CN110536597A - A kind of novel light transmission electromagnetic protection film and preparation method thereof - Google Patents
A kind of novel light transmission electromagnetic protection film and preparation method thereof Download PDFInfo
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- CN110536597A CN110536597A CN201910788048.6A CN201910788048A CN110536597A CN 110536597 A CN110536597 A CN 110536597A CN 201910788048 A CN201910788048 A CN 201910788048A CN 110536597 A CN110536597 A CN 110536597A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
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- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
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- H05K9/00—Screening of apparatus or components against electric or magnetic fields
- H05K9/0073—Shielding materials
- H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
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Abstract
The invention discloses a kind of novel light transmission electromagnetic protection films and preparation method thereof, novel light transmission electromagnetic protection film, it is prepared in optical clear substrate, light transmission electromagnetic protection film is made of silver nanowires coating fluid, the silver nanowires coating fluid includes 100 parts of silver nanowires solution by parts by volume, 0.05-0.5 parts of dispersing agent, 0.05-0.5 parts of wetting agent, 0.05-0.5 parts of binder；Preparation method includes: the pretreatment of 1, substrate surface；2, silver nanowires film is prepared in substrate；3, novel light transmission electromagnetic protection film is made in silver nanowires film drying.Using a kind of novel light transmission electromagnetic protection film of the invention, good adhesive property and uniformity are had both.
Description
Technical field
The present invention relates to a kind of novel light transmission electromagnetic protection film and preparation method thereof, belong to electromagnetic shielding material design with
Preparation technical field.
Background technique
With the fast development of electronic information technology and the communication technology, being flooded with space, big energy is different, frequency spectrum letter
Electromagnetic wave abundant is ceased, serious electromagnetic pollution problem is produced, great threat is caused to electronic equipment and human health.Make
Spatially completely cut off electromagnetic wave with microwave defense material, reduce its influence to all kinds of electronics and human body, is a kind of important
Electromagnetic protection means.Currently, common microwave defense material has metal material, carbon-based material and conductive polymer material；However,
In some specific application scenes, due to the limitation of cost, weight, performance requirement, the use of these traditional materials is by biggish
Limitation；For example, all kinds of optical windows and television homing equipment, electromagnetic protection, which does not require nothing more than protective materials, has preferable shielding
Efficiency also has higher requirements to translucency.In addition, the fast development of 5G technology is the extensive use of all kinds of wearable electronics
Fertile soil is provided, while for the considerations of carrying out electromagnetic protection to human body, material is protected to flexibility, lightweight, transparent electromagnetic
Material also produces great demand.
Transparent conductive metal oxide film-indium oxide tin film (ITO) has high transparency, satisfactory electrical conductivity, prominent screen
The advantages that covering efficiency is the most widely used transparent conductive film material of current electronic field.However, a large amount of in recent years
Use, ito film exposes a large amount of disadvantages: (1) indium in ITO raw material belongs to rare metal and non-renewable, and price is increasingly
Valuableness gradually increases the manufacturing cost of ito thin film；(2) ito thin film is brittle, is not suitable for requiring the flexibility of material
Occasion；(3) preparation method of ito thin film has magnetron sputtering, chemical vapor deposition, vacuum reaction evaporation, pulsed laser deposition etc.,
Process is complex, and has high requirement, somewhat expensive to process control；(4) ITO has stronger water imbibition, is easy absorption
CO in air2Chemical change occurs with water, occurs " mildew ".Therefore, there is an urgent need to find a kind of new material ITO is replaced to make
For microwave defense material transparent, flexible.
Silver nanowires not only has the high conductivity of metallic silver itself as a kind of typical one-dimensional metal nano material,
There is nanometer size effect bring unique optical properties and surface plasmon resonance characteristic again, in photoelectricity, biology, sensing etc.
There is important application in field.The silver nanoparticle gauze being made of silver nanowires has conductivity is high, flexible, light transmission is excellent etc.
Plurality of advantages is a kind of ITO alternative materials of great potential；Domestic and international scientific research personnel shields material in the light transmission based on silver nanowires
A large amount of effort has also been made in preparation method for material, and under conditions of realizing light transmittance 80%, shield effectiveness can reach 25dB.
However, the light transmission electromagnetic protection film based on silver nanowires still has silver nanowires conductive film and substrate adhesion
Poor, the caducous problem of energy, and the inadequate problem of property not high and stable in the air there is also uniformity of film.
Summary of the invention
Goal of the invention of the invention is: in view of the above problems, providing a kind of novel light transmission electromagnetic protection film
And preparation method thereof, light transmission electromagnetic protection film prepared by the present invention has both good adhesive property and uniformity.
The technical solution adopted by the invention is as follows:
A kind of novel light transmission electromagnetic protection film, is prepared in optical clear substrate, the light transmission electromagnetic protection film packet
Silver nanowires, dispersing agent, wetting agent and binder are included, light transmission electromagnetic protection film is made to have both good adhesive property and uniformity.
In the above scheme, silver nanowires is main component, and dispersing agent can generate steric effect between silver nanowires, is hindered
The generation of silver nanowires agglomeration, so that finally formed film layer be made to be uniformly dispersed；Wetting agent can effectively reduce surface tension,
The generation for reducing film layer shrinkage cavity phenomenon caused by solvent volatilization during drying and forming-film simultaneously, improves film quality；Bonding agent exists
The adhesive capacity between film layer and substrate is significantly improved while playing solidification, while can effectively completely cut off air, prevents silver
Nano wire is oxidized and causes its performance degradation.To make light transmission electromagnetic protection film have both good adhesive property and uniformity.
Preferably, the optical clear substrate can be glass, polymethyl methacrylate (PMMA), polystyrene
(PS), one of polyethylene terephthalate (PET), polycarbonate (PC) etc..
Preferably, the light transmission electromagnetic protection film is made of silver nanowires coating fluid, the silver nanowires coating fluid
It include 100 parts of silver nanowires solution by parts by volume, 0.05-0.5 parts of dispersing agent, 0.05-0.5 parts of wetting agent, binder 0.05-
0.5 part.
Preferably, the concentration of the silver nanowires solution is 0.1-10mg/ml, wherein the diameter of silver nanowires is 1-
100nm, the length of silver nanowires are 0.5-100 μm.
Preferably, the silver nanowires solution is molten to disperse in deionized water obtained silver nanowires for silver nanowires
Liquid.
Preferably, the dispersing agent is water soluble dispersing agent.
Preferably, the dispersing agent is the copolymer of octyl phenyl polyoxyethylene ether and/or the affinity groups containing pigment.
Preferably, the octyl phenyl polyoxyethylene ether is the Tao Shi TX-100 of commercialization, the affine base containing pigment
The copolymer of group be that chemical KYC-913 is full of in the section being commercialized；Such dispersing agent is rapid with viscosity reduction for dispersing silver nanowires, flows
The good feature of dynamic property.
Preferably, the wetting agent is fluorine-containing non-silicon polymer；Fluorine-containing non-silicon polymer has good reduction surface
The effect of tension plays the role of good wetting action and prevents shrinkage cavity, also has good levelling ability, simultaneously because not
It is siliceous therefore it will not influence to the adhesive force of substrate and recoating performance.
Preferably, chemical KYC-643 is full of in the section that the fluorine-containing non-silicon polymer is commercialization；KYC-643 can effectively drop
Low surface tension, especially suitable for the substrate of low surface tension, and good water solubility, transparency is not influenced, anti-shrinkage cavity ability is excellent
It is different.
Preferably, the binder is soluble polyurethane.
Preferably, the manufacturing process of silver nanowires coating fluid are as follows: stir using blender silver nanowires solution
While mixing, dispersing agent is added thereto；After mixing evenly, wetting agent then is added into above-mentioned solution；Finally, to above-mentioned mixed
It closes in solution and bonding agent is added, stir evenly obtained silver nanowires coating fluid.
The preparation method of novel light transmission electromagnetic protection film as described above, comprising the following steps:
Step a: surface preparation is carried out to optical clear substrate；
Step b: the optical clear substrate Jing Guo surface preparation is placed on coating machine station, silver nanowires is applied
Cloth liquid is uniformly dripped in substrate top edge, and one row's coating fluid of drop spaced apart, and it is thin to start coating machine preparation silver nanowires
Film；
Step c: under vacuum conditions, by the drying of silver nanowires film and final molding, novel light transmission electromagnetic protection is made
Film.
Preferably, in step a, using deionized water, acetone and dehydrated alcohol mixed solution or plasma clean pair
Optical clear substrate surface is handled.
In the above scheme, surface preparation is carried out to optical clear substrate, to guarantee substrate surface cleaning free from admixture, together
When reduce substrate surface tension, allow coating fluid homogeneous film formation in optical clear substrate, be not in the disadvantages such as shrinkage cavity, shadow
Ring film quality.
Preferably, preparing silver nanowires film using bar knife coating in step b, by control coating fluid spacing, scrape
Knife up degree, scraper length and coating speed realize the control to silver nanowires film preparation.
Preferably, in step b, coating fluid spacing 10-100mm, 0.05 μm of -1mm of scraper height, scraper length 30-
600mm, blade coating speed 0.1-100mm/s.
In the above scheme, the control to silver nanowires film thickness may be implemented by controlling relevant parameter, and controls
The quality of forming film of silver nanowires film.
Preferably, film forming is dried using two-period form stoving process in step c, high temperature is dry again after first low temperature drying
It is dry.
In the above scheme, firstly, drying at a lower temperature, solvent is made slowly to volatilize, guarantees that silver nanowires film has
Enough time levelling guarantees that silver nanowires is uniformly distributed；Then, it dries at relatively high temperatures, keeps the binder in system abundant
The bonds well of film layer and substrate is realized in solidification while improving curing degree.
In conclusion by adopting the above-described technical solution, the beneficial effects of the present invention are:
(1) not only there is the novel light transmission electromagnetic protection film prepared good light transmittance and electromagnetic shielding outstanding to imitate
Can, also have many advantages, such as that uniformity is good, strong, flexible prominent with substrate adhesion, greatly film can be pushed from Lab Products
Move towards practical engineering application；
(2) in novel light transmission electromagnetic protection membrane-film preparation process, aqueous polyurethane is introduced in silver nanowires coating fluid
Binder, significantly improves novel light transmission electromagnetic protection film and substrate adhesion energy, while by silver nanowires and air exclusion,
It prevents from leading to performance degradation because of oxidation；
(3) introducing of dispersing agent can generate steric effect between silver nanowires, hinder the generation of agglomeration, make it
It is even and be steadily scattered in silver nanowires coating fluid, so that it is good to have finally obtained novel light transmission electromagnetic protection film
Uniformity；
(4) introducing of wetting agent, is effectively reduced surface tension, and silver nanowires coating fluid is made to be easier to spread in substrate surface
It opens, while during the drying and film forming process, reduces the generation of shrinkage cavity phenomenon in solvent volatilization process, further increase novel light transmission electricity
Magnetic protection film quality.
Detailed description of the invention
Examples of the present invention will be described by way of reference to the accompanying drawings, in which:
Fig. 1 is novel light transmission electromagnetic protection film preparation flow diagram；
Fig. 2 is the electromicroscopic photograph of novel light transmission electromagnetic protection film；
Fig. 3 is visible light (400-760nm) light transmittance curve figure of novel light transmission electromagnetic protection film；
Fig. 4 is electromagnet shield effect curve graph of the novel light transmission electromagnetic protection film in 8-12GHz frequency range；
Fig. 5 is the electromagnet shield effect curve graph that novel light transmission electromagnetic protection film different zones are tested；
Fig. 6 is that novel light transmission electromagnetic protection film places the electromagnet shield effect song tested for 1 year and obtained in atmospheric environment
Line comparison diagram.
Specific embodiment
All features disclosed in this specification or disclosed all methods or in the process the step of, in addition to mutually exclusive
Feature and/or step other than, can combine in any way.
Any feature disclosed in this specification unless specifically stated can be equivalent or with similar purpose by other
Alternative features are replaced.That is, unless specifically stated, each feature is an example in a series of equivalent or similar characteristics
.
As shown in Figure 1, a kind of preparation method of novel light transmission electromagnetic protection film, need to locate in advance by optical clear substrate
Reason prepares silver nanowires film in optical clear substrate, is dried in vacuo and light transmission electromagnetic protection film is made, specifically include following
Three steps:
Step a: using deionized water, acetone and dehydrated alcohol mixed solution or plasma clean to optical clear substrate
Carry out surface preparation；
Step b: the optical clear substrate Jing Guo surface preparation is placed on coating machine station, silver nanowires is applied
Cloth liquid is uniformly dripped in substrate top edge, and one row's coating fluid of drop spaced apart, and it is thin to start coating machine preparation silver nanowires
Film；
Step c: it is under vacuum conditions, silver nanowires film is dry using two-period form stoving process, novel light transmission is made
Electromagnetic protection film.
Wherein, silver nanowires coating fluid by the following components of parts by volume by being made: 100 parts of silver nanowires solution, dispersion
0.05-0.5 parts of agent, 0.05-0.5 parts of wetting agent, 0.05-0.5 parts of binder.
The concentration of silver nanowires solution is 0.1-10mg/ml, and wherein silver nanowires is made using chemical method, a diameter of
1-100nm, length are 0.5-100 μm；Silver nanowires solution is to disperse silver nanowires in deionized water aqueous silver is made to receive
Rice noodles solution.
Dispersing agent is the copolymer of octyl phenyl polyoxyethylene ether and/or the affinity groups containing pigment, is specifically commercialized
TX-100 and KYC-913；Wetting agent is fluorine-containing non-silicon polymer, the KYC-643 being specially commercialized；Binder is water-soluble poly
Urethane.
The manufacturing process of silver nanowires coating fluid are as follows: same being stirred using magnetic stirring apparatus to silver nanowires solution
When, dispersing agent is added thereto；After mixing evenly, wetting agent then is added into above-mentioned solution；Finally, to above-mentioned mixed solution
Middle addition bonding agent stirs evenly obtained silver nanowires coating fluid.
Embodiment 1
A kind of novel transparent electromagnetic protection film, by silver nanowires coating fluid at polyethylene terephthalate (PET)
Silver nanowires film is prepared in substrate, it is finally dry to be made.
Wherein, silver nanoparticle coating fluid includes 100 parts of silver nanowires solution by parts by volume, and 0.1 part of KYC-913 dispersing agent,
0.1 part of KYC-643 wetting agent, 0.2 part of soluble polyurethane；Silver nanowires solution is will be using length 25 made from chemical method
± 2 μm, the silver nanowires of 25 ± 2nm of diameter, are scattered in deionized water, form the silver nanowires solution that concentration is 1mg/ml.
The preparation method of novel transparent electromagnetic protection film, comprising the following steps:
PET base: being cut into the square of 340mm × 340mm by step a, is subsequently placed in deionized water, acetone and anhydrous second
It is ultrasonically treated 20min in alcohol mixed liquor (volume ratio 2:1:1), is then rinsed 3 times, is dried with nitrogen with deionized water；
Step b: surface treated PET base is placed on coating machine station, and coating fluid is uniformly dripped in base
Bottom top edge, and at interval of one row's coating fluid of 50mm drop；Set coating machine parameter, 50 μm of scraper height, scraper length
400mm, coating speed 20mm/s, starting coating machine are coated preparation silver nanowires film；
Step c: it after silver nanowires film preparation is good, is transferred in two-period form vacuum drying oven and is dried；Firstly, In
2h is toasted under the conditions of 100 DEG C, then toasts 30min under the conditions of 120 DEG C, and novel light transmission electromagnetic protection film is made.
In another embodiment, silver nanoparticle coating fluid includes 100 parts of silver nanowires solution by parts by volume, TX-100 dispersing agent
0.05 part, 0.05 part of KYC-643 wetting agent, 0.05 part of soluble polyurethane；Silver nanowires solution is that will use chemical method system
15 ± 2 μm of length, the silver nanowires of 20 ± 2nm of diameter obtained, is scattered in deionized water, forms the silver that concentration is 0.5mg/ml
Nanowire solution；Optical clear substrate is glass.
In another embodiment, silver nanoparticle coating fluid includes 100 parts of silver nanowires solution by parts by volume, KYC-913 dispersion
0.5 part of agent, 0.5 part of KYC-643 wetting agent, 0.5 part of soluble polyurethane；Silver nanowires solution is that will be made using chemical method
100 ± 10 μm of length, the silver nanowires of 100 ± 5nm of diameter, be scattered in deionized water, formed concentration be 3mg/ml silver
Nanowire solution；Optical clear substrate is PMMA substrate.
As shown in Fig. 2, for the electromicroscopic photograph of novel light transmission electromagnetic protection film is made, it can be seen that novel light transmission obtained
Electromagnetic protection film has good uniformity.
Adhesion strength test is carried out to novel light transmission electromagnetic protection film obtained, stripping area reaches 4B grades less than 5%
Not, show that the adhesiveness between the novel light transmission electromagnetic protection film and substrate is good, reach requirement.
As shown in figure 3, light transmission features characterization is carried out to the novel light transmission electromagnetic protection film being prepared, using model
The UV-Vis spectrometer of UV-2700 tests the novel light transmission electromagnetic protection film in the saturating of visible region (400-760nm)
Light rate, it can be seen from the figure that the light transmittance of 550nm green light is up to 84%.
As shown in figure 4, carrying out electromagnet shield effect test to the novel light transmission electromagnetic protection film being prepared, can see
Out, novel light transmission electromagnetic protection film electromagnet shield effect in 8-12GHz frequency range is greater than 25dB.
As shown in figure 5, for the novel light transmission electromagnetic protection film of preparation, to the shield effectiveness of its 6 different zones into
Row test characterization, the electromagnet shield effect of novel light transmission electromagnetic protection film different zones is almost the same, further demonstrates new
Type light transmission electromagnetic protection film has good uniformity.
Fig. 6 is that freshly prepd novel light transmission electromagnetic protection film and the novel light transmission electromagnetism being placed in 1 year in atmospheric environment are prevented
Protect the electromagnet shield effect comparison diagram of film, it can be seen that novel light transmission electromagnetic protection membrane shield performance is more stable, big
It is placed 1 year in compression ring border, electromagnet shield effect is basically unchanged.
In conclusion using a kind of novel light transmission electromagnetic protection film of the invention, not only have good light transmittance with
Electromagnet shield effect outstanding also has many advantages, such as that uniformity is good, strong, flexible prominent with substrate adhesion, can greatly push
Film moves towards practical engineering application from Lab Products；In novel light transmission electromagnetic protection membrane-film preparation process, in silver nanowires
Waterborne polyurethane binders are introduced in coating fluid, significantly improve novel light transmission electromagnetic protection film and substrate adhesion energy, together
When by silver nanowires and air exclusion, prevent from leading to performance degradation because of oxidation；The introducing of dispersing agent can produce between silver nanowires
Raw steric effect, hinders the generation of agglomeration, is scattered in it uniformly and stably in silver nanowires coating fluid, to make most
The novel light transmission electromagnetic protection film obtained eventually has good uniformity；The introducing of wetting agent, is effectively reduced surface tension, makes
Silver nanowires coating fluid is easier to spread out in substrate surface, while during the drying and film forming process, reducing and contracting in solvent volatilization process
The generation of hole phenomenon further increases novel light transmission electromagnetic protection film quality.
The invention is not limited to specific embodiments above-mentioned.The present invention, which expands to, any in the present specification to be disclosed
New feature or any new combination, and disclose any new method or process the step of or any new combination.
Claims (10)
1. a kind of novel light transmission electromagnetic protection film, is prepared in optical clear substrate, it is characterised in that: the light transmission electromagnetism is anti-
Shield film includes silver nanowires, dispersing agent, wetting agent and binder, make light transmission electromagnetic protection film have both good adhesive property and
Uniformity.
2. novel light transmission electromagnetic protection film as described in claim 1, it is characterised in that: the light transmission electromagnetic protection film by
Silver nanowires coating fluid is made, and the silver nanowires coating fluid includes 100 parts of silver nanowires solution by parts by volume, dispersing agent
0.05-0.5 parts, 0.05-0.5 parts of wetting agent, 0.05-0.5 parts of binder.
3. novel light transmission electromagnetic protection film as claimed in claim 2, it is characterised in that: the concentration of the silver nanowires solution
For 0.1-10mg/ml, wherein the diameter of silver nanowires is 1-100nm, and the length of silver nanowires is 0.5-100 μm.
4. novel light transmission electromagnetic protection film as described in claim 1, it is characterised in that: the dispersing agent is poly- for octyl phenyl
The copolymer of ethylene oxide ether and/or the affinity groups containing pigment.
5. novel light transmission electromagnetic protection film as described in claim 1, it is characterised in that: the wetting agent is poly- for fluorine-containing non-silicon
Close object.
6. novel light transmission electromagnetic protection film as described in claim 1, it is characterised in that: the binder is water-soluble poly ammonia
Ester.
7. the preparation method of novel light transmission electromagnetic protection film as claimed in any one of claims 1 to 6, it is characterised in that including
Following steps:
Step a: surface preparation is carried out to optical clear substrate；
Step b: the optical clear substrate Jing Guo surface preparation is placed on coating machine station, by silver nanowires coating fluid
Uniformly drop is in substrate top edge, and one row's coating fluid of drop spaced apart, starting coating machine prepare silver nanowires film；
Step c: under vacuum conditions, by the drying of silver nanowires film and final molding, novel light transmission electromagnetic protection film is made.
8. novel light transmission electromagnetic protection film as claimed in claim 7 and preparation method thereof, it is characterised in that: in step a, adopt
Optical clear substrate surface is handled with deionized water, acetone and dehydrated alcohol mixed solution or plasma clean.
9. novel light transmission electromagnetic protection film as claimed in claim 7 and preparation method thereof, it is characterised in that: in step b, adopt
Silver nanowires film is prepared with bar knife coating, it is real by control coating fluid spacing, scraper height, scraper length and coating speed
Now to the control of silver nanowires film preparation.
10. novel light transmission electromagnetic protection film as claimed in claim 7 and preparation method thereof, it is characterised in that: in step c,
Film forming is dried using two-period form stoving process, high temperature drying again after first low temperature drying.
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| CN2019107282016 | 2019-08-08 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1461779A (en) * | 2002-04-19 | 2003-12-17 | 捷时雅株式会社 | Substance for forming electrically-conducting film and electrically-conducting film and its manufacturing method |
| US20100147563A1 (en) * | 2008-12-11 | 2010-06-17 | Samsung Electro Mechanics Co., Ltd. | Substrate having electromagnetic shielding member |
| CN109021710A (en) * | 2018-08-02 | 2018-12-18 | 电子科技大学中山学院 | Nano silver wire conductive ink, preparation method and preparation method of transparent conductive film |
| CN109273168A (en) * | 2018-09-05 | 2019-01-25 | 中国工程物理研究院应用电子学研究所 | Have both the preparation method of composite film of high transparency Yu excellent electromagnetic shield effectiveness |
-
2019
- 2019-08-26 CN CN201910788048.6A patent/CN110536597B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1461779A (en) * | 2002-04-19 | 2003-12-17 | 捷时雅株式会社 | Substance for forming electrically-conducting film and electrically-conducting film and its manufacturing method |
| US20100147563A1 (en) * | 2008-12-11 | 2010-06-17 | Samsung Electro Mechanics Co., Ltd. | Substrate having electromagnetic shielding member |
| CN109021710A (en) * | 2018-08-02 | 2018-12-18 | 电子科技大学中山学院 | Nano silver wire conductive ink, preparation method and preparation method of transparent conductive film |
| CN109273168A (en) * | 2018-09-05 | 2019-01-25 | 中国工程物理研究院应用电子学研究所 | Have both the preparation method of composite film of high transparency Yu excellent electromagnetic shield effectiveness |
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