CN107768023A - There is composite construction conducting film of high adhesion force and preparation method thereof based on graphene - Google Patents
There is composite construction conducting film of high adhesion force and preparation method thereof based on graphene Download PDFInfo
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Abstract
The present invention relates to graphene composite material field, discloses composite construction conducting film for having high adhesion force based on graphene and preparation method thereof, the preparation method prepares graphene oxide including S1.；S2. twice ultrasonic disperses：Graphene oxide that step S1 is prepared is soluble in water to carry out secondary ultrasonic disperse processing, then obtains aqueous solution of single-layer grapheme oxide；S3.PET film process：PET film is handled using physical etchings first, obtains the PET film of surface irregularity, is cleaned, after drying, then hydrophilic radical is plated on PET film surface by corona method, the PET film after being handled；S4. spin coating：To PET film progressively spin coating poly (glycidyl methacrylate) solution, graphene oxide water solution, the AgNWs aqueous solution and the graphene oxide water solution after being handled in step S3, whole process is placed in atmosphere of inert gases, after obtained film drying, it is placed in hydrazine steam and reduces, has reacted and cleaned with deionized water.
Description
Technical field
The present invention relates to graphene composite material field, has answering for high adhesion force more particularly, to based on graphene
Close structural conductive film and preparation method thereof.
Background technology
Conductive and transparent film is needed in the manufacturing process of flat-panel monitor and touch-screen.It is most commonly used at present to be
Tin indium oxide (ITO) film, it is primarily due to target preparation and the film-forming process all comparative maturities of the material.Although ito thin film
There are good electric conductivity and the transparency, but its cost is high, flexibility is poor, environment is unfriendly (indium has severe toxicity).So research and development can substitute
ITO film is extremely urgent.
Graphene nanometer sheet causes great concern due to its excellent machinery, optics, calorifics and electric property, it
It is cheaper than CNT or AgNWs, there is abundant material source, substantially increase the feasibility of its practical application, it is existing
Flexible curved surface equipment in the backing material used be mostly polyethylene terephthalate (PET) film, PET macromoleculars link
Structure is regular, and crystallinity is higher, and without highly polar group in molecule, therefore its surface compatibility is poor.Use PET base material conduct at present
For the graphene transparent conductive film of flexible substrate when by multiple Bending Deformation, there is a certain degree of tortoise in graphene conductive layer
Split or even fall from pet sheet emaciated face, cause flexible apparatus disabler, yield is relatively low, and which has limited graphene transparent conductive film
Further apply.Mainly there are surface cladding process, surface oxidation method, plasma method, height to PET base material surface treatment method at present
Can radiate etc., but this have impact on PET bulk properties or is unable to reach long-term modified effect.
Graphene conductive film generally use redox solution method at present, can be notable because not needing vacuum equipment
Cost is reduced, therefore various countries all are stepping up to study to the field.However, graphene obtained by redox solution method is reduction-oxidation
Graphene, its lamella is simultaneously discontinuous, " the carbon cake " of composition is mutually mixed for multi-layer graphene piece, in addition, molten using redox
The problem of can not fully reducing film resistor, the redox graphene film and common graphite be present in graphene film made of liquid method
Film resistor and the similar even below existing ito thin film product of transparency.
The content of the invention
The shortcomings that technical problems to be solved of the present invention are to be directed to prior art ito thin film, introduce graphene and receive
Meter Yin, while graphene adhesive force is improved, also improve Thin film conductive rate and light transmittance, there is provided have based on graphene high attached
The composite construction conduction membrane preparation method puted forth effort.
The present invention also provides a kind of composite junction based on graphene with high adhesion force being prepared using the above method
Structure conducting film.
The purpose of the present invention is achieved by the following technical programs：
There is provided has the composite construction conduction membrane preparation method of high adhesion force based on graphene, comprises the following steps：
S1. graphene oxide is prepared：Graphene oxide is prepared using Hummers methods are improved；
S2. twice ultrasonic disperses：Graphene oxide that step S1 is prepared is soluble in water to be carried out at secondary ultrasonic disperse
Reason, then obtains aqueous solution of single-layer grapheme oxide；
S3.PET film process：PET film is handled using physical etchings first, the PET film of surface irregularity is obtained, cleaning, does
After dry, then hydrophilic radical plated on PET film surface by corona method, the PET film after being handled；
S4. spin coating：To in step S3 handle after PET film progressively spin coating poly (glycidyl methacrylate) solution, oxidation stone
Black aqueous solution, the AgNWs aqueous solution and graphene oxide water solution, whole process are placed in atmosphere of inert gases, thin by being made
After film is dried, it is placed in hydrazine steam and reduces, reacted and cleaned with deionized water, finally give has high attachment based on graphene
The composite construction conducting film of power.
The graphene oxide being prepared in step S1 of the present invention using improvement Hummers methods possesses more polyfunctional group, phase
To larger surface area, beneficial to follow-up recombination reaction；Step S2 handles to obtain dispersiveness preferably using secondary ultrasonic disperse
Aqueous solution of single-layer grapheme oxide, film evenly can be obtained in coating procedure, lamella and discontinuous is avoided, is multilayer stone
Black alkene piece mutually mixes " the carbon cake " of composition；After being handled in step S3 by physical etchings, film surface is set to become rough,
Appropriate roughness is effective to the adhesion for improving pet sheet face, coordinates corona further to improve adhesive force；Step S4
It is middle that thickness can effectively be controlled using spin coating proceeding, the uniformity of film is improved, is made using poly (glycidyl methacrylate) solution
For binding agent, because itself contains aerobic, nitrogen-atoms, it can not only be acted with PET, be attached to pet sheet face well, and
And oxygen activity group can also be coordinated with graphene in molecular structure so that this structure is firmer, and current-carrying part is creative
Ground is using graphene, Nano Silver, graphene three-decker, and due to connection and shearing effect, the graphene interlayers structure can be more
Closely contacted with Nano Silver, effectively reduce resistance, in the case where content of nanometer silver is low, graphene plays connection nanometer
The effect of silver, so as to significantly reduce AgNWs usage amounts, reduces cost.
Preferably, the temperature of first time ultrasonic disperse is 30 ~ 50 DEG C in step S2, frequency is 10000 ~ 25000 Hz, stream
Speed is 1.0 ~ 4.0m3/ h, circulation stirring speed are 1000 ~ 2000r/min, the ultrasonic disperse time is 0.5 ~ 2.0h；Second super
The scattered temperature of sound is 30 ~ 50 DEG C, frequency is 18000 ~ 25000 Hz, flow velocity is 2.0 ~ 5.0m3/ h, circulation stirring speed are
1000 ~ 2000r/min, ultrasonic disperse time are 2 ~ 5h.
Preferably, graphene oxide water solution concentration described in step S2 is 0.1~0.5g/L.
Preferably, corona method described in step S3 is to use corona machine, and discharge power is 0.3~1.5 KVA, rotating speed
100~500r/min.
Preferably, poly (glycidyl methacrylate) solution concentration described in step S4 is 0.2~1.0g/L, and solvent is
THF。
Preferably, the AgNWs concentration of aqueous solution is 3.0~15g/L.
Preferably, spin speed described in step S4 is 100~200rpm, time 10s.
Preferably, film drying temperature described in step S4 is 70~100 DEG C, and the time is 5~10min.
Preferably, 100 DEG C of hydrazine steam reduction temperature described in step S4, recovery time 24h.
The present invention also provides a kind of composite junction based on graphene with high adhesion force being prepared using the above method
Structure conducting film, applied to solar cell, flat-panel monitor or touch-screen field.
Compared with prior art, the beneficial effects of the invention are as follows：
The present invention using improving Hummers methods, being handled by secondary ultrasonic disperse, obtained polyfunctional group, large surface area,
The preferable single-layer graphene oxide solution of dispersiveness, using the solution as raw material, be advantageous to subsequently with Nano Silver it is compound with
And the uniformity of coating, by the use to PET etching processings and binding agent, the adhesive force of PET film is drastically increased,
Nano Silver is introduced in graphene interlayers framework, effectively reduces resistance, in the case where content of nanometer silver is low, graphene plays
The effect of Nano Silver is connected, so as to significantly reduce AgNWs usage amounts, reduces cost, also improves the machine of film in itself
Tool performance, coming off for nano-silver thread, fixed conductive network so that thoroughly can effectively be prevented by the protection of graphene interlayers structure
The electric conductivity of conductive film is more stable.
Preparation technology of the present invention is simple, by twice ultrasonic decentralized processing, obtains finely dispersed single-layer graphene oxide
The aqueous solution, evenly, solving prior art oxidation-reduction method, to be prepared into graphene film lamella discontinuous, overlapping for coating, so as to
The problem of influenceing conductive and light transmittance.
The graphene/nano silver line nesa coating electric property and optical property that the present invention is prepared are outstanding, compare
Traditional ito thin film product, sheet resistance be 22.9 Europe/square, light transmittance 87%.It can be seen that the electric conductivity of the transparent conductive film
Can be excellent, translucency is good.In addition, after doing bend test 500 times to the transparent conductive film, its sheet resistance be 26.2 Europe/square,
After doing bend test 1000 times, its sheet resistance become turn to 30.8 Europe/square, show that the transparent conductive film adhesive force is stronger.
Brief description of the drawings
Fig. 1 the first ultrasonic device structural representations.
Fig. 2 the second ultrasonic device structural representations.
Embodiment
The present invention is further illustrated with reference to specific embodiment.Following examples are only illustrative examples, not structure
Into inappropriate limitation of the present invention, the multitude of different ways that the present invention can be limited and covered by the content of the invention is implemented.It is unless special
Do not mentionlet alone bright, the present invention reagent, compound and the equipment that use is the art conventional reagent, compound and equipment.
Embodiment 1
The present embodiment provides the composite construction conduction membrane preparation method based on graphene with high adhesion force, comprises the following steps：
S1. graphene oxide is prepared：Graphene oxide is prepared using Hummers methods are improved；
S2. twice ultrasonic disperses：The graphene oxide twice ultrasonic soluble in water that carries out that step S1 is prepared disperses, then
Obtain 0.1g/L graphene oxide water solutions；
S3.PET film process：PET film is handled using physical etchings first, the PET film of surface irregularity is obtained, cleaning, does
After dry, then hydrophilic radical plated on PET film surface by corona method, specifically using corona machine, discharge power 0.3
~1.5 KVA, 100~500r/min of rotating speed, the PET film after being handled；
S4. spin coating：PET film after handling in step s3 instills 0.2g/L poly (glycidyl methacrylate) solution（Solvent
For THF）, it is then spin coated onto, spin speed is 100~200rpm, time 10s, and 5~10min is dried at 40~60 DEG C, is used
The above method coats 0.1g/L graphene oxide water solutions, 3.0g/L the AgNWs aqueous solution and 0.1g/L graphene oxides successively
The aqueous solution, whole process are placed in atmosphere of inert gases, and by obtained film drying, drying temperature is 70~100 DEG C, and the time is
5~10min, reductase 12 4h in 100 DEG C of hydrazine steam is subsequently placed in, all graphene oxide films is reduced, has reacted and used deionized water
Cleaning, finally gives the composite construction conducting film with high adhesion force based on graphene；
Wherein, in step S2 the temperature of first time ultrasonic disperse be 30 ~ 50 DEG C, frequency be 10000 ~ 25000 Hz, flow velocity 1.0
~4.0m3/ h, circulation stirring speed are 1000 ~ 2000 r/min, the ultrasonic disperse time is 0.5 ~ 2.0 h；
The temperature of second of ultrasonic disperse is 30 ~ 50 DEG C, frequency is 18000 ~ 25000 Hz, flow velocity is 2.0 ~ 5.0 m3/ h, follow
Ring mixing speed is 1000 ~ 2000 r/min, the ultrasonic disperse time is 2 ~ 5h；
Inert gas is nitrogen, argon gas, the one or more of helium in step S4；
The AgNWs aqueous solution is synthesized using two step polyol reduction methods, and detailed process is as follows：0.3M PVP and 0.2M NaCl are existed
Mixed in reaction vessel and in 160 DEG C of heating.By 1MAgNO 3It is added in mixture, then after 5 minutes, is delayed using peristaltic pump
It is slow to add 1M AgNO3；When the color of solution becomes mist, by the AgNO of residual3Solution is added in container immediately.30 points
Zhong Hou, prepared AgNWs is washed with deionized three times by centrifuging.
As shown in Fig. 1~2, the present embodiment also provides a kind of twice ultrasonic dispersing apparatus, including the first ultrasonic device and
Two ultrasonic devices, the first circulation system that the first ultrasonic device includes the first batch mixing pond 1 and multiple first ultrasonic reaction kettles form,
First ultrasonic reaction kettle includes Vltrasonic device 3 and reactor 4, and the first batch mixing pond 1 is provided with dog-house 101, and upper end passes through pipeline 2
It is connected with the first ultrasonic reaction kettle, lower end connects the first ultrasonic reaction kettle by pipeline 6 respectively, pipeline 7 connects with the first discharge port 8
Connect, pipeline 6 is provided with centrifugal pump 61 and flowmeter 62, and multiple first ultrasonic reaction kettles are in difference in height arrangement connection, wherein horizontal
Connected between position minimum the first ultrasonic reaction kettle and pipeline 7 by pipeline 9；
The second circulation system that second ultrasonic device includes the second batch mixing pond 10 and multiple second ultrasonic reaction kettles form, the second surpasses
Phonoresponse kettle is identical with the first ultrasonic reaction kettle structure, and the upper end in the second batch mixing pond is connected by the ultrasonic reaction kettle of pipeline 11 and second
Connect, lower end is connected with pipeline 12；Pipeline 12 is provided with charging aperture 13, centrifugal pump 14, the flowmeter 15 being connected with the first discharge port 8
With the second discharge port 16, the second ultrasonic reaction kettle horizontal level is sequentially connected, and is provided with air bleeding valve, and passes through pipeline 17 and pipe
Road 12 connects, wherein the first ultrasonic device and the second ultrasonic device also include multiple ball valves 18 being arranged on pipeline.
The present embodiment ultrasonic disperse equipment controls frequency and temperature by Vltrasonic device 3, and centrifugal pump carrys out coutroi velocity, the
First, agitator in the second batch mixing pond controls mixing speed, is then carried out step by step by controlling ball valve to realize.
The graphene oxide being prepared in the present embodiment step S1 using improvement Hummers methods possesses more polyfunctional group,
Relatively large surface area, beneficial to follow-up recombination reaction；Step S2 using secondary ultrasonic disperse handle to obtain dispersiveness compared with
Good aqueous solution of single-layer grapheme oxide, can obtain film evenly in coating procedure, avoid lamella and discontinuous, be multilayer
Graphene film mutually mixes " the carbon cake " of composition；After being handled in step S3 by physical etchings, make film surface become it is coarse not
Flat, appropriate roughness is effective to the adhesion for improving pet sheet face, coordinates corona further to improve adhesive force；Step
Thickness can effectively be controlled using spin coating proceeding in rapid S4, improve the uniformity of film, it is molten using poly (glycidyl methacrylate)
Liquid, because itself contains aerobic, nitrogen-atoms, can not only act with PET as binding agent, be attached to pet sheet well
Face, and oxygen activity group can also be coordinated with graphene in molecular structure so that and this structure is firmer, current-carrying part wound
Graphene, Nano Silver, graphene three-decker are used to the property made, due to connection and shearing effect, the graphene interlayers structure can
More closely to be contacted with Nano Silver, resistance is effectively reduced, in the case where content of nanometer silver is low, graphene plays connection
The effect of Nano Silver, so as to significantly reduce AgNWs usage amounts, reduce cost.
Use the electric conductivity and light transmittance of four-point probe and ultraviolet specrophotometer testing film.The present embodiment obtains
Transparent conductive film sheet resistance for 23.2 Europe/square, light transmittance 85%.It can be seen that the electric conductivity of the transparent conductive film
Excellent, translucency is good.After bend test 500 times is done to the transparent conductive film, its sheet resistance be 26.7 Europe/square, bend
Experiment 1000 times after, its sheet resistance become turn to 31.8 Europe/square.
Embodiment 2
The present embodiment provides the composite construction conduction membrane preparation method based on graphene with high adhesion force, comprises the following steps：
S1. graphene oxide is prepared：Graphene oxide is prepared using Hummers methods are improved；
S2. twice ultrasonic disperses：The graphene oxide twice ultrasonic soluble in water that carries out that step S1 is prepared disperses, then
Obtain 0.5g/L graphene oxide water solutions；
S3.PET film process：PET film is handled using physical etchings first, the PET film of surface irregularity is obtained, cleaning, does
After dry, then hydrophilic radical plated on PET film surface by corona method, specifically using corona machine, discharge power 0.3
~1.5 KVA, 100~500r/min of rotating speed, the PET film after being handled；
S4. spin coating：PET film after handling in step s3 instills 1.0g/L poly (glycidyl methacrylate) solution（Solvent
For THF）, it is then spin coated onto, spin speed is 100~200rpm, time 10s, and 5~10min is then dried at 40~60 DEG C,
Coat 0.5g/L graphene oxide water solutions, 15g/L the AgNWs aqueous solution and 0.5g/L graphite oxides successively using the above method
Aqueous solution, whole process are placed in atmosphere of inert gases, and by obtained film drying, drying temperature is 70~100 DEG C, the time
For 5~10min, reductase 12 4h in 100 DEG C of hydrazine steam is subsequently placed in, all graphene oxide films is reduced, has reacted and used deionization
Water cleans, and finally gives the composite construction conducting film with high adhesion force based on graphene；
Wherein, in step S2 the temperature of first time ultrasonic disperse be 30 ~ 50 DEG C, frequency be 10000 ~ 25000 Hz, flow velocity 1.0
~4.0m3/ h, circulation stirring speed are 1000 ~ 2000 r/min, the ultrasonic disperse time is 0.5 ~ 2.0 h；
The temperature of second of ultrasonic disperse is 30 ~ 50 DEG C, frequency is 18000 ~ 25000 Hz, flow velocity is 2.0 ~ 5.0 m3/ h, follow
Ring mixing speed is 1000 ~ 2000 r/min, the ultrasonic disperse time is 2 ~ 5h；
Inert gas is nitrogen, argon gas, the one or more of helium in step S4.
Use the electric conductivity and light transmittance of four-point probe and ultraviolet specrophotometer testing film.The present embodiment obtains
Transparent conductive film sheet resistance for 22.9 Europe/square, light transmittance 87%.It can be seen that the electric conductivity of the transparent conductive film
Excellent, translucency is good.After bend test 500 times is done to the transparent conductive film, its sheet resistance be 26.2 Europe/square, bend
Experiment 1000 times after, its sheet resistance become turn to 30.8 Europe/square.
Comparative example 1
This comparative example is substantially the same manner as Example 1, and difference is, does not use physical etchings to handle in step S3, obtains table
The smooth PET film in face.
Use the electric conductivity and light transmittance of four-point probe and ultraviolet specrophotometer testing film.The present embodiment obtains
Transparent conductive film sheet resistance for 23.5 Europe/square, light transmittance 84%.Bend test 500 is done to the transparent conductive film
After secondary, its sheet resistance be 31.6 Europe/square, after doing bend test 1000 times, its sheet resistance become turn to 37.5 Europe/square, main cause
It is by the surface treatment to PET film, adhesion property can be improved.
Comparative example 2
This comparative example is substantially the same manner as Example 1, and difference is, poly (glycidyl methacrylate) is not had in step S4
Solution, successively spin coating graphene oxide, the AgNWs aqueous solution and graphene oxide.
Use the electric conductivity and light transmittance of four-point probe and ultraviolet specrophotometer testing film.The present embodiment obtains
Transparent conductive film sheet resistance for 23.3 Europe/square, light transmittance 84%.Bend test 500 is done to the transparent conductive film
After secondary, its sheet resistance be 35.7 Europe/square, this comparative example conductive coating after bend test 500 times is done is easy to and PET material point
Open, do not possess performance.
Comparative example 3
This comparative example is substantially the same manner as Example 1, and difference is, spin coating process is the poly- methyl-prop of spin coating successively in step S4
Olefin(e) acid glycidol ester solution, graphene oxide and the AgNWs aqueous solution.
Use the electric conductivity and light transmittance of four-point probe and ultraviolet specrophotometer testing film.The present embodiment obtains
Transparent conductive film sheet resistance for 29.7 Europe/square, light transmittance 84%.
Claims (10)
1. there is the composite construction conduction membrane preparation method of high adhesion force based on graphene, it is characterised in that comprise the following steps：
S1. graphene oxide is prepared：Graphene oxide is prepared using Hummers methods are improved；
S2. twice ultrasonic disperses：Graphene oxide that step S1 is prepared is soluble in water to be carried out at secondary ultrasonic disperse
Reason, then obtains aqueous solution of single-layer grapheme oxide；
S3.PET film process：PET film is handled using physical etchings first, the PET film of surface irregularity is obtained, cleaning, does
After dry, then hydrophilic radical plated on PET film surface by corona method, the PET film after being handled；
S4. spin coating：To in step S3 handle after PET film progressively spin coating poly (glycidyl methacrylate) solution, oxidation stone
Black aqueous solution, the AgNWs aqueous solution and graphene oxide water solution, whole process are placed in atmosphere of inert gases, thin by being made
After film is dried, it is placed in hydrazine steam and reduces, reacted and cleaned with deionized water, finally give has high attachment based on graphene
The composite construction conducting film of power.
2. there is the composite construction conduction membrane preparation method of high adhesion force, its feature based on graphene according to claim 1
Be, the temperature of first time ultrasonic disperse is 30~50 DEG C in step S2, frequency is 10000~25000Hz, flow velocity be 1.0~
4.0m3/ h, circulation stirring speed are 1000~2000r/min, the ultrasonic disperse time is 0.5~2.0h；Second of ultrasonic disperse
Temperature be 30~50 DEG C, frequency is 18000~25000Hz, flow velocity is 2.0~5.0m3/ h, circulation stirring speed be 1000~
2000r/min, ultrasonic disperse time are 2~5h.
3. there is the composite construction conduction membrane preparation method of high adhesion force, its feature based on graphene according to claim 1
It is, graphene oxide water solution concentration described in step S2 is 0.1~0.5g/L.
4. there is the composite construction conduction membrane preparation method of high adhesion force, its feature based on graphene according to claim 1
It is, corona method described in step S3 is to use corona machine, and discharge power is 0.3~1.5KVA, 100~500r/ of rotating speed
min。
5. there is the composite construction conduction membrane preparation method of high adhesion force, its feature based on graphene according to claim 1
It is, poly (glycidyl methacrylate) solution concentration described in step S4 is 0.2~1.0g/L, solvent THF.
6. there is the composite construction conduction membrane preparation method of high adhesion force, its feature based on graphene according to claim 1
It is, the AgNWs concentration of aqueous solution is 3.0~15g/L.
7. there is the composite construction conduction membrane preparation method of high adhesion force, its feature based on graphene according to claim 1
It is, spin speed described in step S4 is 100~200rpm, time 10s.
8. there is the composite construction conduction membrane preparation method of high adhesion force, its feature based on graphene according to claim 1
It is, film drying temperature described in step S4 is 70~100 DEG C, and the time is 5~10min.
9. there is the composite construction conduction membrane preparation method of high adhesion force, its feature based on graphene according to claim 1
It is, 100 DEG C of hydrazine steam reduction temperature described in step S4, recovery time 24h.
10. there is the composite construction conducting film of high adhesion force based on graphene, it is characterised in that any one by claim 1~9
The composite construction conduction membrane preparation method for having high adhesion force based on graphene described in is prepared.
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| CN116231061A (en) * | 2023-02-23 | 2023-06-06 | 北京纯锂新能源科技有限公司 | Preparation device and method of fluorinated crosslinked polymer film |
| CN116231061B (en) * | 2023-02-23 | 2023-10-03 | 北京纯锂新能源科技有限公司 | Preparation device and method of fluorinated crosslinked polymer film |
| CN118416710A (en) * | 2024-07-03 | 2024-08-02 | 浙江钱江水利供水有限公司 | Ultra-filtration microporous reverse osmosis PTFE membrane and preparation method thereof |
| CN118416710B (en) * | 2024-07-03 | 2024-09-06 | 浙江钱江水利供水有限公司 | Ultra-filtration microporous reverse osmosis PTFE membrane and preparation method thereof |
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