CN107805314A - A kind of antireflecting coating based on nano silver wire and preparation method thereof - Google Patents
A kind of antireflecting coating based on nano silver wire and preparation method thereof Download PDFInfo
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- CN107805314A CN107805314A CN201710955284.3A CN201710955284A CN107805314A CN 107805314 A CN107805314 A CN 107805314A CN 201710955284 A CN201710955284 A CN 201710955284A CN 107805314 A CN107805314 A CN 107805314A
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- C—CHEMISTRY; METALLURGY
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
- C08J7/06—Coating with compositions not containing macromolecular substances
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2333/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2333/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters
- C08J2333/06—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters of esters containing only carbon, hydrogen, and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C08J2333/10—Homopolymers or copolymers of methacrylic acid esters
- C08J2333/12—Homopolymers or copolymers of methyl methacrylate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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Abstract
The present invention relates to a kind of antireflecting coating based on nano silver wire and preparation method thereof, to solve the problems, such as further to improve nano silver wire coating translucency, long-time stability, the present invention proposes is coated in nano silver wire coating surface using tin indium oxide nano dispersion fluid, and the Ag/ITO compound anti-reflection coatings based on nano silver wire are obtained after solidification.A kind of described antireflecting coating based on nano silver wire has good light transmittance, electric conductivity, longer service life.
Description
Technical field
The present invention relates to a kind of conductive antireflecting coating, and in particular to a kind of antireflecting coating and its preparation based on nano silver wire
Method.
Background technology
In transparent conducting coating field, tin indium oxide(ITO)Transparent conducting coating and nano silver wire transparent conducting coating are
Two important branches.Ito thin film have the advantages that the transparency it is good, electric conductivity is high, it is easy etching and easy low temperature preparation, be always
The preferred material of bright conductive coating.The wider method of its current commercial Application is magnetron sputtering method, and shortcoming is that required equipment is non-
Often complicated, equipment investment height, target require high.For the shortcoming, directly ITO nanometer grade powders are scattered in solvent, added
Enter film forming matter and dispersant etc. and be prepared into coating, it is final directly to obtain the method more and more hand of ito thin film coated on substrate surface
Section concern.But ito thin film has the disadvantages that:First, expensive, second, flex capability is very poor, surface is easily produced after bending
Give birth to slight crack and lose good electric conductivity.
Nano silver wire coating has excellent translucency, stretch-proof, bending resistance, therefore causes basic research and answer
Extensive attention.But the shortcomings that nano silver wire one is that corrosion resisting property is poor, second, comprehensive electric conductivity and light transmission and
Speech, in terms of nano silver wire still lags behind ito transparent electrode, particularly light transmission at this stage, thus how further to improve silver
The translucency of nano wire coating turns into the problem that everybody is studied.But the shortcomings that prior art is not consider how further
Improve the translucency of nano silver wire coating.For example, to disclose a kind of electric conductivity compound for Publication No. CN101724822A patent
Atom oxygen protective coating ITO/MgF2 preparation method, it is that have the anti-reflection effect of light based on MgF2, so as to prepare circle first
ITO targets, then MgF2 flaky materials are uniformly pasted onto on ITO targets and have obtained ITO/MgF2 composition targets, are obtained through magnetron sputtering
ITO/MgF2 conductivity type compound atom oxygen protective coatings.The ITO/MgF2 composite coatings of the invention have anti-reflection effect to light, use
Operating efficiency can be improved in some optics.
Therefore, this area is badly in need of a kind of translucency for further improving nano silver wire coating, has the base of long-time stability
In the preparation method of the antireflecting coating of nano silver wire.
The content of the invention
To solve the problems, such as further to improve nano silver wire coating translucency, long-time stability, the present invention proposes one kind
Antireflecting coating based on nano silver wire and preparation method thereof, the light transmission of the composite coating, service life contrast nano silver wire
Coating is improved.
The present invention is realized by following technical method.
1. a kind of preparation method of the antireflecting coating based on nano silver wire, it is characterised in that described preparation method includes
Following steps:
(1)Prepare the solution containing nano silver wire, step is as follows, first synthesis of silver nano-wire, wherein synthesis of silver nano-wire when adopt
Protective agent is done with polyvinylpyrrolidone, is then disperseed nano silver wire washing in a solvent after purification, so as to obtain containing silver
The solution of nano wire;Or directly buy the solution containing nano silver wire;
(2)By the solution containing nano silver wire coated in nano silver wire coating and the drying that network-like structure is formed in substrate;
(3)Tin indium oxide nano dispersion fluid is coated in nano silver wire coating surface, the particle diameter of indium tin oxide particles is 10 ~ 50nm,
Ag/ITO composite coatings are obtained after solidification, wherein, ITO thicknesses of layers is 50 ~ 400nm, indium tin oxide particles uniform particle sizes, together
Maximum particle diameter in one tin indium oxide nano dispersion fluid is with minimum grain size difference in 10nm.
For step(1)Further description it is as follows.
Step(1)In the nano silver wire voluntarily synthesized or the solution containing nano silver wire directly bought, nano silver wire
It is preferred that a diameter of 70 ~ 120nm, length is 10 ~ 40 μm.Further preferred a diameter of 70 ~ 90nm, length are 20 ~ 30 μm.
Washing purifying nano silver wire is to remove the impurity in nano silver wire, and its washing methods is those skilled in the art
Known.For example, its detailed process can be to take the nano silver wire of bottom precipitation, 2- isopropoxide ethanols are added, are well mixed
After stand, pour out supernatant, only leave bottom precipitation, obtain the nano silver wire of washing after purification.
To obtain the solution containing nano silver wire with good stability, step(1)In solvent be preferably acetic acid fourth
Ester either 2- isopropoxide ethanols or ethanol.
For step(3)Further description it is as follows.
Step(3)In, in tin indium oxide nano dispersion fluid, the particle diameter of ITO particles is preferably 10 ~ 50nm.ITO grain diameters
Difference, the porosity of coating is different, that is, the ratio shared by air is different, and coating refraction index obtained from entering is different, enters
And different coating antireflective effects can be obtained.Inventor also found that the particle diameter of ITO particles is more preferably 20nm, now contrasts and only applies
Nano silver wire coating is covered, the light transmittance of Ag/ITO composite coatings is uniformly carried in whole 400 ~ 800nm wavelength bands
It is high.
In addition, it is found by the applicant that indium tin oxide particles need uniform particle sizes, the maximum in same tin indium oxide nano dispersion fluid
Particle diameter could obtain antireflective effect with minimum grain size difference in 10nm.When in same tin indium oxide nano dispersion fluid, indium oxide
When the particle diameter difference of tin particles is big, light absorbs, light scattering can be caused, influences translucency.
ITO thicknesses of layers is 50 ~ 400nm, preferably 80 ~ 200nm.ITO thicknesses of layers affects the light of ito film layer
Learn thickness, if therefore ITO coatings it is too thin or too thick when, compared with Ag nano wire coatings, Ag/ITO composite coatings 400 ~
800nm visible region can not also realize that it increases the function of light transmittance.
ITO content preferably 5 ~ 30 weight %, more preferably 10 ~ 20 weight % in tin indium oxide nano dispersion fluid.
The method for coating tin indium oxide is that the thermohardening type nano dispersion fluid containing tin indium oxide is coated in through step(2)Place
Nano silver wire coating surface after reason, is then heating and curing;Or by the ultraviolet curing type nano dispersion fluid containing tin indium oxide
Coated in through step(2)Nano silver wire coating surface after processing, then ultraviolet light solidification.The method of the coating can be showering,
One or more in spraying, blade coating, spin coating, dip-coating, brushing or ink-jet printing process, preferably spraying, spin coating, the painting of inkjet printing
Coating process.
The present invention also provides a kind of antireflecting coating based on nano silver wire, and it uses preparation method described above to be prepared into
Arrive.
Conductive antireflecting coating provided by the invention can be applied to extensive base material, including transparent substrates, opaque base
Bottom, flexible substrates, rigid basement, flat base and bending substrate.The base material can be selected from PMA, poly- carbonic acid
Ester, polyester, polystyrene, polyamide, polyimides, polysulfones, polyether sulfone, glass and ceramics, preferably poly-methyl methacrylate
Ester (PMMA), makrolon (PC), polyethylene terephthalate (PET) or glass.
The preparation method of conductive antireflecting coating provided by the invention can apply to a surface of substrate, forms one side and applies
Layer;Two surfaces of substrate are can also be applied to, coated on both sides are formed, further to improve the light transmittance of nano silver wire coating.
The present invention is to be less than nano silver wire as different materials, the refraction index of ITO coatings from nano silver wire based on ITO
Refraction index, thus compared with Ag nano wire coatings, Ag/ITO composite coatings can play antireflective effect.Thus, the present invention adopts
Nano silver wire coating surface is coated in by tin indium oxide nano dispersion fluid, Ag/ITO compound anti-reflection coatings are obtained after solidification.This
Invention provides a kind of preparation method of the antireflecting coating based on nano silver wire, and is prepared for composite coating accordingly, described
A kind of antireflecting coating based on nano silver wire has good light transmittance, electric conductivity, longer service life.
Compared with prior art, the beneficial effects of the invention are as follows:
(1)The present invention is further coated with appropriate particle size, the ITO coatings of thickness on nano silver wire surface, so as to effectively increase
The light transmittance of nano silver wire coating;On the one hand ITO coatings completely cut off empty gas and water and prevent nano silver wire from placing oxygen after long-time
Change, another aspect ITO coatings have good mechanical property, thus improve the service life of composite coating;In addition, ITO is applied
Layer also has certain electric conductivity, ITO and nano silver wire the coating compound electric conductivity for further increasing coating, ensures
Composite coating has good electric conductivity;
(2)To substrate without destruction, can be applied to flexible or rigid substrate, can bend, wind or be cut into it is any use size,
Technique can be carried out at normal temperatures and pressures, and application field is extensive;
(3)Using painting methods such as showering, spraying, spin coatings, coating large area film forming can be achieved.
Brief description of the drawings
Fig. 1 be 400 ~ 800nm wave-length coverages in, made from embodiment 1 substrate surface coating Ag/ITO antireflecting coatings with only
Coat the light transmittance spectrum comparison diagram of nano silver wire coating;
Fig. 2 is in 400 ~ 800nm wave-length coverages, and substrate surface made from embodiment 2 coats Ag/ITO antireflecting coatings with only coating
The light transmittance spectrum comparison diagram of nano silver wire coating.
Embodiment
The present invention is further described in detail with reference to embodiment, the embodiment provided is only for explaining
The bright present invention, the scope being not intended to be limiting of the invention.
Embodiment 1
(1)10mL ethylene glycol is added in a round bottom three-necked bottle, flow back 1h at 180 DEG C, then by temperature stabilization at 180 DEG C,
The ethylene glycol solution containing high chloroplatinic acid that then addition 5mL concentration is 0.06mM after heating 10 minutes, then adds simultaneously as crystal seed
Enter ethylene glycol solution containing silver nitrate that 5mL concentration is 0.1mM and 5mL concentration is that 0.5mM contains PVP(K30)Ethylene glycol it is molten
Liquid, both rate of addition are controlled so that time for adding is 1h, continue to stop heating after reacting 1.5h after completion of dropwise addition, obtain
Solution containing nano silver wire.A diameter of 80 ~ 100nm of the nano silver wire, length are 20 ~ 30 μm.The nano silver wire that will be obtained
Solution left standstill, the precipitation of bottom is nano silver wire, takes the nano silver wire of bottom precipitation to add 2- isopropoxide ethanols, mixed manually
8h is stood after closing uniformly, pours out supernatant, only leaves bottom precipitation, obtains the nano silver wire of washing after purification.Washing is purified
Nano silver wire afterwards is added in ethanol solution, and to obtain the dispersion liquid containing nano silver wire, its concentration is 3wt%.
(2)By the above-mentioned solution containing nano silver wire coated in the nano silver wire coating that network-like structure is formed on substrate PC
And dry.
(3)One layer of thermohardening type tin indium oxide nano dispersion fluid is coated using spin-coating again in coating surface, tin indium oxide
Concentration is 15wt%, and the uniform particle sizes of ITO particles are 20nm.Then it is heating and curing, so as to obtain the Ag/ITO based on nano silver wire
Composite coating, now tin indium oxide thicknesses of layers is 100nm.Four-point method is used to measure the sheet resistance value of coating as 90 Ohm/
sq.Accompanying drawing 1 shown in 400 ~ 800nm wave-length coverages, the Ag/ITO antireflecting coatings and the printing opacity for only coating nano silver wire coating
Rate spectrum comparison diagram.Wherein, curve B is the light transmittance spectrum of Ag/ITO antireflecting coatings, and curve A applies only to coat nano silver wire
The light transmittance spectrum of layer.Therefrom it can be seen that in 400 ~ 800nm whole wave-length coverage, the light transmittance of Ag/ITO antireflecting coatings
It is above only coating nano silver wire coating, light transmittance of the Ag/ITO antireflecting coatings at 550nm is 82.9%.
Embodiment 2
(1) nano silver wire coating and the drying of network-like structure are formed on substrate PC using method same as Example 1.
(2) one layer of thermohardening type tin indium oxide nano dispersion fluid is coated using spin-coating again in coating surface, the concentration of tin indium oxide is
The particle size range of 15wt%, ITO particle is 40~50nm.Then it is heating and curing, so as to obtain the Ag/ITO based on nano silver wire
Composite coating, now tin indium oxide thicknesses of layers is 100nm.Four-point method is used to measure the sheet resistance value of coating as 88Ohm/
sq.Accompanying drawing 2 shows in 400~800nm wave-length coverages that the Ag/ITO antireflecting coatings are with only coating the saturating of nano silver wire coating
Light rate spectrum comparison diagram.Wherein, curve C is the light transmittance spectrum of Ag/ITO antireflecting coatings, and curve A is only to coat silver nanoparticle
The light transmittance spectrum of line coating.Therefrom it can be seen that contrast only coats nano silver wire coating, the light transmittance of Ag/ITO antireflecting coatings
It is improved, light transmittance of the Ag/ITO antireflecting coatings at 550nm is 82.3%.
Embodiment 3
(1)The commercially available solution containing nano silver wire is bought, is then coated with being formed the Yin Na of network-like structure on substrate PMMA
Rice noodles coating and drying.A diameter of 90 ~ the 120nm of nano silver wire, length are 30 ~ 40 μm.Now, nano silver wire coating is in 550nm
The light transmittance at place is 75%.
(2)One layer of ultraviolet curing type tin indium oxide nano dispersion fluid of spray coating, indium oxide are used again in coating surface
The concentration of tin is 20wt%, and the particle size range of ITO particles is 10 ~ 20nm.Then ultraviolet light solidifies, so as to obtain being based on silver nanoparticle
The Ag/ITO composite coatings of line, now tin indium oxide thicknesses of layers is 50nm.The sheet resistance value of coating is measured using four-point method
For 120 Ohm/sq.Light transmittance of the Ag/ITO antireflecting coatings at 550nm is 76.7%.
Embodiment 4
(1)The solution containing nano silver wire is voluntarily synthesized using polyol process, is then coated with forming network-like knot on substrate PET
The nano silver wire coating of structure and drying.A diameter of 70 ~ the 90nm of nano silver wire, length are 10 ~ 20 μm.The solvent of nano silver wire solution
For butyl acetate.Now, light transmittance of the nano silver wire coating at 550nm is 80.2%.
(2)One layer of thermohardening type tin indium oxide nano dispersion fluid is coated using dip-coating again in coating surface, tin indium oxide
Concentration is 10wt%, and the particle size range of ITO particles is 40 ~ 50nm.Then heat cure, so as to obtain the Ag/ based on nano silver wire
ITO composite coatings, now tin indium oxide thicknesses of layers is 400nm.Four-point method is used to measure the sheet resistance value of coating as 80
Ohm/sq.Light transmittance of the Ag/ITO antireflecting coatings at 550nm is 81.3%.
Comparative example 1
(1)10mL ethylene glycol is added in a round bottom three-necked bottle, flow back 1h at 180 DEG C, then by temperature stabilization at 180 DEG C,
The ethylene glycol solution containing high chloroplatinic acid that then addition 5mL concentration is 0.06mM after heating 10 minutes, then adds simultaneously as crystal seed
Enter ethylene glycol solution containing silver nitrate that 5mL concentration is 0.1mM and 5mL concentration is that 0.5mM contains PVP(K30)Ethylene glycol it is molten
Liquid, both rate of addition are controlled so that time for adding is 1h, continue to stop heating after reacting 1.5h after completion of dropwise addition, obtain
Solution containing nano silver wire.A diameter of 80 ~ 100nm of the nano silver wire, length are 20 ~ 30 μm.The nano silver wire that will be obtained
Solution left standstill, the precipitation of bottom is nano silver wire, takes the nano silver wire of bottom precipitation to add 2- isopropoxide ethanols, mixed manually
8h is stood after closing uniformly, pours out supernatant, only leaves bottom precipitation, obtains the nano silver wire of washing after purification.Washing is purified
Nano silver wire afterwards is added in ethanol solution, and to obtain the dispersion liquid containing nano silver wire, its concentration is 3wt%.
(2)By the above-mentioned solution containing nano silver wire coated in the nano silver wire coating that network-like structure is formed on substrate PC
And dry.Four-point method is used to measure the sheet resistance value of coating as 98 Ohm/sq.Curve A in accompanying drawing 1,2 is coating silver
The light transmittance spectrum of nano wire coating, its light transmittance at 550nm are 80.7%.
Applicant states that the present invention illustrates the method detailed of the present invention, but not office of the invention by above-described embodiment
It is limited to above-mentioned method detailed, that is, does not mean that the present invention has to rely on above-mentioned method detailed and could implemented.Art
Technical staff it will be clearly understood that any improvement in the present invention, equivalence replacement and auxiliary element to each raw material of product of the present invention
Addition, selection of concrete mode etc., within the scope of all falling within protection scope of the present invention and disclosing.
Claims (9)
1. a kind of preparation method of the antireflecting coating based on nano silver wire, it is characterised in that described preparation method includes following
Step:
(1)Prepare the solution containing nano silver wire, step is as follows, first synthesis of silver nano-wire, wherein synthesis of silver nano-wire when adopt
Protective agent is done with polyvinylpyrrolidone, is then disperseed nano silver wire washing in a solvent after purification, so as to obtain containing silver
The solution of nano wire;Or directly buy the solution containing nano silver wire;
(2)By the solution containing nano silver wire coated in nano silver wire coating and the drying that network-like structure is formed in substrate;
(3)Tin indium oxide nano dispersion fluid is coated in nano silver wire coating surface, the particle diameter of indium tin oxide particles is 10 ~ 50nm,
Ag/ITO composite coatings are obtained after solidification, wherein, ITO thicknesses of layers is 50 ~ 400nm, indium tin oxide particles uniform particle sizes, together
Maximum particle diameter in one tin indium oxide nano dispersion fluid is with minimum grain size difference in 10nm.
2. preparation method according to claim 1, it is characterised in that step(3)Tin indium oxide nano dispersion fluid in,
The particle diameter of ITO particles is 20nm.
3. according to the preparation method described in claim any one of 1-2, it is characterised in that step(1)The nano silver wire of synthesis is straight
Footpath is 70 ~ 120nm, and length is 10 ~ 40 μm.
4. according to the preparation method described in claim any one of 1-3, it is characterised in that step(3)Middle ITO thicknesses of layers is
80~200nm。
5. according to the preparation method described in claim any one of 1-4, it is characterised in that step(3)Middle tin indium oxide nanometer point
ITO content is 10 ~ 20 weight % in dispersion liquid.
6. according to the preparation method described in claim any one of 1-5, it is characterised in that step(1)In solvent be acetic acid fourth
Ester either 2- isopropoxide ethanols or ethanol.
7. according to the preparation method described in claim any one of 1-6, it is characterised in that step(3)Middle coating tin indium oxide
Method is that the thermohardening type nano dispersion fluid containing tin indium oxide is sprayed or is spin-coated on through step(2)Nano silver wire after processing applies
Layer surface, then it is heating and curing.
8. according to the preparation method described in claim any one of 1-6, it is characterised in that step(3)Middle coating tin indium oxide
Method is that the ultraviolet curing type nano dispersion fluid containing tin indium oxide is coated in through step(2)Nano silver wire coating after processing
Surface, then ultraviolet light solidification.
9. a kind of antireflecting coating based on nano silver wire, it is characterised in that using the preparation side described in claim any one of 1-8
Method is prepared.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN108774450A (en) * | 2018-06-08 | 2018-11-09 | 上海大学 | Metal nanoparticle welds the preparation method of nano silver wire electromagnetic shielding slurry |
CN108892811A (en) * | 2018-06-21 | 2018-11-27 | 中国科学技术大学 | A kind of inorganic wire material-organic polymer composite material and preparation method thereof |
CN109265643A (en) * | 2018-08-06 | 2019-01-25 | 中山大学 | A kind of sunlight selfreparing transparent flexible strain sensing composite material and preparation method and application |
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2017
- 2017-10-14 CN CN201710955284.3A patent/CN107805314A/en active Pending
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108774450A (en) * | 2018-06-08 | 2018-11-09 | 上海大学 | Metal nanoparticle welds the preparation method of nano silver wire electromagnetic shielding slurry |
CN108892811A (en) * | 2018-06-21 | 2018-11-27 | 中国科学技术大学 | A kind of inorganic wire material-organic polymer composite material and preparation method thereof |
CN108892811B (en) * | 2018-06-21 | 2020-02-07 | 中国科学技术大学 | Inorganic material-organic polymer composite material and preparation method thereof |
CN109265643A (en) * | 2018-08-06 | 2019-01-25 | 中山大学 | A kind of sunlight selfreparing transparent flexible strain sensing composite material and preparation method and application |
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