CN107673328A - A kind of graphene/nano silver line nesa coating and its preparation method and application - Google Patents
A kind of graphene/nano silver line nesa coating and its preparation method and application Download PDFInfo
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- CN107673328A CN107673328A CN201710886120.XA CN201710886120A CN107673328A CN 107673328 A CN107673328 A CN 107673328A CN 201710886120 A CN201710886120 A CN 201710886120A CN 107673328 A CN107673328 A CN 107673328A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/42—Coating with noble metals
- C23C18/44—Coating with noble metals using reducing agents
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
- H01B5/14—Non-insulated conductors or conductive bodies characterised by their form comprising conductive layers or films on insulating-supports
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- C01B2204/02—Single layer graphene
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/22—Electronic properties
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- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
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Abstract
The present invention relates to graphene composite material field, discloses a kind of graphene/nano silver line nesa coating and its preparation method and application.The graphene/nano silver line electrically conducting transparent membrane preparation method includes：S1. graphene oxide is prepared, S2. twice ultrasonics disperse, S3. glass substrates, S4. spin coatings.Preparation technology of the present invention is simple, by twice ultrasonic decentralized processing, obtains finely dispersed aqueous solution of single-layer grapheme oxide, and it is discontinuous, overlapping to solve the problems, such as that prior art oxidation-reduction method is prepared into graphene film lamella.Graphene oxide of the present invention only needs to react in substrate of glass after modification, adhesive force is improved without using other physical methods by APTS, and without secondary transferring graphene film, using finely dispersed single-layer graphene oxide solution, it is preferred that graphene solution and AgNWs concentration of aqueous solution, using spin coating proceeding, the stability that nano-silver thread adds in surface of graphene oxide ensure that.
Description
Technical field
The present invention relates to graphene composite material field, more particularly, to a kind of graphene/nano silver line electrically conducting transparent
Film and its preparation method and application.
Background technology
Graphene, is a kind of carbon atom by sp2 hydridization bonding in the form of hexagon grid, the two dimension of the carbon formed
Planar monolayer structure, it is the allotrope of carbon.Graphene is the elementary cell for building other dimension carbon materials, when it is with bag
When the mode wrapped up in, wind and piled up changes, the fullerene, one-dimensional CNT and three-dimensional stone of zero dimension can be formed respectively
Ink.Graphene has good electricity-optics performance, mechanical property, heat-conductive characteristic and the migration of high electric charge carrier
Rate, while also outstanding mechanical strength and pliability.These properties of graphene, it is allowed to be rapidly become by numerous concerns
The focus of research.The graphene and its derivative handled by chemical modification is even more the material with specific function, available for crystalline substance
Body pipe, liquid-crystal apparatus, electrochemica biological sensor, ultracapacitor, fuel cell, solar cell etc..
As the method that large area film is formed using graphene, that currently attempts has chemical vapor deposition (referred to as
CVD) method and redox solution method.Prior art CVD equipment level demand is high.In process of production, CVD is needed carbon
Then source high temperature deposition is shifted graphene film by the method for transfer in metal matrix surface.However, this method not only into
This height, and defect and hole are easily caused, have a strong impact on its transverse conductance efficiency.
Redox solution method can significantly reduce cost because do not need vacuum equipment, thus various countries to the field all
Stepping up to study.However, graphene obtained by redox solution method is redox graphene, its lamella is simultaneously discontinuous, is more
Layer graphene piece mutually mixes " the carbon cake " of composition, is existed using graphene film made of redox solution method and can not fully dropped
The problem of low film resistor, the redox graphene film are similar with common graphite film resistor and transparency even below existing
Ito thin film product.
Silver (0.63 × 106S/cm nature electric conductivity and electrical conductivity highest metal) are used as, thus preparation can be passed through
RGO/Ag composites improve RGO electric conductivity.Correlative study both at home and abroad is many at present, and Chinese patent CN102993995A is disclosed
Nano-silver thread is pressed in clear PET film table by a kind of preparation method of transparent conductive film, this method using the method for hot pressing
On face；This method technique is simple, and device therefor is cheap, but deficiency is that pressure sintering will heat, pressurize, and is easily formed after film forming
Bubble, film are easily deformed.Chinese patent CN102820074A discloses a kind of electrically-conductive backing plate and its system for photoelectric device
Preparation Method, to improve the electric conductivity of graphene conductive film in this method, one layer of nano-silver thread is addition of on its surface；Although this
Method can be effectively improved the electric conductivity of the film, but nano-silver thread is attached to film surface and is easier to come off, and the film does not have
The conductive component for being attached to surface is reinforced using other method, influences the stability of conductive film.
The content of the invention
The technical problems to be solved of the present invention are to be prepared into graphene film lamella for prior art oxidation-reduction method
Discontinuously, the problem of and technique of RGO/Ag composites is present, there is provided a kind of good dispersion single-layer graphene film and
The graphene/nano silver line electrically conducting transparent membrane preparation method be unlikely to deform, to come off.
The present invention also provides a kind of graphene/nano silver line nesa coating being prepared using the above method.
The purpose of the present invention is achieved by the following technical programs：
A kind of preparation method of graphene/nano silver line nesa coating is provided, comprised 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 graphene oxide water solution is obtained；
S3. glass substrate：Glass substrate is cleaned, after drying, be surface-treated using APTS, obtain APTS modifications
Glass substrate；
S4. spin coating：The APTS modified glass substrate obtained to step S3 progressively spin coating graphene oxide water solution, AgNWs
The aqueous solution, whole process are placed in atmosphere of inert gases, after obtained film vacuum is dried, are subsequently placed in hydrazine steam also
Original, finally film is heat-treated, obtains graphene/nano silver line nesa coating；
Wherein, the temperature of first time ultrasonic disperse is 30~50 DEG C in step S2, frequency is 10000~25000Hz, flow velocity
For 1.0~4.0m3/ h, circulation stirring speed are 1000~2000r/min, the ultrasonic disperse time is 0.5~2.0h；
The temperature of second of ultrasonic disperse is 30~50 DEG C, frequency is 18000~25000Hz, flow velocity is 2.0~5.0m3/
H, circulation stirring speed be 1000~2000r/min, the ultrasonic disperse time be 2~5h.
The present invention is disperseed by twice ultrasonic, obtains aqueous solution of single-layer grapheme oxide, the glass lined being modified using APTS
Bottom, graphene/nano silver line nesa coating is finally prepared by spin coating proceeding, is unlikely to deform, comes off.
Preferably, graphene oxide water solution described in step S2 is 0.02~0.04g/L.
Preferably, spin speed described in step S4 is 100~140rpm, time 10s.
Preferably, the AgNWs aqueous solution described in step S4 is 3.0~4mg/ml.
Preferably, inert gas described in step S4 is nitrogen, argon gas, the one or more of helium.
Preferably, the heat treatment of film described in step S4 refers to be heat-treated 1h at 200~220 DEG C.
Preferably, the recovery time described in step S4 is 24h.
Preferably, film vacuum drying temperature described in step S4 is 100~140 DEG C, and the time is 10~20min.
The present invention also provides a kind of graphene/nano silver line nesa coating being prepared using the above method, applies
In solar cell, flat-panel monitor or touch-screen field.
Compared with prior art, the beneficial effects of the invention are as follows：
Preparation technology of the present invention is simple, by twice ultrasonic decentralized processing, obtains finely dispersed single-layer graphene oxide
The aqueous solution, it is discontinuous, overlapping to solve the problems, such as that prior art oxidation-reduction method is prepared into graphene film lamella.
Graphene oxide of the present invention only needs to react in substrate of glass after modification, by APTS improve adhesive force without
Need to use other physical methods, and without secondary transferring graphene film, using finely dispersed single-layer graphene oxide
Solution, preferably graphene solution and AgNWs concentration of aqueous solution, using spin coating proceeding, it ensure that nano-silver thread in graphene oxide
The additional stability in surface.
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 17~23 Europe/square, light transmittance be higher than 91%, the composite is applied to solar-electricity
Pond, flat-panel monitor or touch-screen field, its application prospect are considerable.
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 a kind of graphene/nano silver line electrically conducting transparent membrane preparation method, 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 0.02g/L graphene oxide water solutions are obtained；
S3. glass substrate：Glass substrate is cleaned, after drying, be surface-treated using APTS, obtain APTS modifications
Glass substrate；
S4. spin coating：The graphene oxide that 0.2mg/ml is instilled on the APTS modified glass substrates that step S3 is obtained is water-soluble
Liquid, be then spin coated onto, spin speed 100rpm, time 10s, whole process is placed in atmosphere of inert gases, then 40~
5~10min is dried at 60 DEG C；The 3.0mg/ml AgNWs aqueous solution is coated in APTS modified glass substrates using the above method
On, obtained film is dried in vacuo, wherein drying temperature is 100 DEG C, time 20min, is subsequently placed in 100 DEG C of hydrazines and steams
Reductase 12 4h in vapour, finally film is carried out to be heat-treated 1h at 220 DEG C, obtains graphene/nano silver line nesa coating；
Wherein, the temperature of first time ultrasonic disperse is 30~50 DEG C in step S2, frequency is 10000~25000Hz, flow velocity
For 1.0~4.0m3/ h, circulation stirring speed are 1000~2000r/min, the ultrasonic disperse time is 0.5~2.0h；
The temperature of second of ultrasonic disperse is 30~50 DEG C, frequency is 18000~25000Hz, flow velocity is 2.0~5.0m3/
H, circulation stirring speed be 1000~2000r/min, the ultrasonic disperse time be 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：By 0.3MPVP and 0.2MNaCl
Mixed in reaction vessel and in 160 DEG C of heating.By 1MAgNO3It is added in mixture, then after 5 minutes, uses peristaltic pump
It is slowly added to 1MAgNO3；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
Two ultrasonic reaction kettles are identical with the first ultrasonic reaction kettle structure, and the upper end in the second batch mixing pond passes through the ultrasonic reaction of pipeline 11 and second
Kettle is connected, and lower end is connected with pipeline 12；Pipeline 12 is provided with charging aperture 13, centrifugal pump 14, the flow being connected with the first discharge port 8
The discharge port 16 of meter 15 and second, the second ultrasonic reaction kettle horizontal level is sequentially connected, and is provided with air bleeding valve, and passes through pipeline 17
It is connected with pipeline 12, 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.
Embodiment 2
The present embodiment provides a kind of graphene/nano silver line electrically conducting transparent membrane preparation method, 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 0.04g/L graphene oxide water solutions are obtained；
S3. glass substrate：Glass substrate is cleaned, after drying, be surface-treated using APTS, obtain APTS modifications
Glass substrate；
S4. spin coating：The graphene oxide that 0.3mg/ml is instilled on the APTS modified glass substrates that step S3 is obtained is water-soluble
Liquid, be then spin coated onto, spin speed 140rpm, time 10s, whole process is placed in atmosphere of inert gases, then 40~
5~10min is dried at 60 DEG C；The 4.0mg/ml AgNWs aqueous solution is coated in APTS modified glass substrates using the above method
On, obtained film is dried in vacuo, wherein drying temperature is 140 DEG C, time 10min, is subsequently placed in 100 DEG C of hydrazines and steams
Reductase 12 4h in vapour, finally film is carried out to be heat-treated 1h at 220 DEG C, obtains graphene/nano silver line nesa coating；
Wherein, the temperature of first time ultrasonic disperse is 30~50 DEG C in step S2, frequency is 10000~25000Hz, flow velocity
For 1.0~4.0m3/ h, circulation stirring speed are 1000~2000r/min, the ultrasonic disperse time is 0.5~2.0h；
The temperature of second of ultrasonic disperse is 30~50 DEG C, frequency is 18000~25000Hz, flow velocity is 2.0~5.0m3/
H, circulation stirring speed be 1000~2000r/min, the ultrasonic disperse time be 2~5h；
Inert gas is nitrogen, argon gas, the one or more of helium in step S4.
Comparative example 1
This comparative example is substantially the same manner as Example 1, and difference is, a ultrasonic disperse, temperature are used in step S2
Be 10000~25000Hz for 30~50 DEG C, frequency, flow velocity be 1.0~4.0m3/ h, circulation stirring speed are 1000~2000r/
Min, ultrasonic disperse time are 0.5~2.0h.
Comparative example 2
This comparative example is substantially the same manner as Example 1, a ultrasonic disperse is used in step S2, temperature is 30~50 DEG C, frequency
Rate is 18000~25000Hz, flow velocity is 2.0~5.0m3/ h, circulation stirring speed are 1000~2000r/min, ultrasonic disperse
Time is 2~5h.
Performance characterization
Four-point probe and ultraviolet specrophotometer testing film are used to embodiment 1~2 and comparative example 1~2
Electric conductivity and light transmittance, as a result as shown in table 1：
Table 1
| Embodiment | Sheet resistance (Europe/square) | Light transmittance (%) |
| Embodiment 1 | 23 | 91 |
| Embodiment 2 | 17 | 92 |
| Comparative example 1 | 47 | 78 |
| Comparative example 2 | 43 | 76 |
Claims (10)
1. a kind of preparation method of graphene/nano silver line nesa coating, 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：The graphene oxide twice ultrasonic soluble in water that carries out that step S1 is prepared disperses, then
Obtain graphene oxide water solution；
S3. glass substrate：Glass substrate is cleaned, after drying, be surface-treated using APTS, obtain APTS modified glass
Substrate；
S4. spin coating：Progressively spin coating graphene oxide water solution, AgNWs are water-soluble for the APTS modified glass substrate obtained to step S3
Liquid, whole process are placed in atmosphere of inert gases, after obtained film vacuum is dried, are subsequently placed in hydrazine steam and are reduced,
Finally film is heat-treated, obtains graphene/nano silver line nesa coating；
Wherein, the temperature of first time ultrasonic disperse is 30~50 DEG C in step S2, frequency is 10000~25000Hz, flow velocity is
1.0~4.0m3/ h, circulation stirring speed are 1000~2000r/min, the ultrasonic disperse time is 0.5~2.0h；
The temperature of second of ultrasonic disperse is 30~50 DEG C, frequency is 18000~25000Hz, flow velocity is 2.0~5.0m3/ h, follow
Ring mixing speed is 1000~2000r/min, the ultrasonic disperse time is 2~5h.
2. the preparation method of graphene/nano silver line nesa coating according to claim 1, it is characterised in that step S2
Described in graphene oxide water solution be 0.02~0.04g/L.
3. the preparation method of graphene/nano silver line nesa coating according to claim 1, it is characterised in that step S4
Described in spin speed be 100~140rpm, time 10s.
4. the preparation method of graphene/nano silver line nesa coating according to claim 1, it is characterised in that step S4
Described in the AgNWs aqueous solution be 3.0~4mg/ml.
5. the preparation method of graphene/nano silver line nesa coating according to claim 1, it is characterised in that step S4
Described in inert gas be nitrogen, argon gas, the one or more of helium.
6. the preparation method of graphene/nano silver line nesa coating according to claim 1, it is characterised in that step S4
Described in film heat treatment refer to be heat-treated 1h at 200~220 DEG C.
7. the preparation method of graphene/nano silver line nesa coating according to claim 1, it is characterised in that step S4
Described in the recovery time be 24h.
8. the preparation method of graphene/nano silver line nesa coating according to claim 1, it is characterised in that step S4
Described in film vacuum drying temperature be 100~140 DEG C, the time is 10~20min.
A kind of 9. graphene/nano silver line nesa coating, it is characterised in that the graphite as described in claim 1~8 any one
The preparation method of alkene/nano-silver thread nesa coating is prepared.
10. the application of graphene/nano silver line nesa coating according to claim 9, it is characterised in that applied to the sun
Can battery, flat-panel monitor or touch-screen field.
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| KR20190115639A (en) * | 2018-04-03 | 2019-10-14 | 비엔비머티리얼 주식회사 | Transparent heating film and preparation method thereof |
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Application publication date: 20180209 |