CN109273168A - Have both the preparation method of composite film of high transparency Yu excellent electromagnetic shield effectiveness - Google Patents
Have both the preparation method of composite film of high transparency Yu excellent electromagnetic shield effectiveness Download PDFInfo
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- CN109273168A CN109273168A CN201811029842.4A CN201811029842A CN109273168A CN 109273168 A CN109273168 A CN 109273168A CN 201811029842 A CN201811029842 A CN 201811029842A CN 109273168 A CN109273168 A CN 109273168A
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- H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
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Abstract
The invention discloses a kind of Novel compound film preparation method for having both high transparency Yu excellent electromagnetic shield effectiveness, include the following steps: Step 1: substrate surface is handled；Step 2: preparation silver nanowires, and prepare silver nanowires dispersion liquid；Step 3: bar knife coating prepares silver nanowires transparent conductive film；Step 4: silver nanowires film surface acid is handled；Step 5: substrate obtained in step 4 is placed on sol evenning machine first, PEDOT:PSS is uniformly coated on substrate surface, it is post-processed using laminated film of the DBSA to drying and forming-film, then repeatedly revolve with DBSA of the deionized water to laminated film surface and wash and dry, obtain silver nanowires-(PEDOT:PSS) laminated film.Silver nanowires-(PEDOT:PSS) laminated film being prepared using the method for the present invention, have the characteristics that light transmittance is high, electromagnet shield effect is prominent, conformability is good, solves traditional shielding material in aerospace system electromagnetic compatibility and security application limitation problem.
Description
Technical field
The invention belongs to electromagnetic shielding material design and preparation technical field, and in particular to one kind have both high transparency with it is excellent
The Novel compound film preparation method of different electromagnet shield effect.
Background technique
Now, a large amount of dual-use high powered radar, communication equipments at work to space radiate various frequencies it is different,
The different electromagnetic wave of energy, keeps space electromagnetic environment more and more severe；At the same time, the number of electronic devices in system is being in
Exponential form increases, and system electromagnetic susceptibility is caused to be promoted, and easy broken down by Electromagnetic Interference even can not be normal
Work；It needs to carry out electromagnetic protection research.
Shield technology is one of the key technology of electromagnetic protection design, and it is to influence shielding skill that shielding material, which is chosen with preparation,
The key link of art validity and implementation.According to the difference of conductivity, existing mainstream electromagnetic shielding material can be divided into metal
Material, carbon-based material and conductive polymer material etc..Metal material has the characteristics that conductivity is high, skin depth is shallow, main logical
Reflection loss is crossed to realize that electromagnetic shielding, shield effectiveness are good；However its weight is big, opaque, in some systems, is especially navigating
Empty aerospace system, application are extremely restricted.Carbon-based material is from a wealth of sources, it is (heat resistance, resistance to prepare simple, environmental suitability
Corrosion) it is good, but electric conductivity is poor, modifying process is complicated, translucency is poor, electromagnetic shielding capability is general.Conductive polymer material,
Such as: polyacetylene, polypyrrole, polyaniline, polythiophene have the characteristics that light-weight, good toughness, at low cost, light transmittance is high, are more
It ideal electromagnetic shielding material and has been a great concern in recent years.
However, undoped conductive polymer material conductivity is low, effectiveness is poor, it is difficult to meet practical application
Demand；To improve conductive polymer material electromagnet shield effect, it is carried out to compound, realization mutual supplement with each other's advantages with other materials, into
And improve its electromagnetic shielding capability；But then, the composite material transmittancy after doping vario-property sharply declines.In short, mesh
Preceding existing mainstream electromagnetic shielding material is difficult to have both the two-fold advantage of high transparency Yu excellent electromagnetic shield effectiveness；High transparency
With can not getting both in electromagnetic shielding material like fish and bear's paw for superior barrier efficiency.
In all metals, silver has highest conductivity；In addition, silver nanowires has very high draw ratio, easily formed
Conductive network.In recent years, silver nanowires is successfully synthesized out, the cross-linked network being made of silver nanowires have conductivity it is high,
The characteristics of optical clear (visible light transmittance > 90%), be expected to substitution tin indium oxide and as transparent electrode.Poly- 3,4- ethylene two
Oxygen thiophene: kayexalate (PEDOT:PSS) is a kind of conductive polymer material with high transparency.
Summary of the invention
To overcome conventional electromagnetic shielding material to be difficult to the drawbacks of being provided simultaneously with high transparency and superior barrier efficiency, the present invention
It proposes to carry out silver nanowires and PEDOT:PSS compound, prepares that a kind of light transmittance is high, electromagnet shield effect protrusion, conformability
Good Novel compound film solves traditional shielding material in aerospace system electromagnetic compatibility and security application limitation problem, is
Electromagnetic protection design provides new material selection.
The present invention to achieve the above object, is achieved through the following technical solutions:
A kind of preparation method of composite film having both high transparency Yu excellent electromagnetic shield effectiveness, it is characterised in that including walking as follows
It is rapid:
Step 1: choosing, there is the material of optical transparent properties to handle as substrate, and to the surface of substrate, for mentioning
Rise the adhesive force of silver nanowires and substrate；
Step 2: silver nanowires is distributed in the mixed solution of water and isopropanol, silver nanowires dispersion liquid is obtained, and to silver
Nanowire dispersion is deposited；
Step 3: by treated in step 1, substrate is laid on station, then silver nanowires obtained in step 2 is divided
Dispersion liquid is uniformly dripped at the top edge of substrate, then prepares silver nanowires transparent conducting thin film by bar knife coating；
Step 4: carrying out sour processing to silver nanowires transparent conducting thin film obtained in step 3: silver will be coated in step 3
The substrate tilt of nano wire film is placed, and hydrochloric acid solution is made to flow through entire silver nanowires transparent conducting thin film region naturally；
Step 5: substrate obtained in step 4 is placed on sol evenning machine first, PEDOT:PSS is uniformly coated on substrate table
Face, film forming to be dried obtains laminated film, then is post-processed using dodecyl benzene sulfonic acid (DBSA) to laminated film, then
Repeatedly revolve with DBSA of the deionized water to laminated film surface and wash and dry, it is compound to obtain silver nanowires-(PEDOT:PSS)
Film.
In the above-mentioned technical solutions, the substrate surface in step 1 is handled as follows:
A, substrate is cut into fritter；
B, the substrate after cutting is sequentially placed into acetone, in dehydrated alcohol, and is surpassed respectively in acetone and dehydrated alcohol
Sonication；
C, deionized water flushing and drying are carried out to the substrate after ultrasonic treatment；
D, the substrate surface after drying is cleaned, using one of pickling, alkali cleaning, plasma clean mode or more
Kind；
E, the substrate of surface treatment completion is obtained after carrying out cleaning, drying to the substrate after cleaning by deionized water.
In the above-mentioned technical solutions, the substrate can select glass, polyethylene, polyethylene terephthalate, gather
One of carbonic ester etc..
In the above-mentioned technical solutions, the silver nanowires in step 2 is prepared using chemical method, the silver nanoparticle of preparation
0.5 ~ 100 μm of 1 ~ 100nm of linear diameter, length；The volume ratio of water and isopropanol is 0.1 ~ 10 in mixed solution, silver nanowires solution
0.1 ~ 10mg/ml of concentration.
In the above-mentioned technical solutions, the bar in step 3 is Meyer stick, the blade coating speed of the bar is 0.1 ~
100mm/s。
In the above-mentioned technical solutions, the concentration of hydrochloric acid solution in step 4 is 0.1 ~ 5mol/L.
In the above-mentioned technical solutions, the ratio of the PEDOT in the PEDOT:PSS in step 5 and PSS is 1:1 ~ 1:10,
The spin-coating time of PEDOT:PSS is 10s ~ 10min, and DBSA handles 5 ~ 120min of time to laminated film；Further, it can be used
Isopropanol is diluted the PEDOT:PSS for preparing spin coating, and the volume ratio of isopropanol and PEDOT:PSS are 1:10 ~ 10:1.
In conclusion by adopting the above-described technical solution, the invention has the following advantages:
PEDOT:PSS itself has certain conductive capability, therefore imitate with certain shielding as a kind of transparent material
Can, however its own is relied only on, screening ability is very limited, and the present invention is excellent after making full use of silver nanowires to be crosslinked networking to be led
Electrically, translucency and the good translucency of conductive polymer material PEDOT:PSS, preparing a kind of has high transparency, excellent
Silver nanowires-(PEDOT:PSS) New Type of Composite Film Material of different electromagnet shield effect and conformal ability.It on the one hand, can be with
The advantages of PEDOT:PSS and silver nanowires, is combined, the electromagnetic shielding THIN COMPOSITE for having both conformal ability and high transparency is prepared
Film；On the other hand, PEDOT:PSS can effectively completely cut off silver nanowires and air, protect it from being oxidized.Novel compound film can
Meet the pressing needs of window electromagnetic protection in recent years, such as aircraft aircraft window, automotive window and Important building/place window
Electromagnetic protection fills up the technological gap of high light transmission microwave defense material design and preparation to a certain extent.
Detailed description of the invention
Fig. 1 is silver nanowires-of the present invention (PEDOT:PSS) Novel compound film preparation flow schematic diagram.
Fig. 2 is silver nanowires-(PEDOT:PSS) the Novel compound film scanning electricity being prepared using method of the invention
Mirror photo.
Fig. 3 is silver nanowires-(PEDOT:PSS) the Novel compound film visible light being prepared using method of the invention
(400 ~ 760nm) light transmittance curve.
Fig. 4 is silver nanowires-(PEDOT:PSS) Novel compound film that is prepared using method of the invention in X wave
The electromagnet shield effect of section (8 ~ 12GHz).
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.
As shown in Figure 1, a kind of preparation method of composite film for having both high transparency Yu excellent electromagnetic shield effectiveness, need through
Cross that substrate surface processing, preparation silver nanowires and configuration silver nanowires dispersion liquid, silver nanowires is transparent leads for the preparation of bar knife coating
Conductive film, silver nanowires transparent conductive film surface acid etching, PEDOT:PSS coating, DBSA handle laminated film, are done
Silver nanowires-(PEDOT:PSS) laminated film is obtained after dry, specifically includes following five steps:
Step 1: choosing, there is the material of optical transparent properties to handle as substrate, and to the surface of substrate, for mentioning
Rise the adhesive force of silver nanowires and substrate；
Wherein, substrate can select one of glass, polyethylene, polyethylene terephthalate, polycarbonate etc., place
Reason process are as follows:
A, substrate is cut into fritter；
B, the substrate after cutting is sequentially placed into acetone, in dehydrated alcohol, and is surpassed respectively in acetone and dehydrated alcohol
Sonication；
C, deionized water flushing and drying are carried out to the substrate after ultrasonic treatment；
D, the substrate surface after drying is cleaned, using one of pickling, alkali cleaning, plasma clean mode or more
Kind；
E, the substrate of surface treatment completion is obtained after carrying out cleaning, drying to the substrate after cleaning by deionized water.
Step 2: silver nanowires is distributed in the mixed solution of water and isopropanol, silver nanowires dispersion liquid is obtained, and
Silver nanowires dispersion liquid is deposited；
Wherein, silver nanowires is prepared using chemical method, 1 ~ 100nm of silver nanowires diameter, 0.5 ~ 100 μ of length of preparation
m；The volume ratio of water and isopropanol is 0.1 ~ 10 in mixed solution, 0.1 ~ 10mg/ml of silver nanowires solution concentration.
Step 3: by treated in step 1, substrate is laid on station, then by silver nanoparticle obtained in step 2
Line homogeneous dispersion drips at the top edge of substrate, then prepares silver nanowires transparent conducting thin film by bar knife coating；
Wherein, the blade coating speed of bar is 0.1 ~ 100mm/s.
Step 4: carrying out sour processing to silver nanowires transparent conducting thin film obtained in step 3: will be coated in step 3
There is the substrate tilt of silver nanowires film to place, hydrochloric acid solution is made to flow through entire silver nanowires transparent conducting thin film region naturally；
Wherein, concentration of hydrochloric acid solution is 0.1 ~ 5mol/L.
Step 5: substrate obtained in step 4 is placed on sol evenning machine first, PEDOT:PSS is uniformly coated on substrate
Surface, film forming to be dried obtains laminated film, then is post-processed using DBSA to laminated film, then with deionized water to multiple
The DBSA for closing film surface carries out repeatedly rotation and washes and dry, and obtains silver nanowires-(PEDOT:PSS) laminated film；
Wherein, the ratio of the PEDOT in the PEDOT:PSS in step 5 and PSS is 1:1 ~ 1:10, when the spin coating of PEDOT:PSS
Between be 10s ~ 10min, DBSA to laminated film handle 5 ~ 120min of time；Further, isopropanol can be used to preparation spin coating
PEDOT:PSS is diluted, and the volume ratio of isopropanol and PEDOT:PSS are 1:10 ~ 10:1.
Embodiment
A kind of preparation method of composite film having both high transparency Yu excellent electromagnetic shield effectiveness, as shown in Figure 1, using poly- to benzene
Naphthalate (PET) substrate is sequentially placed into third after PET base to be cut into the fritter that size is 100mm × 100mm
In ketone and dehydrated alcohol, ultrasonic treatment 30min is carried out respectively, after then rinsing, drying up by deionized water, using oxygen plasma
Body cleaning machine is surface-treated 10min to PET base, obtains surface after carrying out cleaning, drying to substrate finally by deionized water
Handle the substrate completed.
Meanwhile using chemical method prepare 25 ± 3 μm of length, the silver nanowires of 30 ± 2nm of diameter, be scattered in water and
In the mixed solution of isopropanol (volume ratio of water and isopropanol is 1:1), silver nanowires concentration is 1mg/ml in mixed solution.?
After completing PET base surface treatment and the preparation of silver nanowires solution, PET base is laid on station, silver nanowires is deposited,
Silver nanowires solution is uniformly dripped into side edge on the pet substrate, solution is then paved into blade coating film forming with Meyer stick, obtains Yin Na
Rice noodles film, the blade coating speed of Meyer stick are 20mm/s.
For the electric conductivity and light transmittance for further promoting silver nanowires film, use concentration for the hydrochloric acid solution of 0.5mol/L
Silver nanowires film is handled；It is coated with the PET base slant setting of silver nanowires film, makes hydrochloric acid from base top
Entire silver nanowires thin membrane regions are flowed through to substrate bottom natural, silver nanoparticle is improved by the chemical action of hydrochloric acid and silver nanowires
Overlap joint effect between line.
Then it places the substrate above on sol evenning machine, 1:1, the PEDOT:PSS solution after v/v dilution will be carried out by isopropanol
It uniformly is spin-coated on substrate surface, the volume ratio of PEDOT and PSS in PEDOT:PSS solution are 1:2.5, spin speed 500r/
Min, spin-coating time 2min, then drying and forming-film, obtains laminated film；Finally laminated film is post-processed using DBSA,
The processing time is 30min, then repeatedly revolve with DBSA of the deionized water to laminated film surface and wash, and be can be obtained after dry
Light rate height, conducting wire silver nanowires-of good performance (PEDOT:PSS) laminated film, as shown in Fig. 2.
Light transmission features characterization is carried out to silver nanowires-(PEDOT:PSS) laminated film being prepared, using model
The UV-Vis spectrometer of UV-2700 test silver nanowires-(PEDOT:PSS) laminated film visible region (400 ~
Light transmittance 760nm), test results are shown in figure 3, it can be seen from the figure that the light transmittance of 550nm green light is up to 90%.
Electromagnet shield effect test, test result are carried out to silver nanowires-(PEDOT:PSS) laminated film being prepared
As shown in Figure 4, it can be seen that silver nanowires-(PEDOT:PSS) laminated film is imitated in the electromagnetic shielding of X-band (8 ~ 12GHz)
25dB can be greater than.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (7)
1. having both the preparation method of composite film of high transparency Yu excellent electromagnetic shield effectiveness, it is characterised in that including walking as follows
It is rapid:
Step 1: choosing, there is the material of optical transparent properties to handle as substrate, and to the surface of substrate, for mentioning
Rise the adhesive force of silver nanowires and substrate；
Step 2: silver nanowires is distributed in the mixed solution of water and isopropanol, silver nanowires dispersion liquid is obtained, and to silver
Nanowire dispersion is deposited；
Step 3: by treated in step 1, substrate is laid on station, then silver nanowires obtained in step 2 is divided
Dispersion liquid is uniformly dripped at the top edge of substrate, then prepares silver nanowires transparent conducting thin film by bar knife coating；
Step 4: carrying out sour processing to silver nanowires transparent conducting thin film obtained in step 3: silver will be coated in step 3
The substrate tilt of nano wire film is placed, and hydrochloric acid solution is made to flow through entire silver nanowires transparent conducting thin film region naturally；
Step 5: substrate obtained in step 4 is placed on sol evenning machine first, PEDOT:PSS is uniformly coated on substrate table
Face, film forming to be dried obtains laminated film, then is post-processed using DBSA to laminated film, then with deionized water to compound
The DBSA of film surface carries out repeatedly rotation and washes and dry, and obtains silver nanowires-(PEDOT:PSS) laminated film.
2. the preparation method of composite film according to claim 1 for having both high transparency Yu excellent electromagnetic shield effectiveness,
It is characterized in that the substrate surface in step 1 is handled as follows:
Substrate is cut into fritter；
Substrate after cutting is sequentially placed into acetone, in dehydrated alcohol, and carries out ultrasound respectively in acetone and dehydrated alcohol
Processing；
Deionized water flushing and drying are carried out to the substrate after ultrasonic treatment；
Substrate surface after drying is cleaned, using one of pickling, alkali cleaning, plasma clean mode or a variety of；
The substrate of surface treatment completion is obtained after carrying out cleaning, drying to the substrate after cleaning by deionized water.
3. the preparation method of composite film according to claim 1 for having both high transparency Yu excellent electromagnetic shield effectiveness, special
Sign is that the substrate can select one of glass, polyethylene, polyethylene terephthalate, polycarbonate etc..
4. the preparation method of composite film according to claim 1 for having both high transparency Yu excellent electromagnetic shield effectiveness,
It is characterized in that the silver nanowires in step 2 is prepared using chemical method, 1 ~ 100nm of silver nanowires diameter of preparation, length
0.5~100μm；The volume ratio of water and isopropanol is 0.1 ~ 10 in mixed solution, 0.1 ~ 10mg/ml of silver nanowires solution concentration.
5. the preparation method of composite film according to claim 1 for having both high transparency Yu excellent electromagnetic shield effectiveness,
The bar being characterized in that in step 3 is Meyer stick, and the blade coating speed of the bar is 0.1 ~ 100mm/s.
6. the preparation method of composite film according to claim 1 for having both high transparency Yu excellent electromagnetic shield effectiveness,
The concentration of hydrochloric acid solution being characterized in that in step 4 is 0.1 ~ 5mol/L.
7. the preparation method of composite film according to claim 1 for having both high transparency Yu excellent electromagnetic shield effectiveness,
The ratio of the PEDOT and PSS that are characterized in that in the PEDOT:PSS in step 5 are 1:1 ~ 1:10, the spin-coating time of PEDOT:PSS
5 ~ 120min of time is handled to laminated film for 10s ~ 10min, DBSA；Further, can be used isopropanol to PEDOT:PSS into
The volume ratio of row dilution, isopropanol and PEDOT:PSS are 1:10 ~ 10:1.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110299222A (en) * | 2019-07-29 | 2019-10-01 | 中国工程物理研究院应用电子学研究所 | A kind of visible transparent conductive film and preparation method thereof |
| CN110364303A (en) * | 2019-07-04 | 2019-10-22 | 武汉纺织大学 | A kind of transparent conductive film and preparation method thereof |
| CN110536597A (en) * | 2019-08-08 | 2019-12-03 | 中国工程物理研究院应用电子学研究所 | A kind of novel light transmission electromagnetic protection film and preparation method thereof |
| CN111312434A (en) * | 2020-02-27 | 2020-06-19 | 北京化工大学 | Metal nanowire-based multilayer-structure transparent electromagnetic shielding film and preparation method and application thereof |
| CN111508851A (en) * | 2020-05-06 | 2020-08-07 | 济南南知信息科技有限公司 | Semiconductor structure and forming method thereof |
| CN111809439A (en) * | 2020-06-30 | 2020-10-23 | 陕西科技大学 | Flexible high-strength MXene-based electromagnetic shielding composite film and preparation method thereof |
| CN112778524A (en) * | 2020-12-30 | 2021-05-11 | 江苏慧智新材料科技有限公司 | Polyamide-imide resin and transparent acid-base-resistant electromagnetic shielding composite film prepared from same |
| CN112930100A (en) * | 2021-01-20 | 2021-06-08 | 中国电子科技集团公司第三十三研究所 | Metal transparentized electromagnetic shielding material and preparation method thereof |
| WO2022006655A1 (en) * | 2020-07-06 | 2022-01-13 | Uti Limited Partnership | Film for deicing and electromagnetic interference shielding applications |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110364303A (en) * | 2019-07-04 | 2019-10-22 | 武汉纺织大学 | A kind of transparent conductive film and preparation method thereof |
| CN110299222A (en) * | 2019-07-29 | 2019-10-01 | 中国工程物理研究院应用电子学研究所 | A kind of visible transparent conductive film and preparation method thereof |
| CN110536597A (en) * | 2019-08-08 | 2019-12-03 | 中国工程物理研究院应用电子学研究所 | A kind of novel light transmission electromagnetic protection film and preparation method thereof |
| CN111312434B (en) * | 2020-02-27 | 2021-05-04 | 北京化工大学 | Metal nanowire-based multilayer-structure transparent electromagnetic shielding film and preparation method and application thereof |
| CN111312434A (en) * | 2020-02-27 | 2020-06-19 | 北京化工大学 | Metal nanowire-based multilayer-structure transparent electromagnetic shielding film and preparation method and application thereof |
| CN111508851A (en) * | 2020-05-06 | 2020-08-07 | 济南南知信息科技有限公司 | Semiconductor structure and forming method thereof |
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| CN111809439A (en) * | 2020-06-30 | 2020-10-23 | 陕西科技大学 | Flexible high-strength MXene-based electromagnetic shielding composite film and preparation method thereof |
| CN111809439B (en) * | 2020-06-30 | 2022-05-20 | 陕西科技大学 | Flexible high-strength MXene-based electromagnetic shielding composite film and preparation method thereof |
| WO2022006655A1 (en) * | 2020-07-06 | 2022-01-13 | Uti Limited Partnership | Film for deicing and electromagnetic interference shielding applications |
| CN112778524A (en) * | 2020-12-30 | 2021-05-11 | 江苏慧智新材料科技有限公司 | Polyamide-imide resin and transparent acid-base-resistant electromagnetic shielding composite film prepared from same |
| CN112778524B (en) * | 2020-12-30 | 2023-11-10 | 江苏慧智新材料科技有限公司 | Polyamide-imide resin and transparent acid-alkali-resistant electromagnetic shielding composite film prepared from same |
| CN112930100A (en) * | 2021-01-20 | 2021-06-08 | 中国电子科技集团公司第三十三研究所 | Metal transparentized electromagnetic shielding material and preparation method thereof |
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