nano-wire flexible transparent conductive film, which is characterized in that it includes copper
The preparation of nano wire, the preparation of CuNWsTCF-1, the preparation of CuNWsTCF-2, the preparation of CuNWsTCF-3 and etc. be made.
Specifically, a kind of high-performance stablizes the preparation method of copper nano-wire flexible transparent conductive film, which is characterized in that
It is to include the following steps to be made：It takes copper chloride, glucose to be placed in appropriate vessel, deionized water is added, is heated to 45~55
It DEG C stirs evenly, obtains blue solution A；Separately oleyl amine, oleic acid, absolute ethyl alcohol is taken to be placed in appropriate vessel, stirs evenly, obtain mixed liquor
B；Separately PVP (Mw=55000) is taken to be dissolved in absolute ethyl alcohol to stir evenly, obtain solution C；Above-mentioned B, C mixed liquor is sequentially added molten
In liquid A, deionized water is added and is diluted to 1000ml, 11~13h is stirred in 48~52 DEG C of water-baths, is transferred to after stirring
In reaction kettle, 5~7h is reacted in 120 DEG C, after the completion of reaction, cooled to room temperature, liquid is in rotating speed after taking 50ml to react
10000~12000rpm/min carries out 4~6min of centrifuge washing, then outwells upper solution, and 30~40ml isopropanols are added,
Rotating speed be 10000~12000rpm/min carry out 4~6min of centrifuge washing, then outwell upper solution, be repeated 3 times isopropanol from
Heart cleaning operation collects centrifuge tube bottom precipitation and obtains copper nano-wire；Copper nano-wire isopropanol obtained above is disperseed
Dilution, then the nylon leaching film that via hole diameter is 0.22 μm are filtered by vacuum, and collect filter cake, the filter cake of collection is covered on PET,
Then it uses the weight of 500g to press 3~5min of filter press cake, 10~15min of baking in 75~85 DEG C of baking ovens is placed on after having pressed, is obtained
Copper nano-wire flexible transparent conductive film is labeled as CuNWsTCF-1, CuNWsTCF-1 is then immersed in sodium borohydride ethyl alcohol
In aqueous solution, it is 1 then to use volume ratio:1 absolute ethyl alcohol and the mixed solution of deionized water rinse 3~5 times, after flushing
It is placed in baking oven and toasts, obtain highly conductive copper nano-wire flexible transparent conductive film, be labeled as CuNWsTCF-2, then will
CuNWsTCF-2 is immersed in lauryl mercaptan ethanol solution, is taken out, and is rinsed 3~5 times with absolute ethyl alcohol, is placed in baking oven and toasts,
It obtains high-performance and stablizes copper nano-wire flexible transparent conductive film, be labeled as Cu NWsTCF-3.
Further, a kind of high-performance stablizes the preparation method of copper nano-wire flexible transparent conductive film, which is characterized in that its
In, the quality of copper chloride is 1.6~1.8g in prepared by solution A, and the quality of glucose is 1.90~2.00g, deionized water volume
Dosage is 700~800ml；Oleyl amine volume in prepared by the mixed liquid B is 18~22ml, and oleic acid volume is 0.1~0.3ml,
Absolute ethyl alcohol volume is 30~35ml；The quality of PVP (Mw=55000) is 1.20~1.30g, nothing in the preparation of the solution C
Water-ethanol volume is 20~30ml.
Further, a kind of high-performance stablizes the preparation method of copper nano-wire flexible transparent conductive film, which is characterized in that institute
A diameter of 40~the 60nm of copper nano-wire is stated, length is 60~70 μm；The copper nano-wire isopropanol dispersion is diluted to a concentration of
The copper nano-wire solution of 0.4~0.6mg/ml.
In order to enable copper wire is not in clustering phenomena in preparation process, film surface is not in particle phenomenon, a kind of
High-performance stablizes the preparation method of copper nano-wire flexible transparent conductive film, which is characterized in that the sodium borohydride ethyl alcohol is water-soluble
A concentration of 0.4~0.6mol/L of sodium borohydride in liquid, soaking time are 20~40s, wherein sodium borohydride ethanol water is
Sodium borohydride is dissolved in the mixed solution of absolute ethyl alcohol and deionized water composition, the volume ratio of absolute ethyl alcohol and deionized water
It is 1:1.
In order to enable the phenomenon that being not in fusing phenomenon in preparation process, being not in flavescence greening so that finished product is saturating
Rate higher, product sheet resistance smaller are crossed, a kind of high-performance stablizes the preparation method of copper nano-wire flexible transparent conductive film, feature
It is, a concentration of 0.4~0.6mol/L of the lauryl mercaptan ethanol solution, soaking time is 260s~300s.Further, one
Kind of high-performance stablizes the preparation method of copper nano-wire flexible transparent conductive film, which is characterized in that the baking oven baking temperature is
70~90 DEG C, baking time is 10~15 minutes.
The beneficial effects of the present invention are：
A kind of high-performance of the present invention stablizes copper nano-wire flexible transparent conductive film, and product preparation process copper wire is not in
Clustering phenomena, film surface are not in particle, and the case where fusing will not occur in preparation process, flavescence greening will not occur
The phenomenon that, finished product transmitance is high, and electric conductivity is excellent, and transmitance is up to 86% or more, and sheet resistance is less than 25 Ω/sq, for making
Standby display equipment, the picture of the good visual effect of touch screen, presentation is all the image quality for more having a sense of hierarchy more high definition exquisiteness, color
Seem to compare natural reality, and transmitance height is also smaller to the injury of eyes, finished product stability is good, conventional environment with
And adverse circumstances can be preserved preferably, preparation method simple possible, and marketing application is made.
Description of the drawings
Fig. 1 is each stage SEM figures of copper nano-wire flexible transparent conductive film preparation process, wherein (a) is original copper nanometer
Line chart is (b) to impregnate copper nano-wire figure after sodium borohydride solution, is (c) to impregnate copper nano-wire figure after lauryl mercaptan solution again.
Fig. 2 is each stage contact angle figure of copper nano-wire flexible transparent conductive film preparation process, wherein (a) receives for original copper
The contact angle figure of rice noodles film is (b) the contact angle figure of copper nano-wire film after immersion sodium borohydride solution, is (c) to impregnate again
The contact angle figure of lauryl mercaptan solution copper nano-wire film.
Fig. 3 is the sheet resistance comparison diagram (a) and transmitance pair of the different preparation process of copper nano-wire flexible transparent conductive film
Than figure (b).
Fig. 4 is that the sheet resistance that Cu NWs TCF-2 and Cu NWs TCF-3 made from embodiment 1 are placed 1 month in air becomes
Change situation map.
Fig. 5 be embodiment 1 made from Cu NWs TCF-2 and Cu NWs TCF-3 adverse circumstances (85% relative humidity,
85 DEG C of high temperature) place 9 hours sheet resistance figure of changing.
Specific implementation mode
The present invention is specifically described below by embodiment, it is necessary to which indicated herein is that following embodiment is only used
In invention is further explained, it should not be understood as limiting the scope of the invention, without departing substantially from spirit of that invention
In the case of essence, to modifications or substitutions made by the method for the present invention, step or condition, all belong to the scope of the present invention.
Embodiment 1
It takes copper chloride 1.6g, glucose 1.90g to be placed in beaker, deionized water 700ml is added, it is equal to be heated to 50 DEG C of stirrings
It is even, obtain blue solution A；Separately oleyl amine 18ml, oleic acid 0.1ml, absolute ethyl alcohol 32ml is taken to be placed in appropriate vessel, stirs evenly, obtain
Mixed liquid B；Separately PVP (Mw=55000) 1.20g is taken to be dissolved in 20ml absolute ethyl alcohols to stir evenly, obtain solution C；Above-mentioned B, C are mixed
It closes liquid to sequentially add in solution A, deionized water is added and is diluted to 1000ml, 12h is stirred in 50 DEG C of water-baths, after stirring
It is transferred in reaction kettle, reacts 6h in 120 DEG C, after the completion of reaction, cooled to room temperature, liquid is in rotating speed after taking 50ml to react
4~6min of centrifuge washing is carried out for 10000~12000rpm/min, then outwells upper solution, 35ml isopropanols are added, is being turned
Speed is that 10000~12000rpm/min carries out 4~6min of centrifuge washing, then outwells upper solution, is repeated 3 times isopropanol centrifugation
Cleaning operation, collect centrifuge tube bottom precipitation i.e. obtain copper nano-wire (after testing, obtained copper nano-wire a diameter of 40~
60nm, length are 60~70 μm), it is a concentration of that the isopropanol dispersion of copper nano-wire obtained is diluted to copper nano-wire
0.5mol/L, then the nylon leaching film of 0.22 μm of via hole diameter are filtered by vacuum, and filter cake is collected after suction filtration, and the filter cake of collection is covered
On PET, then uses the weight of 500g to press filter press cake 3min, while being placed in 80 DEG C of baking ovens and toasting 10min, obtain copper nano-wire
Flexible transparent conductive film is labeled as CuNWsTCF-1, CuNWsTCF-1 is then immersed in the boron hydrogen of a concentration of 0.5mol/L
Change 30s in sodium ethanol water, sodium borohydride ethanol water is that sodium borohydride is dissolved in absolute ethyl alcohol and deionized water group
At mixed solution in, the volume ratio of absolute ethyl alcohol and deionized water is 1:1.Then it is 1 to use volume ratio:1 absolute ethyl alcohol and
The mixed solution of deionized water rinses 4 times, is subsequently placed in baking oven and the baking 12 minutes of 80 DEG C of temperature is arranged, obtain highly conductive copper
Nano wire flexible transparent conductive film is labeled as CuNWsTCF-2, then CuNWsTCF-2 is immersed in 12 sulphur of 0.5mol/L
280s in alcohol ethanol solution takes out, and is rinsed 4 times with ethanol solution, is placed in baking oven and 80 DEG C of baking 12min of temperature are arranged,
It obtains high-performance and stablizes copper nano-wire flexible transparent conductive film, be labeled as CuNWsTCF-3.
As a result, it has been observed that do not find copper wire clustering phenomena in preparation process in preparation process, film surface also has no
Grain, the case where also having no fusing, the phenomenon that also not finding flavescence greening, finished product carries out transmitance and sheet resistance measures, and penetrates
Rate is 86%, and sheet resistance is 25 Ω/sq, shows that this product transmitance is high, electric conductivity is excellent.
Experiment one：Finished product stability is tested
CuNWsTCF-2 and CuNWsTCF-3 made from embodiment 1 is placed in air and is placed 1 month, two kinds of films are observed
Sheet resistance situation of change, transmitance is shown in Fig. 4 without significant change, specific experiment result.
CuNWsTCF-2 and CuNWsTCF-3 made from embodiment 1 is placed in relative humidity 85%, the constant temperature that 85 DEG C of temperature
In constant humidity cabinet, the sheet resistance situation of change of two kinds of films is observed.The experimental results showed that CuNWsTCF-2 is in relative humidity 85%, temperature
It spends in 85 DEG C of environment after placing 9h, about 16 times of sheet resistance increase, and CuNWsTCF-3 is in relative humidity 85%, 85 DEG C of environment of temperature
After placing 9h, sheet resistance is almost unchanged, and transmitance, without significant change, specific experiment result is shown in Fig. 5.
Embodiment 2
It takes copper chloride 1.7g, glucose 1.98g to be placed in beaker, deionized water 750ml is added, it is equal to be heated to 50 DEG C of stirrings
It is even, obtain blue solution A；Separately oleyl amine 20ml, oleic acid 0.2ml, absolute ethyl alcohol 30ml is taken to be placed in appropriate vessel, stirs evenly, obtain
Mixed liquid B；Separately PVP (Mw=55000) 1.25g is taken to be dissolved in 25ml absolute ethyl alcohols to stir evenly, obtain solution C；Above-mentioned B, C are mixed
It closes liquid to sequentially add in solution A, deionized water is added and is diluted to 1000ml, 13h is stirred in 48 DEG C of water-baths, after stirring
It is transferred in reaction kettle, reacts 5h in 120 DEG C, after the completion of reaction, cooled to room temperature, liquid is in rotating speed after taking 50ml to react
4~6min of centrifuge washing is carried out for 10000~12000rpm/min, then outwells upper solution, 35ml isopropanols are added, is being turned
Speed is that 10000~12000rpm/min carries out 4~6min of centrifuge washing, then outwells upper solution, is repeated 3 times isopropanol centrifugation
Cleaning operation, collect centrifuge tube bottom precipitation i.e. obtain copper nano-wire (after testing, obtained copper nano-wire a diameter of 40~
60nm, length are 60~70 μm), it is a concentration of that the isopropanol dispersion of copper nano-wire obtained is diluted to copper nano-wire
0.4mol/L, then the nylon leaching film of 0.22 μm of via hole diameter are filtered by vacuum, and filter cake is collected after suction filtration, and the filter cake of collection is covered
On PET, then uses the weight of 500g to press filter press cake 3min, while being placed in 75 DEG C of baking ovens and toasting 10min, obtain copper nano-wire
Flexible transparent conductive film is labeled as CuNWsTCF-1, CuNWsTCF-1 is then immersed in the boron hydrogen of a concentration of 0.4mol/L
Change 20s in sodium ethanol water, sodium borohydride ethanol water is that sodium borohydride is dissolved in absolute ethyl alcohol and deionized water group
At mixed solution in, the volume ratio of absolute ethyl alcohol and deionized water is 1:1.Then it is 1 to use volume ratio:1 absolute ethyl alcohol and
The mixed solution of deionized water rinses 4 times, is subsequently placed in baking oven and the baking 12 minutes of 80 DEG C of temperature is arranged, obtain highly conductive copper
Nano wire flexible transparent conductive film is labeled as CuNWsTCF-2, then CuNWsTCF-2 is immersed in 12 sulphur of 0.4mol/L
260s in alcohol ethanol solution takes out, and is rinsed 4 times with ethanol solution, is placed in baking oven and temperature 70 C baking 13min is arranged,
It obtains high-performance and stablizes copper nano-wire flexible transparent conductive film, be labeled as Cu NWsTCF-3.
As a result, it has been observed that do not find copper wire clustering phenomena in preparation process in preparation process, film surface also has no
Grain, the case where also having no fusing, the phenomenon that also not finding flavescence greening, finished product carries out transmitance and sheet resistance measures, and penetrates
Rate is 87%, and sheet resistance is 23 Ω/sq, shows that this product transmitance is high, electric conductivity is excellent.
By the experimental method of embodiment 1, stability experiment is carried out, the experimental results showed that, a kind of high-performance of the present invention is stablized
Copper nano-wire flexible transparent conductive film is placed at room temperature for one month, and sheet resistance has no significant change with transmitance.In relative humidity
85%, after placing 9h in 85 DEG C of environment of temperature, sheet resistance is almost unchanged, and transmitance shows that the present invention stablizes without significant change
Property is good.
Embodiment 3
It takes copper chloride 1.8g, glucose 2.00g to be placed in beaker, deionized water 800ml is added, it is equal to be heated to 50 DEG C of stirrings
It is even, obtain blue solution A；Separately oleyl amine 22ml, oleic acid 0.3ml, absolute ethyl alcohol 35ml is taken to be placed in appropriate vessel, stirs evenly, obtain
Mixed liquid B；Separately PVP (Mw=55000) 1.30g is taken to be dissolved in 25ml absolute ethyl alcohols to stir evenly, obtain solution C；Above-mentioned B, C are mixed
It closes liquid to sequentially add in solution A, deionized water is added and is diluted to 1000ml, 12h is stirred in 52 DEG C of water-baths, after stirring
It is transferred in reaction kettle, reacts 7h in 120 DEG C, after the completion of reaction, cooled to room temperature, liquid is in rotating speed after taking 50ml to react
4~6min of centrifuge washing is carried out for 10000~12000rpm/min, then outwells upper solution, 35ml isopropanols are added, is being turned
Speed is that 10000~12000rpm/min carries out 4~6min of centrifuge washing, then outwells upper solution, is repeated 3 times isopropanol centrifugation
Cleaning operation, collect centrifuge tube precipitation i.e. obtain copper nano-wire (after testing, a diameter of 40~60nm of obtained copper nano-wire,
Length is 60~70 μm), the isopropanol dispersion of copper nano-wire obtained is diluted to a concentration of 0.6mol/L of copper nano-wire, then
The nylon leaching film that 0.22 μm of via hole diameter is filtered by vacuum, and collects filter cake after suction filtration, the filter cake of collection is covered on PET, so
It uses the weight of 500g to press filter press cake 3min afterwards, while being placed in 75 DEG C of baking ovens and toasting 10min, obtain copper nano-wire flexible and transparent and lead
Conductive film is labeled as CuNWsTCF-1, CuNWsTCF-1 is then immersed in the sodium borohydride ethanol water of a concentration of 0.6mol/L
30s in solution, sodium borohydride ethanol water be by sodium borohydride be dissolved in absolute ethyl alcohol and deionized water composition mixing it is molten
In liquid, the volume ratio of absolute ethyl alcohol and deionized water is 1:1.Then it is 1 to use volume ratio:1 absolute ethyl alcohol and deionized water
Mixed solution rinses 4 times, is subsequently placed in baking oven and the baking 12 minutes of 80 DEG C of temperature is arranged, it is flexible to obtain highly conductive copper nano-wire
Transparent conductive film is labeled as CuNWsTCF-2, then CuNWsTCF-2 is immersed in the lauryl mercaptan ethanol solution of 0.5mol/L
Middle 260s takes out, and is rinsed 3 times with ethanol solution, is placed in baking oven and 80 DEG C of temperature baking 13min are arranged to get to high property
Copper nano-wire flexible transparent conductive film can be stablized, be labeled as Cu NWsTCF-3.
As a result, it has been observed that do not find copper wire clustering phenomena in preparation process in preparation process, film surface also has no
Grain, the case where also having no fusing, the phenomenon that also not finding flavescence greening, finished product carries out transmitance and sheet resistance measures, and penetrates
Rate is 86%, and sheet resistance is 24 Ω/sq, shows that this product transmitance is high, electric conductivity is excellent.
By the experimental method of embodiment 1, stability experiment is carried out, the experimental results showed that, a kind of high-performance of the present invention is stablized
Copper nano-wire flexible transparent conductive film is placed at room temperature for one month, and sheet resistance has no significant change with transmitance.In relative humidity
85%, after placing 9h in 85 DEG C of environment of temperature, sheet resistance is almost unchanged, and transmitance shows that the present invention stablizes without significant change
Property is good.
Claims (7)
1. a kind of high-performance stablizes the preparation method of copper nano-wire flexible transparent conductive film, which is characterized in that it includes that copper is received
The preparation of rice noodles, the preparation of CuNWsTCF-1, the preparation of CuNWsTCF-2, the preparation of CuNWsTCF-3 and etc. be made.
2. a kind of high-performance as described in claim 1 stablizes the preparation method of copper nano-wire flexible transparent conductive film, special
Sign is that it is to include the following steps to be made：It takes copper chloride, glucose to be placed in appropriate vessel, deionized water is added, is heated to
45 ~ 55 DEG C stir evenly, and obtain blue solution A；Separately oleyl amine, oleic acid, absolute ethyl alcohol is taken to be placed in appropriate vessel, stirs evenly, obtain
Mixed liquid B；Separately take PVP（Mw=55000）It is dissolved in absolute ethyl alcohol and stirring evenly, obtain solution C；Above-mentioned B, C mixed liquor is added successively
Enter in solution A, deionized water is added and is diluted to 1000ml, 11 ~ 13h is stirred in 48 ~ 52 DEG C of water-baths, is shifted after stirring
Into reaction kettle, 5 ~ 7h is reacted in 120 DEG C, after the completion of reaction, cooled to room temperature, liquid is in rotating speed after taking 50ml to react
10000 ~ 12000rpm/min carries out 4 ~ 6min of centrifuge washing, then outwells upper solution, and 35ml isopropanols are added, are in rotating speed
10000 ~ 12000rpm/min carries out 4 ~ 6min of centrifuge washing, then outwells upper solution, is repeated 3 times isopropanol eccentric cleaning behaviour
Make, collects centrifuge tube bottom precipitation and obtain copper nano-wire；Copper nano-wire obtained above is disperseed to dilute with isopropanol, then is passed through
Aperture is that 0.22 μm of nylon leaching film is filtered by vacuum, and collects filter cake, the filter cake of collection is covered on PET, is then used
The weight of 500g presses 3 ~ 5min of filter press cake, and 10 ~ 15min of baking in 75 ~ 85 DEG C of baking ovens is placed on after having pressed, it is soft to obtain copper nano-wire
Property transparent conductive film, be labeled as CuNWsTCF-1, then CuNWsTCF-1 is immersed in sodium borohydride ethanol water, so
It is 1 to use volume ratio afterwards:1 absolute ethyl alcohol and the mixed solution of deionized water rinse 3 ~ 5 times, and flushing, which finishes to be placed in baking oven, dries
It is roasting, highly conductive copper nano-wire flexible transparent conductive film is obtained, is labeled as CuNWsTCF-2, then CuNWsTCF-2 is immersed in
It in lauryl mercaptan ethanol solution, takes out, is rinsed 3 ~ 5 times with ethanol solution, be placed in baking oven and toast to get steady to high-performance
Determine copper nano-wire flexible transparent conductive film, is labeled as Cu NWsTCF-3.
3. a kind of high-performance as claimed in claim 2 stablizes the preparation method of copper nano-wire flexible transparent conductive film, special
Sign is, wherein the quality of copper chloride is 1.6 ~ 1.8g in prepared by solution A, and the quality of glucose is 1.90 ~ 2.00g, deionization
Water volume dosage is 700 ~ 800ml；Oleyl amine volume in prepared by the mixed liquid B is 18 ~ 22ml, oleic acid volume is 0.1 ~
0.3ml, absolute ethyl alcohol volume are 30 ~ 35ml；PVP in the preparation of the solution C（Mw=55000）Quality be 1.20 ~ 1.30g,
Absolute ethyl alcohol volume is 20 ~ 30ml.
4. a kind of high-performance as claimed in claim 3 stablizes the preparation method of copper nano-wire flexible transparent conductive film, special
Sign is that a diameter of 40 ~ 60nm of copper nano-wire, length is 60 ~ 70 μm；The copper nano-wire isopropanol dispersion is diluted to
The copper nano-wire solution of a concentration of 0.4 ~ 0.6mg/ml.
5. a kind of high-performance as claimed in claim 4 stablizes the preparation method of copper nano-wire flexible transparent conductive film, special
Sign is that a concentration of 0.4 ~ 0.6mol/L of sodium borohydride in the sodium borohydride ethanol water, soaking time is 20 ~ 40s,
Wherein, sodium borohydride ethanol water is dissolved in sodium borohydride in the mixed solution of absolute ethyl alcohol and deionized water composition,
The volume ratio of absolute ethyl alcohol and deionized water is 1:1.
6. a kind of high-performance as claimed in claim 5 stablizes the preparation method of copper nano-wire flexible transparent conductive film, special
Sign is that a concentration of 0.4 ~ 0.6mol/L of the lauryl mercaptan ethanol solution, soaking time is 260s ~ 300s.
7. a kind of high-performance as claimed in claim 6 stablizes the preparation method of copper nano-wire flexible transparent conductive film, special
Sign is that the baking oven baking temperature is 70 ~ 90 DEG C, and baking time is 10 ~ 15 minutes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810188525.0A CN108376587A (en) | 2018-03-07 | 2018-03-07 | A kind of high-performance stablizes the preparation method of copper nano-wire flexible transparent conductive film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810188525.0A CN108376587A (en) | 2018-03-07 | 2018-03-07 | A kind of high-performance stablizes the preparation method of copper nano-wire flexible transparent conductive film |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108376587A true CN108376587A (en) | 2018-08-07 |
Family
ID=63018611
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810188525.0A Pending CN108376587A (en) | 2018-03-07 | 2018-03-07 | A kind of high-performance stablizes the preparation method of copper nano-wire flexible transparent conductive film |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108376587A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108976914A (en) * | 2018-08-14 | 2018-12-11 | 重庆文理学院 | A kind of copper nano-wire conductive ink of high dispersive, conductive film and preparation method thereof |
| CN109465440A (en) * | 2018-11-08 | 2019-03-15 | 陕西煤业化工技术研究院有限责任公司 | A method of it is separated for silver nanowires length |
| CN113410339A (en) * | 2021-06-18 | 2021-09-17 | 中科检测技术服务(重庆)有限公司 | Preparation and application of high-stability nano-copper conductive film |
| CN114603154A (en) * | 2022-03-22 | 2022-06-10 | 武汉纺织大学 | Preparation method of copper nanowire and copper nanowire prepared by same |
| TWI793635B (en) * | 2020-06-15 | 2023-02-21 | 德克薩斯農工大學系統 | Copper nanowires and their use in plastics to improve thermal and electrical conductivity |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104299722A (en) * | 2014-09-05 | 2015-01-21 | 中国科学院合肥物质科学研究院 | Method for improving electrical conductivity of silver-nanowire transparent conductive film through solution method |
| CN104959622A (en) * | 2015-06-09 | 2015-10-07 | 重庆文理学院 | Synthesis method for copper nanowire with different length-diameter ratios |
| CN107103945A (en) * | 2017-06-23 | 2017-08-29 | 合肥工业大学 | A kind of copper nano-wire transparent conductive film and preparation method |
| CN107331445A (en) * | 2017-07-11 | 2017-11-07 | 湖南大学 | A kind of method of the electric conductivity and inoxidizability of modified nano silver wire nesa coating and raising nano silver wire nesa coating |
-
2018
- 2018-03-07 CN CN201810188525.0A patent/CN108376587A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104299722A (en) * | 2014-09-05 | 2015-01-21 | 中国科学院合肥物质科学研究院 | Method for improving electrical conductivity of silver-nanowire transparent conductive film through solution method |
| CN104959622A (en) * | 2015-06-09 | 2015-10-07 | 重庆文理学院 | Synthesis method for copper nanowire with different length-diameter ratios |
| CN107103945A (en) * | 2017-06-23 | 2017-08-29 | 合肥工业大学 | A kind of copper nano-wire transparent conductive film and preparation method |
| CN107331445A (en) * | 2017-07-11 | 2017-11-07 | 湖南大学 | A kind of method of the electric conductivity and inoxidizability of modified nano silver wire nesa coating and raising nano silver wire nesa coating |
Non-Patent Citations (1)
| Title |
|---|
| 王然龙: "铜纳米线透明导电薄膜的制备及性能研究", 《中国优秀硕士学位论文全文数据库工程科技I辑》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108976914A (en) * | 2018-08-14 | 2018-12-11 | 重庆文理学院 | A kind of copper nano-wire conductive ink of high dispersive, conductive film and preparation method thereof |
| CN108976914B (en) * | 2018-08-14 | 2021-06-22 | 重庆文理学院 | High-dispersion copper nanowire conductive ink, conductive film and preparation method thereof |
| CN109465440A (en) * | 2018-11-08 | 2019-03-15 | 陕西煤业化工技术研究院有限责任公司 | A method of it is separated for silver nanowires length |
| TWI793635B (en) * | 2020-06-15 | 2023-02-21 | 德克薩斯農工大學系統 | Copper nanowires and their use in plastics to improve thermal and electrical conductivity |
| CN113410339A (en) * | 2021-06-18 | 2021-09-17 | 中科检测技术服务(重庆)有限公司 | Preparation and application of high-stability nano-copper conductive film |
| CN113410339B (en) * | 2021-06-18 | 2023-08-15 | 中科检测技术服务(重庆)有限公司 | Preparation and application of high-stability nano copper conductive film |
| CN114603154A (en) * | 2022-03-22 | 2022-06-10 | 武汉纺织大学 | Preparation method of copper nanowire and copper nanowire prepared by same |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108376587A (en) | A kind of high-performance stablizes the preparation method of copper nano-wire flexible transparent conductive film | |
| CN105359070B (en) | Touch panel laminate, touch panel | |
| CN104599737B (en) | Micro-nano silver/high-molecular conductive composite material and preparation method and application thereof | |
| US20160196890A1 (en) | Conductive graphene-metal composite material, the production method of the same and use of the same | |
| CN102667969A (en) | Electroconductive film, method of manufacturing same, and touch panel | |
| CN108707997A (en) | Redox graphene coats the preparation method of copper nano-wire conducing composite material | |
| CN110518125A (en) | A kind of preparation method of cation doping perovskite solar battery | |
| CN107419244B (en) | A kind of nano-silver conductive film and preparation method thereof | |
| TW201435927A (en) | Transparent conductive film coating composition, transparent conductive film, and method for manufacturing transparent conductive film | |
| CN107275006A (en) | Redox graphene/SnO2Compound transparent electricity conductive film and preparation method thereof | |
| CN108695014A (en) | A kind of copper nano-wire preparation method and copper nano-wire compound transparent electricity conductive film | |
| TW201137896A (en) | Conductive film, method for producing the same, touch panel and integrated solar battery | |
| CN105609217B (en) | A kind of graphene transparent electrode, its preparation method and display device | |
| CN104733541B (en) | Conductive structure and preparation method thereof, array base palte, display device | |
| CN107103945A (en) | A kind of copper nano-wire transparent conductive film and preparation method | |
| CN102533261A (en) | Preparing method and application of red light materials based on ZnO doped with Co | |
| CN111922359A (en) | Preparation method of pure silver nanowires | |
| CN108735349A (en) | A kind of nano silver wire transparent conductive film and preparation method thereof containing ionic liquid | |
| CN108376588A (en) | A kind of nano silver wire and nickel oxide compound transparent electricity conductive film preparation method | |
| CN110085763A (en) | Flexible transparent electrode, flexible display panels, related manufacturing processes and display device | |
| CN108048842A (en) | A kind of etching liquid and its application method of nano silver wire conductive film | |
| CN104988475A (en) | Copper-nickel alloy nanowire flexible electrode and preparation method thereof | |
| CN102993995B (en) | Preparation method of transparent conductive film | |
| CN110783025A (en) | Oxidation-resistant conductive copper nanowire film and preparation method and application thereof | |
| CN109535078A (en) | A kind of naphthalimide derivative and solar battery |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20180807 |
|
| WD01 | Invention patent application deemed withdrawn after publication |