CN108376573A - A method of preparing high shielding effect flexibility form film using nano-silver thread - Google Patents
A method of preparing high shielding effect flexibility form film using nano-silver thread Download PDFInfo
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- CN108376573A CN108376573A CN201810167725.8A CN201810167725A CN108376573A CN 108376573 A CN108376573 A CN 108376573A CN 201810167725 A CN201810167725 A CN 201810167725A CN 108376573 A CN108376573 A CN 108376573A
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 230000000694 effects Effects 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims abstract description 37
- 239000010408 film Substances 0.000 claims abstract description 57
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical class [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000010409 thin film Substances 0.000 claims abstract description 32
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 27
- 238000012986 modification Methods 0.000 claims abstract description 19
- 230000004048 modification Effects 0.000 claims abstract description 19
- 238000006243 chemical reaction Methods 0.000 claims description 34
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 24
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- 239000007788 liquid Substances 0.000 claims description 22
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 20
- 238000012545 processing Methods 0.000 claims description 16
- 239000002904 solvent Substances 0.000 claims description 16
- 238000002604 ultrasonography Methods 0.000 claims description 16
- -1 polyethylene Polymers 0.000 claims description 15
- 239000004698 Polyethylene Substances 0.000 claims description 14
- 229920000573 polyethylene Polymers 0.000 claims description 14
- 229910021389 graphene Inorganic materials 0.000 claims description 13
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical group CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 12
- 239000012159 carrier gas Substances 0.000 claims description 12
- 239000006185 dispersion Substances 0.000 claims description 12
- TVQFCUYSVLMXOC-UHFFFAOYSA-N ethane-1,2-diol;pyrrolidin-2-one Chemical compound OCCO.O=C1CCCN1 TVQFCUYSVLMXOC-UHFFFAOYSA-N 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 12
- 229910001220 stainless steel Inorganic materials 0.000 claims description 12
- 239000010935 stainless steel Substances 0.000 claims description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims description 10
- 239000012454 non-polar solvent Substances 0.000 claims description 10
- 230000005855 radiation Effects 0.000 claims description 9
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 8
- WQYVRQLZKVEZGA-UHFFFAOYSA-N hypochlorite Chemical compound Cl[O-] WQYVRQLZKVEZGA-UHFFFAOYSA-N 0.000 claims description 8
- UGWRVHSFESMVND-UHFFFAOYSA-N silver;ethane-1,2-diol;nitrate Chemical compound [Ag+].OCCO.[O-][N+]([O-])=O UGWRVHSFESMVND-UHFFFAOYSA-N 0.000 claims description 8
- 238000007789 sealing Methods 0.000 claims description 7
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical group ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 6
- 239000000443 aerosol Substances 0.000 claims description 6
- 238000000889 atomisation Methods 0.000 claims description 6
- 230000005684 electric field Effects 0.000 claims description 6
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- 238000006386 neutralization reaction Methods 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 5
- 229920006395 saturated elastomer Polymers 0.000 claims description 5
- HDPLHDGYGLENEI-UHFFFAOYSA-N 2-[1-(oxiran-2-ylmethoxy)propan-2-yloxymethyl]oxirane Chemical compound C1OC1COC(C)COCC1CO1 HDPLHDGYGLENEI-UHFFFAOYSA-N 0.000 claims description 4
- BSKHPKMHTQYZBB-UHFFFAOYSA-N 2-methylpyridine Chemical compound CC1=CC=CC=N1 BSKHPKMHTQYZBB-UHFFFAOYSA-N 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- WHUUTDBJXJRKMK-UHFFFAOYSA-N Glutamic acid Natural products OC(=O)C(N)CCC(O)=O WHUUTDBJXJRKMK-UHFFFAOYSA-N 0.000 claims description 4
- NQTADLQHYWFPDB-UHFFFAOYSA-N N-Hydroxysuccinimide Chemical compound ON1C(=O)CCC1=O NQTADLQHYWFPDB-UHFFFAOYSA-N 0.000 claims description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 4
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 4
- 238000010041 electrostatic spinning Methods 0.000 claims description 4
- 235000013922 glutamic acid Nutrition 0.000 claims description 4
- 239000004220 glutamic acid Substances 0.000 claims description 4
- 239000011261 inert gas Substances 0.000 claims description 4
- 230000002687 intercalation Effects 0.000 claims description 4
- 238000009830 intercalation Methods 0.000 claims description 4
- 238000013508 migration Methods 0.000 claims description 4
- 230000005012 migration Effects 0.000 claims description 4
- 239000007800 oxidant agent Substances 0.000 claims description 4
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 4
- 238000001556 precipitation Methods 0.000 claims description 4
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 4
- 239000000758 substrate Substances 0.000 claims description 4
- IBZJNLWLRUHZIX-UHFFFAOYSA-N 1-ethyl-3-methyl-2h-imidazole Chemical class CCN1CN(C)C=C1 IBZJNLWLRUHZIX-UHFFFAOYSA-N 0.000 claims description 3
- 239000004310 lactic acid Substances 0.000 claims description 3
- 235000014655 lactic acid Nutrition 0.000 claims description 3
- 150000001336 alkenes Chemical class 0.000 claims description 2
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- DCPMPXBYPZGNDC-UHFFFAOYSA-N hydron;methanediimine;chloride Chemical compound Cl.N=C=N DCPMPXBYPZGNDC-UHFFFAOYSA-N 0.000 claims description 2
- 230000001678 irradiating effect Effects 0.000 claims description 2
- HNJBEVLQSNELDL-UHFFFAOYSA-N pyrrolidin-2-one Chemical compound O=C1CCCN1 HNJBEVLQSNELDL-UHFFFAOYSA-N 0.000 claims description 2
- PQUXFUBNSYCQAL-UHFFFAOYSA-N 1-(2,3-difluorophenyl)ethanone Chemical compound CC(=O)C1=CC=CC(F)=C1F PQUXFUBNSYCQAL-UHFFFAOYSA-N 0.000 claims 1
- 230000001476 alcoholic effect Effects 0.000 claims 1
- 229940047670 sodium acrylate Drugs 0.000 claims 1
- 239000004575 stone Substances 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 5
- 238000002834 transmittance Methods 0.000 abstract description 3
- 230000005540 biological transmission Effects 0.000 description 11
- 230000008901 benefit Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 235000015165 citric acid Nutrition 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 3
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 description 3
- 239000002356 single layer Substances 0.000 description 3
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 description 3
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000004020 conductor Substances 0.000 description 2
- MRNHPUHPBOKKQT-UHFFFAOYSA-N indium;tin;hydrate Chemical compound O.[In].[Sn] MRNHPUHPBOKKQT-UHFFFAOYSA-N 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000003643 water by type Substances 0.000 description 2
- OIQGMAAUSGKPEX-UHFFFAOYSA-N C(C(O)C)(=O)O.C(C)N1CN(C=C1)C Chemical compound C(C(O)C)(=O)O.C(C)N1CN(C=C1)C OIQGMAAUSGKPEX-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 241001282153 Scopelogadus mizolepis Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000002109 single walled nanotube Substances 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
Classifications
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
- H01B5/14—Non-insulated conductors or conductive bodies characterised by their form comprising conductive layers or films on insulating-supports
Abstract
The invention discloses a kind of methods preparing high shielding effect flexibility form film using nano-silver thread, including：(1) preparation of nano-silver thread；(2) assembling body thin film is prepared using Lang Gemiaoer Buji trick；(3) assembling body thin film is modified；(4) modification assembling body thin film is immersed in modified graphene solution, adds condensing agent, reacts, it is washed, dry, obtain high shielding effect flexibility form film.Nano-silver thread prepared by the present invention is had excellent performance, electric conductivity, light transmittance and stability are greatly improved, simultaneously high shielding effect flexible shielding form film is prepared using overlength nano-silver thread, obtained film can be directly used for window fitting, and need not destroy window structure, easily realize low square resistance, shield effectiveness is preferable, light transmittance is high, high shielding effect, high flexibility.
Description
Technical field
The present invention relates to a kind of preparation methods of film, and in particular to a kind of to prepare high shielding effect flexibility using nano-silver thread and regard
The method of window film.
Background technology
High shielding effect flexibility form film is most important for many photoelectric devices and component, liquid crystal flat panel display, etc.
It is mostly used as electrode in the electronic devices such as ion display screen, touch-control tablet, Organic Light Emitting Diode and solar cell.Together
When, also it is widely used as antistatic coating and electromagnetic shielding material.The metal oxidation of the multi-purpose doping of general transparent conductive film
Object is prepared, and most commonly used is tin indium oxide (ITO) conductive film, and the electric conductivity and translucency of ITO is excellent.So
And the brittleness of ever-increasing manufacturing cost, indium tin oxide films and the high-temperature process in preparation process limit it
Application in the following photoelectric device, especially flexible photoelectric device.In recent years, such as single-walled carbon nanotube, graphene, nano silver
The new conductive material such as line continues to bring out out.High shielding effect flexibility form film is prepared using above-mentioned conductive material as being expected to replace
For the material of indium tin oxide films.Wherein, nano-silver thread is a kind of ultra-thin metal wire of nanoscale, except excellent leading with silver
Electrically, due to nanometer size effect, nano-silver thread is weaker in visible light region absorption, has excellent translucency and bend resistance
Property.Since nano-silver thread is a kind of direct band gap wide-band gap material, energy gap reaches 3.37ev, in the transmission of visible light wave range
Rate is very high, up to 90% or more, and raw material have derive from a wealth of sources, be resourceful, is nontoxic, is pollution-free, is environmental-friendly, in hydrogen etc.
Stability is better than the advantages of indium tin oxide films form in gas ions.Therefore, nano-silver thread electrically conducting transparent form is considered as most
It is possible that substituting the form material of tin indium oxide, the application of nano-silver thread electrically conducting transparent form will bring significant society's effect
Benefit.Currently, prepare nano-silver thread generally existing instrument and equipment costliness, complex technical process, it is of high cost the problems such as, cannot be satisfied big
Scale prepares the actual demand of high quality nano silver wire.Hence it is imperative that developing a kind of technology, it is equal can efficiently to prepare size
One, the nano-silver thread of good conductivity.Prepare high shielding effect flexibility form film using nano-silver thread simultaneously there is also technologies it is immature,
The problems such as film performance of preparation is poor.
Invention content
It is excellent it is an object of the invention to solve at least the above and/or defect, and provide at least to will be described later
Point.
In order to realize these purposes and other advantages according to the present invention, a kind of utilization nano-silver thread preparation Gao Ping is provided
The method of the flexible form film of effect, includes the following steps：
Step 1: the polyethylene of 30~50 1~1.5mol/L of parts by volume is adjoined pyrrolidone using high-voltage electrostatic spinning apparatus
Ethylene glycol solution is ejected into reactor；The silver nitrate ethylene glycol solution of 20~40 0.5~1mol/L of parts by volume is placed in simultaneously
In ultrasonic atomizer, it is aerosol by silver nitrate ethylene glycol solution ultrasonic atomizatio, aerosol is passed through by carrier gas in reactor,
The temperature being arranged in reactor is 120~160 DEG C, is stirred 30~60min of reaction, obtains reaction solution；In the reactor
The polyethylene for filling a concentration of 0.3~0.5mol/L of 50~100 parts by volume adjoins pyrrolidone ethylene glycol solution and 1~5 parts by volume 0.1
The Klorvess Liquid of~0.3mol/L；
Step 2: the acetone solvent for being three times in reaction solution is added into the reaction solution of step 1, then ultrasound produces gained
Object is placed in the centrifuge that rotating speed is 4500r/min and centrifuges 30min, and after discarding upper solution, precipitation is dispersed in 50-
To get to nano-silver thread in the absolute ethyl alcohol that the volume fraction of 100 parts by volume is 95%；
Step 3: after nano-silver thread, amphiphilic solvent and nonpolar solvent are mixed, obtained dispersion liquid；Using
Lang Gemiaoer-Buji trick after being assembled dispersion liquid on gas-liquid interface, forms the single layer of orderly one-dimensional nano line
Film；Then again the single thin film of the one-dimensional nano line from water-air interfacial migration to substrate on, reached by controlling the number of plies
To the control to assembly film thickness, assembling body thin film is obtained；
Step 4: 10~20 mass parts assembling body thin film is taken to be added in 80~100 parts of dressing agents, surpass at 80~100 DEG C
30~60min of sound is filtered, dry, obtains modification assembling body thin film；1~5 mass parts graphene powder is dispersed in 1000
In mass parts deionized water, after sodium hydroxide is added, then mix with postassium hypochlorite, after ultrasonic reaction, washed be dried to obtain changes
Property graphene；The mass ratio of the graphene powder and sodium hydroxide is 1:30；The graphene powder and strong oxidizer
Mass ratio is 1:10；
Step 5: preparing the modified graphene solution of 1~2g/L, it is molten that modification assembling body thin film is immersed in modified graphene
In liquid, condensing agent is added, reacts 1~3h, it is washed, dry, obtain high shielding effect flexibility form film.
Preferably, in the step 1, the polyethylene of 30~50 1~1.5mol/L of parts by volume is adjoined into pyrrolidone ethylene glycol
In solution extraction to the syringe with stainless steel syringe needle and it is fixed on the propulsion pump for being equipped with high voltage electrostatic equipment, it will be stainless
In draw point head intercalation reaction device, certain high pressure then is set using high voltage electrostatic equipment on the stainless steel syringe needle of syringe,
Propulsion pump fltting speed is set simultaneously, polyethylene is adjoined into pyrrolidone ethylene glycol solution solution and is ejected into reactor；It is described not
It is 10~20mL/h that the internal diameter of rust draw point head, which is 0.5~1mm, promotes the fltting speed of pump, the size of high-pressure electrostatic be 6~
12kV。
Preferably, in the step 1, the power of ultrasonic atomizatio is 1~10kW, and frequency is 1.8~2.4MHz, atomization
Rate is 20~100kg/h；The carrier gas is inert gas, and flow rate of carrier gas is 5~20L/min.
Preferably, further include following procedure between the step 1 neutralization procedure two：High-voltage pulse is added in reaction solution
In electric field processing chamber, handled using high-pressure pulse electric；The parameter of high-pressure pulse electric processing is：Impulse amplitude is
8~12KV, pulse frequency are 800~1000Hz, and pulse width is 8~12us, processing time 60-90min.
Preferably, in the step 3, amphiphilic solvent is n,N-Dimethylformamide, and nonpolar solvent is three chloromethanes
Alkane；The volume ratio of the amphiphilic solvent and nonpolar solvent is 1:1~2；In the dispersion liquid, nano-silver thread it is a concentration of
0.01~0.05g/mL.
Preferably, in the step 4, the frequency of the ultrasound used during modification assembling body thin film is obtained as 30
~45KHz, and ultrasound uses intermitant irradiation, intermittent time when intermitant irradiation is 15~20s/5~10s.
Preferably, the dressing agent includes the raw material of following parts by weight：10~20 parts of glutamic acid, 1~5 part of citric acid, 2
~5 parts of polyvinyl alcohol, 0.1~0.3 part of picoline, 1~3 part of propylene glycol diglycidylether, 1~2 part of 1- ethyl -3- methyl
Imidazole lactic acid, 0.5~1 part of Sodium Polyacrylate, 2~5 parts of γ-(2,3- glycidoxies) propyl trimethoxy silicanes, 10~30
Part acetone, 50~80 parts of water.
Preferably, the reaction process in the step 5 is：By modification assembling body thin film, modified graphene solution and contracting
Mixture is placed in sealing container, and being passed through nitrogen thereto makes nitrogen be saturated, and the sealing container is then placed in 1.5MeV, 30mA
60~90min of radiation treatment is carried out in electron accelerator.
Preferably, the radiation dose rate that uses of irradiating is 100~200kGy/h, irradiation dose for 200~
400kGy。
Preferably, the dosage of the condensing agent is modify assembly film quality 1/5~1/6；The condensing agent is
Mass ratio is 1:3 1- ethyls-(3- dimethylaminopropyls) carbodiimide hydrochloride and n-hydroxysuccinimide.
The present invention includes at least following advantageous effect：Nano-silver thread prepared by the present invention is had excellent performance, electric conductivity, light transmittance
And stability is greatly improved, while high shielding effect flexible shielding form film is prepared using overlength nano-silver thread, it obtains
To film can be directly used for window fitting, and need not destroy window structure, easily realize that low square resistance, shield effectiveness are preferable, thoroughly
Light rate is high, high shielding effect, high flexibility.
Part is illustrated to embody by further advantage, target and the feature of the present invention by following, and part will also be by this
The research and practice of invention and be understood by the person skilled in the art.
Specific implementation mode：
With reference to embodiment, the present invention is described in further detail, to enable those skilled in the art with reference to specification
Word can be implemented according to this.
It should be appreciated that such as " having ", "comprising" and " comprising " term used herein do not allot one or more
The presence or addition of a other elements or combinations thereof.
Embodiment 1：
A method of high shielding effect flexibility form film being prepared using nano-silver thread, is included the following steps：
Step 1: it is molten that the polyethylene of 30 parts by volume 1.5mol/L adjoined pyrrolidone ethylene glycol using high-voltage electrostatic spinning apparatus
Liquid is drawn into the syringe with stainless steel syringe needle and is fixed on the propulsion pump for being equipped with high voltage electrostatic equipment, by stainless steel
In syringe needle intercalation reaction device, certain high pressure then is set using high voltage electrostatic equipment on the stainless steel syringe needle of syringe, together
When setting promote pump fltting speed, polyethylene is adjoined into pyrrolidone ethylene glycol solution solution and is ejected into reactor；Simultaneously by 20 bodies
The silver nitrate ethylene glycol solution of product part 1mol/L is placed in ultrasonic atomizer, is atomization by silver nitrate ethylene glycol solution ultrasonic atomizatio
Aerosol is passed through by carrier gas in reactor by object, and the temperature being arranged in reactor is 160 DEG C, is stirred reaction 60min,
Obtain reaction solution；The polyethylene that a concentration of 0.3mol/L of 100 parts by volume is filled in the reactor adjoins pyrrolidone ethylene glycol solution
With the Klorvess Liquid of 1 parts by volume 0.1mol/L；The internal diameter of the stainless steel syringe needle is 0.5mm, promotes the fltting speed of pump
Size for 10mL/h, high-pressure electrostatic is 8kV；The power of ultrasonic atomizatio is 5kW, frequency 2.4MHz, atomization rates 80kg/
h；The carrier gas is inert gas, flow rate of carrier gas 20L/min；
Step 2: the acetone solvent for being three times in reaction solution is added into the reaction solution of step 1, then ultrasound produces gained
Object is placed in the centrifuge that rotating speed is 4500r/min and centrifuges 30min, and after discarding upper solution, precipitation is dispersed in 100 bodies
To get to nano-silver thread in the absolute ethyl alcohol that the volume fraction of product part is 95%；
Step 3: after nano-silver thread, amphiphilic solvent and nonpolar solvent are mixed, obtained dispersion liquid；Using
Lang Gemiaoer-Buji trick after being assembled dispersion liquid on gas-liquid interface, forms the single layer of orderly one-dimensional nano line
Film；Then again the single thin film of the one-dimensional nano line from water-air interfacial migration to substrate on, reached by controlling the number of plies
To the control to assembly film thickness, assembling body thin film is obtained；Amphiphilic solvent is n,N-Dimethylformamide, and nonpolarity is molten
Agent is chloroform；The volume ratio of the amphiphilic solvent and nonpolar solvent is 1:1；In the dispersion liquid, nano-silver thread
A concentration of 0.01g/mL；
Step 4: 20 mass parts assembling body thin film is taken to be added in 100 parts of dressing agents, and the ultrasound 60min at 100 DEG C, filtering,
It is dry, obtain modification assembling body thin film；5 mass parts graphene powders are dispersed in 1000 mass parts deionized waters, are added
After entering sodium hydroxide, then mix with postassium hypochlorite, it is washed to be dried to obtain modified graphene after ultrasonic reaction；The graphite
The mass ratio of alkene powder and sodium hydroxide is 1:30；The mass ratio of the graphene powder and strong oxidizer is 1:10；Wherein, it obtains
The frequency of the ultrasound used during assembling body thin film to modification is for 45KHz, and ultrasound is using intermitant irradiation, when intermitant irradiation
Intermittent time be 15s/10s；
Step 5: preparing the modified graphene solution of 2g/L, modification assembling body thin film is immersed in modified graphene solution
In, condensing agent is added, 3h is reacted, it is washed, dry, obtain high shielding effect flexibility form film；The dosage of the condensing agent is
Modify the 1/5 of assembly film quality；The condensing agent is that mass ratio is 1:3 1- ethyls-(3- dimethylaminopropyls) carbon
Diimmonium salt hydrochlorate and n-hydroxysuccinimide.
Wherein, after tested and statistics, the diameter about 42nm of the nano-silver thread obtained in step 2, length about 40um, major diameter
Than being 952；Average light transmission rate of the high shielding effect flexibility form film obtained in step 5 in visible light region is 88%, sheet resistance
For 30 Ω/sq.
Embodiment 2：
A method of high shielding effect flexibility form film being prepared using nano-silver thread, is included the following steps：
Step 1: the polyethylene of 50 parts by volume 1mol/L is adjoined pyrrolidone ethylene glycol solution using high-voltage electrostatic spinning apparatus
It is drawn into the syringe with stainless steel syringe needle and is fixed on the propulsion pump for being equipped with high voltage electrostatic equipment, by stainless pin
In head intercalation reaction device, certain high pressure then is set using high voltage electrostatic equipment on the stainless steel syringe needle of syringe, simultaneously
Setting promotes pump fltting speed, and polyethylene is adjoined pyrrolidone ethylene glycol solution solution and is ejected into reactor；Simultaneously by 30 volumes
The silver nitrate ethylene glycol solution of part 0.8mol/L is placed in ultrasonic atomizer, is atomization by silver nitrate ethylene glycol solution ultrasonic atomizatio
Aerosol is passed through by carrier gas in reactor by object, and the temperature being arranged in reactor is 150 DEG C, is stirred reaction 60min,
Obtain reaction solution；The polyethylene that a concentration of 0.5mol/L of 100 parts by volume is filled in the reactor adjoins pyrrolidone ethylene glycol solution
With the Klorvess Liquid of 3 parts by volume 0.2mol/L；The internal diameter of the stainless steel syringe needle is 1mm, the fltting speed of propulsion pump is
15mL/h, high-pressure electrostatic size be 12kV；The power of ultrasonic atomizatio is 10kW, frequency 2MHz, atomization rates 50kg/h；
The carrier gas is inert gas, flow rate of carrier gas 15L/min；
Step 2: the acetone solvent for being three times in reaction solution is added into the reaction solution of step 1, then ultrasound produces gained
Object is placed in the centrifuge that rotating speed is 4500r/min and centrifuges 30min, and after discarding upper solution, precipitation is dispersed in 80 bodies
To get to nano-silver thread in the absolute ethyl alcohol that the volume fraction of product part is 95%；
Step 3: after nano-silver thread, amphiphilic solvent and nonpolar solvent are mixed, obtained dispersion liquid；Using
Lang Gemiaoer-Buji trick after being assembled dispersion liquid on gas-liquid interface, forms the single layer of orderly one-dimensional nano line
Film；Then again the single thin film of the one-dimensional nano line from water-air interfacial migration to substrate on, reached by controlling the number of plies
To the control to assembly film thickness, assembling body thin film is obtained；Amphiphilic solvent is n,N-Dimethylformamide, and nonpolarity is molten
Agent is chloroform；The volume ratio of the amphiphilic solvent and nonpolar solvent is 1:2；In the dispersion liquid, nano-silver thread
A concentration of 0.03g/mL；
Step 4: 10 mass parts assembling body thin film is taken to be added in 80 parts of dressing agents, the ultrasound 45min at 80 DEG C is filtered, and is done
It is dry, obtain modification assembling body thin film；3 mass parts graphene powders are dispersed in 1000 mass parts deionized waters, are added
After sodium hydroxide, then mix with postassium hypochlorite, it is washed to be dried to obtain modified graphene after ultrasonic reaction；The graphene
The mass ratio of powder and sodium hydroxide is 1:30；The mass ratio of the graphene powder and strong oxidizer is 1:10；Wherein, it obtains
The frequency of the ultrasound used during modification assembling body thin film is for 45KHz, and ultrasound is using intermitant irradiation, when intermitant irradiation
Intermittent time is 15s/10s；
Step 5: preparing the modified graphene solution of 2g/L, modification assembling body thin film is immersed in modified graphene solution
In, condensing agent is added, 3h is reacted, it is washed, dry, obtain high shielding effect flexibility form film；The dosage of the condensing agent is
Modify the 1/6 of assembly film quality；The condensing agent is that mass ratio is 1:3 1- ethyls-(3- dimethylaminopropyls) carbon
Diimmonium salt hydrochlorate and n-hydroxysuccinimide.
Wherein, after tested and statistics, the diameter about 43nm of the nano-silver thread obtained in step 2, length about 42um, major diameter
Than being 976；Average light transmission rate of the high shielding effect flexibility form film obtained in step 5 in visible light region is 89%, sheet resistance
For 28 Ω/sq.
Embodiment 3：
Further include following procedure between the step 1 neutralization procedure two：High-voltage pulse electric field processing chamber is added in reaction solution
In, it is handled using high-pressure pulse electric；The parameter of high-pressure pulse electric processing is：Impulse amplitude is 12KV, pulse
Frequency is 1000Hz, pulse width 12us, processing time 90min；
Remaining technical process and parameter with it is identical in embodiment 1.
Wherein, after tested and statistics, the diameter about 40nm of the nano-silver thread obtained in step 2, length about 45um, major diameter
Than being 1125；Average light transmission rate of the high shielding effect flexibility form film obtained in step 5 in visible light region is 91%, side
Resistance is 26 Ω/sq.
Embodiment 4：
Further include following procedure between the step 1 neutralization procedure two：High-voltage pulse electric field processing chamber is added in reaction solution
In, it is handled using high-pressure pulse electric；The parameter of high-pressure pulse electric processing is：Impulse amplitude is 10KV, pulse
Frequency is 800Hz, pulse width 10us, processing time 60min；
Remaining technical process and parameter with it is identical in embodiment 1.
Wherein, after tested and statistics, the diameter about 40nm of the nano-silver thread obtained in step 2, length about 45um, major diameter
Than being 1125；Average light transmission rate of the high shielding effect flexibility form film obtained in step 5 in visible light region is 90%, side
Resistance is 27 Ω/sq.
Embodiment 5：
The dressing agent includes the raw material of following parts by weight：20 parts of glutamic acid, 5 parts of citric acids, 2 parts of polyvinyl alcohol, 0.3 part
Picoline, 2 parts of propylene glycol diglycidylethers, 2 parts of 1- ethyl-3-methylimidazoles lactic acid, 1 part of Sodium Polyacrylate, 2 parts of γ-
(2,3- glycidoxies) propyl trimethoxy silicane, 30 parts of acetone, 80 parts of water.
Remaining technical process and parameter with it is identical in embodiment 1.
Wherein, after tested and statistics, the diameter about 42nm of the nano-silver thread obtained in step 2, length about 40um, major diameter
Than being 952；Average light transmission rate of the high shielding effect flexibility form film obtained in step 5 in visible light region is 91%, sheet resistance
For 26 Ω/sq.
Embodiment 6：
The dressing agent includes the raw material of following parts by weight：15 parts of glutamic acid, 2 parts of citric acids, 2 parts of polyvinyl alcohol, 0.3 part
Picoline, 2 parts of propylene glycol diglycidylethers, 1 part of 1- ethyl-3-methylimidazoles lactic acid, 1 part of Sodium Polyacrylate, 5 parts of γ-
(2,3- glycidoxies) propyl trimethoxy silicane, 10 parts of acetone, 80 parts of water.
Remaining technical process and parameter with it is identical in embodiment 1.
Wherein, after tested and statistics, the diameter about 42nm of the nano-silver thread obtained in step 2, length about 40um, major diameter
Than being 952；Average light transmission rate of the high shielding effect flexibility form film obtained in step 5 in visible light region is 91.8%, side
Resistance is 26 Ω/sq.
Embodiment 7：
Reaction process in the step 5 is：Modification assembling body thin film, modified graphene solution and condensing agent are placed in
In sealing container, being passed through nitrogen thereto makes nitrogen be saturated, and then electronics which is placed in 1.5MeV, 30mA accelerates
Radiation treatment 90min is carried out in device；The radiation dose rate used that irradiates is 100kGy/h, irradiation dose 400kGy.
Remaining technical process and parameter with it is identical in embodiment 1.
Wherein, after tested and statistics, the diameter about 42nm of the nano-silver thread obtained in step 2, length about 40um, major diameter
Than being 952；Average light transmission rate of the high shielding effect flexibility form film obtained in step 5 in visible light region is 92.5%, side
Resistance is 24 Ω/sq.
Embodiment 8：
Reaction process in the step 5 is：Modification assembling body thin film, modified graphene solution and condensing agent are placed in
In sealing container, being passed through nitrogen thereto makes nitrogen be saturated, and then electronics which is placed in 1.5MeV, 30mA accelerates
Radiation treatment 60min is carried out in device；The radiation dose rate used that irradiates is 200kGy/h, irradiation dose 300kGy.
Remaining technical process and parameter with it is identical in embodiment 1.
Wherein, after tested and statistics, the diameter about 42nm of the nano-silver thread obtained in step 2, length about 40um, major diameter
Than being 952；Average light transmission rate of the high shielding effect flexibility form film obtained in step 5 in visible light region is 92.8%, side
Resistance is 24 Ω/sq.
Embodiment 9：
Reaction process in the step 5 is：Modification assembling body thin film, modified graphene solution and condensing agent are placed in
In sealing container, being passed through nitrogen thereto makes nitrogen be saturated, and then electronics which is placed in 1.5MeV, 30mA accelerates
Radiation treatment 60min is carried out in device；The radiation dose rate used that irradiates is 200kGy/h, irradiation dose 300kGy.
Remaining technical process and parameter with it is identical in embodiment 6.
Wherein, after tested and statistics, the diameter about 42nm of the nano-silver thread obtained in step 2, length about 40um, major diameter
Than being 952；Average light transmission rate of the high shielding effect flexibility form film obtained in step 5 in visible light region is 93.5%, side
Resistance is 22 Ω/sq.
Embodiment 10：
Further include following procedure between the step 1 neutralization procedure two：High-voltage pulse electric field processing chamber is added in reaction solution
In, it is handled using high-pressure pulse electric；The parameter of high-pressure pulse electric processing is：Impulse amplitude is 10KV, pulse
Frequency is 800Hz, pulse width 10us, processing time 60min；
Remaining technical process and parameter with it is identical in embodiment 9.
Wherein, after tested and statistics, the diameter about 40nm of the nano-silver thread obtained in step 2, length about 45um, major diameter
Than being 1125；Average light transmission rate of the high shielding effect flexibility form film obtained in step 5 in visible light region is 94.3%,
Sheet resistance is 20 Ω/sq.
Although the embodiments of the present invention have been disclosed as above, but its is not only in the description and the implementation listed
With it can be fully applied to various fields suitable for the present invention, for those skilled in the art, can be easily
Realize other modification, therefore without departing from the general concept defined in the claims and the equivalent scope, the present invention is simultaneously unlimited
In specific details and example shown and described herein.
Claims (10)
1. a kind of method preparing high shielding effect flexibility form film using nano-silver thread, which is characterized in that include the following steps：
Step 1: the polyethylene of 30~50 1~1.5mol/L of parts by volume is adjoined pyrrolidone second two using high-voltage electrostatic spinning apparatus
Alcoholic solution is ejected into reactor；The silver nitrate ethylene glycol solution of 20~40 0.5~1mol/L of parts by volume is placed in ultrasound simultaneously
In atomizer, it is aerosol by silver nitrate ethylene glycol solution ultrasonic atomizatio, aerosol is passed through by carrier gas in reactor, is arranged
Temperature in reactor is 120~160 DEG C, is stirred 30~60min of reaction, obtains reaction solution；It is filled in the reactor
The polyethylene of a concentration of 0.3~0.5mol/L of 50~100 parts by volume adjoin pyrrolidone ethylene glycol solution and 1~5 parts by volume 0.1~
The Klorvess Liquid of 0.3mol/L；
Step 2: the acetone solvent for being three times in reaction solution is added into the reaction solution of step 1, then ultrasound sets products therefrom
In centrifuging 30min in the centrifuge that rotating speed is 4500r/min, after discarding upper solution, precipitation is dispersed in 50-100 bodies
To get to nano-silver thread in the absolute ethyl alcohol that the volume fraction of product part is 95%；
Step 3: after nano-silver thread, amphiphilic solvent and nonpolar solvent are mixed, obtained dispersion liquid；Using bright lattice
Miao Er-Buji trick after being assembled dispersion liquid on gas-liquid interface, forms the single thin layer of orderly one-dimensional nano line
Film；Then again the single thin film of the one-dimensional nano line from water-air interfacial migration to substrate on, reached by controlling the number of plies
Control to assembly film thickness obtains assembling body thin film；
Step 4: 10~20 mass parts assembling body thin film is taken to be added in 80~100 parts of dressing agents, the ultrasound 30 at 80~100 DEG C
~60min is filtered, dry, obtains modification assembling body thin film；1~5 mass parts graphene powder is dispersed in 1000 mass
In part deionized water, after sodium hydroxide is added, then mix with postassium hypochlorite, it is washed to be dried to obtain modified stone after ultrasonic reaction
Black alkene；The mass ratio of the graphene powder and sodium hydroxide is 1:30；The quality of the graphene powder and strong oxidizer
Than being 1:10；
Step 5: preparing the modified graphene solution of 1~2g/L, modification assembling body thin film is immersed in modified graphene solution
In, condensing agent is added, 1~3h is reacted, it is washed, dry, obtain high shielding effect flexibility form film.
2. the method for preparing high shielding effect flexibility form film using nano-silver thread as described in claim 1, which is characterized in that institute
It states in step 1, the polyethylene of 30~50 1~1.5mol/L of parts by volume, which is adjoined pyrrolidone ethylene glycol solution, to be drawn into stainless
It in the syringe of draw point head and is fixed on the propulsion pump for being equipped with high voltage electrostatic equipment, by stainless steel syringe needle intercalation reaction device
In, certain high pressure then is set using high voltage electrostatic equipment on the stainless steel syringe needle of syringe, while propulsion pump is set and is pushed away
Into speed, polyethylene is adjoined into pyrrolidone ethylene glycol solution solution and is ejected into reactor；The internal diameter of the stainless steel syringe needle is
The fltting speed that 0.5~1mm, propulsion pump is 10~20mL/h, the size of high-pressure electrostatic is 6~12kV.
3. the method for preparing high shielding effect flexibility form film using nano-silver thread as described in claim 1, which is characterized in that institute
It states in step 1, the power of ultrasonic atomizatio is 1~10kW, and frequency is 1.8~2.4MHz, and atomization rates are 20~100kg/h；Institute
It is inert gas to state carrier gas, and flow rate of carrier gas is 5~20L/min.
4. the method for preparing high shielding effect flexibility form film using nano-silver thread as described in claim 1, which is characterized in that institute
It further includes following procedure to state between step 1 neutralization procedure two：Reaction solution is added in high-voltage pulse electric field processing chamber, height is utilized
Pressure impulse electric field is handled；The parameter of high-pressure pulse electric processing is：Impulse amplitude is 8~12KV, and pulse frequency is
800~1000Hz, pulse width are 8~12us, processing time 60-90min.
5. the method for preparing high shielding effect flexibility form film using nano-silver thread as described in claim 1, which is characterized in that institute
It states in step 3, amphiphilic solvent is n,N-Dimethylformamide, and nonpolar solvent is chloroform；The amphiphilic solvent with
The volume ratio of nonpolar solvent is 1:1~2；In the dispersion liquid, a concentration of 0.01~0.05g/mL of nano-silver thread.
6. the method for preparing high shielding effect flexibility form film using nano-silver thread as described in claim 1, which is characterized in that institute
It states in step 4, obtains the frequency of the ultrasound used during modification assembling body thin film for 30~45KHz, and between ultrasound use
It has a rest irradiation, intermittent time when intermitant irradiation is 15~20s/5~10s.
7. the method for preparing high shielding effect flexibility form film using nano-silver thread as described in claim 1, which is characterized in that institute
State the raw material that dressing agent includes following parts by weight：10~20 parts of glutamic acid, 1~5 part of citric acid, 2~5 parts of polyvinyl alcohol, 0.1~
0.3 part of picoline, 1~3 part of propylene glycol diglycidylether, 1~2 part of 1- ethyl-3-methylimidazoles lactic acid, 0.5~1 part it is poly-
Sodium acrylate, 2~5 parts of γ-(2,3- glycidoxies) propyl trimethoxy silicanes, 10~30 parts of acetone, 50~80 parts of water.
8. the method for preparing high shielding effect flexibility form film using nano-silver thread as described in claim 1, which is characterized in that institute
The reaction process stated in step 5 is：Modification assembling body thin film, modified graphene solution and condensing agent are placed in sealing container,
Being passed through nitrogen thereto makes nitrogen be saturated, and then the sealing container is placed in the electron accelerator of 1.5MeV, 30mA and carries out spoke
According to 60~90min of processing.
9. the method for preparing high shielding effect flexibility form film using nano-silver thread as claimed in claim 8, which is characterized in that institute
The radiation dose rate for irradiating and using is stated as 100~200kGy/h, irradiation dose is 200~400kGy.
10. the method for preparing high shielding effect flexibility form film using nano-silver thread as described in claim 1, which is characterized in that
The dosage of the condensing agent is modify assembly film quality 1/5~1/6；The condensing agent is that mass ratio is 1:3 1- second
Base-(3- dimethylaminopropyls) carbodiimide hydrochloride and n-hydroxysuccinimide.
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| CN110752066A (en) * | 2019-11-25 | 2020-02-04 | 四川浩宇华东科技有限公司 | Preparation method of high-transmittance shielding film based on silver nanowires |
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