CN105810364A - Processing method for silver nanowire conductive thin film - Google Patents
Processing method for silver nanowire conductive thin film Download PDFInfo
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- CN105810364A CN105810364A CN201610312744.6A CN201610312744A CN105810364A CN 105810364 A CN105810364 A CN 105810364A CN 201610312744 A CN201610312744 A CN 201610312744A CN 105810364 A CN105810364 A CN 105810364A
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- nano silver
- silver wire
- conductive film
- processing method
- wire conductive
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 71
- 238000003672 processing method Methods 0.000 title claims abstract description 17
- 239000002042 Silver nanowire Substances 0.000 title claims abstract description 10
- 239000010409 thin film Substances 0.000 title abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 230000001476 alcoholic effect Effects 0.000 claims description 15
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 12
- 239000002253 acid Substances 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 8
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 6
- 229910017604 nitric acid Inorganic materials 0.000 claims description 6
- 239000002244 precipitate Substances 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 6
- 238000004528 spin coating Methods 0.000 claims description 6
- 230000015572 biosynthetic process Effects 0.000 claims description 5
- 238000003786 synthesis reaction Methods 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 239000000047 product Substances 0.000 claims description 4
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 4
- 229910021607 Silver chloride Inorganic materials 0.000 claims description 3
- 238000004917 polyol method Methods 0.000 claims description 3
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 3
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 3
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 3
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 claims description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 229910001507 metal halide Inorganic materials 0.000 claims description 2
- 150000005309 metal halides Chemical class 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- GGCZERPQGJTIQP-UHFFFAOYSA-N sodium;9,10-dioxoanthracene-2-sulfonic acid Chemical compound [Na+].C1=CC=C2C(=O)C3=CC(S(=O)(=O)O)=CC=C3C(=O)C2=C1 GGCZERPQGJTIQP-UHFFFAOYSA-N 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 239000001117 sulphuric acid Substances 0.000 claims description 2
- 235000011149 sulphuric acid Nutrition 0.000 claims description 2
- 238000010306 acid treatment Methods 0.000 abstract description 4
- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Chemical compound [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-UHFFFAOYSA-N 0.000 abstract description 4
- 239000012776 electronic material Substances 0.000 abstract description 2
- 229910001923 silver oxide Inorganic materials 0.000 abstract description 2
- 239000010408 film Substances 0.000 description 30
- 239000000243 solution Substances 0.000 description 15
- 239000002105 nanoparticle Substances 0.000 description 6
- 229910052709 silver Inorganic materials 0.000 description 6
- 239000004332 silver Substances 0.000 description 6
- 230000005540 biological transmission Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000010413 mother solution Substances 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 239000000428 dust Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910021389 graphene Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000523 sample Substances 0.000 description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 2
- JHJLBTNAGRQEKS-UHFFFAOYSA-M sodium bromide Chemical compound [Na+].[Br-] JHJLBTNAGRQEKS-UHFFFAOYSA-M 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
Landscapes
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Powder Metallurgy (AREA)
- Non-Insulated Conductors (AREA)
- Manufacturing Of Electric Cables (AREA)
Abstract
The invention discloses a processing method for a silver nanowire conductive thin film, and belongs to the technical field of a flexible electronic material and a thin film. According to the processing method, the photoelectric property of the silver nanowire conductive thin film is improved mainly by acid treatment on the silver nanowire conductive thin film. The processing method has the advantages of (1) the process is simple and is easy to operate; (2) silver oxide on the surface of the silver nanowire conductive thin film is efficiently removed; (3) the surface flatness of the silver nanowire conductive thin film is improved; and (4) the conductivity of the silver nanowire conductive thin film is improved, and the square resistance of the thin film is reduced.
Description
Technical field
The present invention relates to flexible electronics and thin film technique field.Specifically, relate to a kind of electric conductivity that can improve thin film, reduce the processing method of the nano silver wire conductive film of the sheet resistance of thin film.
Technical background
Conductive film is widely used in fields such as photoelectron and microelectronics, the device such as such as information shows, information storage, energy conversion, bioelectronics.Currently, the most common conductive film is based on the metal-oxide film of conventional inorganic material, such as ITO, IZO etc..But, rare earth metal is increasingly deficient, causes price increasingly expensive.Along with the fast development of flexible electronic, the products such as following mobile terminal, wearable device, intelligent appliance are had powerful demand by people, and the exploitation electronic material that raw material is rich, cheap, pliability is good is significant with thin-film device.At present, flexible conducting material mainly has nano silver wire, metal grill, Graphene, CNT etc..Metal grill has the electric conductivity of excellence, but there is the broad and rough unauspicious interference ripple caused of the made metal wire of technique, is not suitable for high-resolution products.CNT has outstanding electric property and excellent mechanical performance, is one of ideal material preparing flexible conductive film.But, CNT productivity in preparation with purge process is low, and separation difficulty and poor efficiency between metallicity and semiconductive carbon nano tube, there is the deficiency that preparation process is complicated and cost is high.Graphene has high mobility and good mechanicalness, but it is still in development, it is achieved low cost volume production is challenging.
In recent years, along with day by day vigorous to flexible conductive film demand of flexible electronic, the R & D Enterprises focusing on nano silver wire technology emerges day by day, such as TPK company of Taiwan panel supplier, nano silver wire material supplier CambriosTechnologies company.Nano silver wire conductive film not only has high conductivity, the high grade of transparency, also has certain ductility simultaneously.The process of nano silver wire thin film is also received much concern, Stanford Univ USA Cui Yi et al. is at ACSNano, 2010,4, the upper electric conductivity by strengthening nano silver wire in nano silver wire surface gold-plating and physical pressure of 2955-2963 and reduce surface roughness, but the method preparation cost height, complex process, it is not easy to industrialized production.
So, a kind of cost of urgent need is low, technique simple, be prone to industrialized production, can strengthen the processing method of the nano silver wire conductive film of the electric conductivity of nano silver wire simultaneously.
Summary of the invention
For above-mentioned technical problem, present invention is primarily targeted at the processing method proposing a kind of nano silver wire conductive film, at conductive film (particularly flexible conductive film) and photoelectric functional devices field, there is potential actual application value.
For achieving the above object, the present invention adopts the following technical scheme that
The processing method of a kind of nano silver wire conductive film, comprises the following steps:
1) adopting polyol process synthesis of silver nano-wire, then configuration nano silver wire alcoholic solution is standby；
2) clean microscope slide, respectively ultrasonic cleaning in deionized water, ethanol, isopropanol (hydrophilicity-imparting treatment), dry up standby；
3) adopt step 1) nano silver wire alcoholic solution and step 2) microscope slide utilize spin-coating method to prepare nano silver wire conductive film, under room temperature, dry 0.5-2h, tests its sheet resistance；
4) certain density dilute acid soln is configured with deionized water；
5) by step 3) in the nano silver wire conductive film of preparation immerse in dilute acid soln a period of time, take out and immerse again in deionized water and quickly remove, N2Drying up, under room temperature, dry 1-4h, tests its sheet resistance.
Further technical scheme, in described step 1, the synthetic method of nano silver wire comprises the following steps: 1) by ethylene glycol, polyvinylpyrrolidone, metal halide mixing, obtain mixed liquor；2) by step 1) heating of the solution that obtains is to after 165-175 DEG C, add silver chloride powder, disposable addition silver salt reacts wherein again, product is centrifuged cleaning after terminating by reaction, obtain nano silver wire precipitate, finally adopt ethanol precipitate is extracted and disperses, obtain nano silver wire alcoholic solution.
Further technical scheme, in described step 4, diluted acid includes: hydrochloric acid, sulphuric acid, nitric acid.
Further technical scheme, the concentration of described dilute acid soln is 0.05-0.4M.
Further technical scheme, in described step 5, the time immersing dilute acid soln is 1-20min.
Further technical scheme, in described step 1, the concentration of nano silver wire alcoholic solution is 2-10mg/ml.
Further technical scheme, in described step 2, the time of different solvents cleaning microscope slide is 10-30min.
Further technical scheme, in described step 3, spin-coating method is prepared the condition of nano silver wire conductive film and is: spin speed is 500-3000rpm.
Beneficial effect
Compared with prior art, the present invention has following remarkable advantage:
1, nano silver wire conductive film is passed through dilute acid pretreatment by the present invention, belong to Whote-wet method to process, improve the electric conductivity of nano silver wire thin film, reduce the sheet resistance (as shown in Figures 1 to 4) of thin film and provide reliable solution for realizing nano silver wire conductive film post processing, and the method cost of the present invention is low, method simply, easily operate.
2, when the diluted acid of the present invention selects dust technology, the silver oxide of film surface can not only be eliminated efficiently, improve the electric conductivity of nano silver wire thin film, moreover it is possible to effectively reduce roughness of film, improve nano silver wire thin film surface planeness.
3, the nano silver wire conductive film of the present invention has excellent electric conductivity and mechanical flexibility, it it is the ideal electrode material substituting tradition ITO conductive film, can be widely applied to flexible electronic field, such as touch screen, luminescence display, solaode, wearable electronic etc..
Accompanying drawing explanation
Fig. 1 is the relation curve of sheet resistance and film transmission rate before embodiment 1 nitric acid treatment.
Fig. 2 is the relation curve of sheet resistance and film transmission rate after embodiment 1 nitric acid treatment.
Fig. 3 is the relation curve of sheet resistance and film transmission rate before embodiment 2 HCl treatment.
Fig. 4 is the relation curve of sheet resistance and film transmission rate after embodiment 2 HCl treatment.
Detailed description of the invention
In order to be more fully understood that the content of patent of the present invention, further illustrate below by instantiation.But these embodiments are not limiting as the present invention, those skilled in the art make some nonessential improvement and adjustment according to the content of foregoing invention, belong to scope.
The preparation method of nano silver wire alcoholic solution, comprises the following steps:
1) adding 16ml ethylene glycol, 0.01g sodium bromide, 0.66g polyvinylpyrrolidone in reactor, then stir and heat, heating-up temperature is to 165 DEG C.Being eventually adding 0.05g silver chloride, after reaction 3min, be slow added into 4ml and contain the ethylene glycol solution of 0.22g silver nitrate, rate of addition is 0.4ml/min, and response time 30min is cooled to room temperature, obtains silver nanoparticle mother solution.
2) nano silver wire mother solution is poured in centrifuge tube, centrifugal 30min under 2000rpm speed, discard precipitate, retain upper strata silver nanoparticle mother solution, add the ethanol of nano silver wire mother solution parts by volume 4 times, then pass through 6000rpm centrifugal treating and remove supernatant, so repeating 3 times, finally adopt ethanol precipitate is extracted and disperses, obtain nano silver wire alcoholic solution.
Embodiment 1
Nitric acid treatment strengthens the method for silver nanoparticle film conductivity, comprises the following steps:
1) 5mg/ml nano silver wire alcoholic solution is configured with the nano silver wire of above-mentioned synthesis；
2) cleaning microscope slide, ultrasonic cleaning 15min in deionized water, ethanol, isopropanol, dries up respectively；
3) spin-coating method prepares nano silver wire conductive film, and spin speed is 1000rpm, and under room temperature, dry 1h, utilizes four probe sheet resistance instrument to test its sheet resistance；
4) it is the dilute nitric acid solution of 0.2M with deionized water configuration concentration；
5) silver nanoparticle thin film is immersed 5min in dust technology, take out and immerse again in alcoholic solution and quickly remove, N2Drying up, under room temperature, dry 1h, tests its sheet resistance.
Embodiment 2
HCl treatment strengthens the method for silver nanoparticle film conductivity, comprises the following steps:
1) with the nano silver wire of above-mentioned synthesis, 10mg/ml nano silver wire alcoholic solution is configured；
2) cleaning microscope slide, ultrasonic cleaning 20min in deionized water, ethanol, isopropanol, dries up respectively；
3) spin-coating method prepares nano silver wire conductive film, and spin speed is 3000rpm, and under room temperature, dry 0.5h, utilizes four probe sheet resistance instrument to test its sheet resistance；
4) it is the dilute hydrochloric acid solution of 0.1M with deionized water configuration concentration；
5) silver nanoparticle thin film is immersed dust technology 15min, take out and immerse again in alcoholic solution and quickly remove, N2Drying up, under room temperature, dry 2h, tests its sheet resistance.
Claims (8)
1. the processing method of a nano silver wire conductive film, it is characterised in that: comprise the following steps:
1) adopting polyol process synthesis of silver nano-wire, then configuration nano silver wire alcoholic solution, standby；
2) clean microscope slide, respectively ultrasonic cleaning in deionized water, ethanol, isopropanol, dry up standby；
3) adopt step 1) nano silver wire alcoholic solution and step 2) microscope slide utilize spin-coating method to prepare nano silver wire conductive film, under room temperature, dry 0.5-2h, tests its sheet resistance；
4) certain density dilute acid soln is configured with deionized water；
5) by step 3) in the nano silver wire conductive film of preparation immerse in dilute acid soln a period of time, take out and immerse again in deionized water and quickly remove, N2Drying up, under room temperature, dry 1-4h, tests its sheet resistance.
2. the processing method of a kind of nano silver wire conductive film according to claim 1, it is characterized in that: described step 1 adopts polyol process synthesis of silver nano-wire, that prepares nano silver wire alcoholic solution specifically comprises the following steps that 1) by ethylene glycol, polyvinylpyrrolidone, metal halide mixing, obtain mixed liquor；2) by step 1) heating of the solution that obtains is to after 165-175 DEG C, add silver chloride powder, disposable addition silver salt reacts wherein again, product is centrifuged cleaning after terminating by reaction, obtain nano silver wire precipitate, finally adopt ethanol precipitate is extracted and disperses, obtain nano silver wire alcoholic solution.
3. the processing method of a kind of nano silver wire conductive film according to claim 1, it is characterised in that: in described step 4, diluted acid includes: hydrochloric acid, sulphuric acid, nitric acid.
4. the processing method of a kind of nano silver wire conductive film according to claim 1 or 3, it is characterised in that: the concentration of described dilute acid soln is 0.05-0.4M.
5. the processing method of a kind of nano silver wire conductive film according to claim 1, it is characterised in that: in described step 5, the time immersing dilute acid soln is 1-20min.
6. the processing method of a kind of nano silver wire conductive film according to claim 1, it is characterised in that: in described step 1, the concentration of nano silver wire alcoholic solution is 2-10mg/ml.
7. the processing method of a kind of nano silver wire conductive film according to claim 1, it is characterised in that: in described step 2, the time of different solvents cleaning microscope slide is 10-30min.
8. the processing method of a kind of nano silver wire conductive film according to claim 1, it is characterised in that: in described step 3, spin-coating method is prepared the condition of nano silver wire conductive film and is: spin speed is 500-3000rpm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610312744.6A CN105810364A (en) | 2016-05-12 | 2016-05-12 | Processing method for silver nanowire conductive thin film |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610312744.6A CN105810364A (en) | 2016-05-12 | 2016-05-12 | Processing method for silver nanowire conductive thin film |
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| CN201610312744.6A Pending CN105810364A (en) | 2016-05-12 | 2016-05-12 | Processing method for silver nanowire conductive thin film |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106131984A (en) * | 2016-09-12 | 2016-11-16 | 南京工业大学 | A kind of preparation method of nano silver wire graphene oxide composite conductive thin film heater |
| CN108364711A (en) * | 2018-01-30 | 2018-08-03 | 南京邮电大学 | A kind of post-processing approach of silk-screen printing nano silver wire transparent conductive film |
| CN108538498A (en) * | 2018-04-04 | 2018-09-14 | 苏州尤林斯新材料科技有限公司 | A kind of preparation process for the nano silver wire suspension solution being used to prepare conductive film |
| CN108877991A (en) * | 2018-06-27 | 2018-11-23 | 苏州向心力纳米科技有限公司 | A kind of processing method of efficient silver nanowires conductive film |
| CN109065214A (en) * | 2018-07-13 | 2018-12-21 | 华南理工大学 | A kind of preparation method of the flexible transparent conductive film of conduction homogenous silver nano line high adhesion force |
| 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 |
| CN110137276A (en) * | 2018-02-09 | 2019-08-16 | 张陆成 | The device and method for repairing solar battery |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106131984A (en) * | 2016-09-12 | 2016-11-16 | 南京工业大学 | A kind of preparation method of nano silver wire graphene oxide composite conductive thin film heater |
| CN108364711A (en) * | 2018-01-30 | 2018-08-03 | 南京邮电大学 | A kind of post-processing approach of silk-screen printing nano silver wire transparent conductive film |
| CN110137276A (en) * | 2018-02-09 | 2019-08-16 | 张陆成 | The device and method for repairing solar battery |
| CN108538498A (en) * | 2018-04-04 | 2018-09-14 | 苏州尤林斯新材料科技有限公司 | A kind of preparation process for the nano silver wire suspension solution being used to prepare conductive film |
| CN108877991A (en) * | 2018-06-27 | 2018-11-23 | 苏州向心力纳米科技有限公司 | A kind of processing method of efficient silver nanowires conductive film |
| CN109065214A (en) * | 2018-07-13 | 2018-12-21 | 华南理工大学 | A kind of preparation method of the flexible transparent conductive film of conduction homogenous silver nano line high adhesion force |
| 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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Application publication date: 20160727 |