CN114874593A - Preparation method of PET silver film - Google Patents
Preparation method of PET silver film Download PDFInfo
- Publication number
- CN114874593A CN114874593A CN202210661314.0A CN202210661314A CN114874593A CN 114874593 A CN114874593 A CN 114874593A CN 202210661314 A CN202210661314 A CN 202210661314A CN 114874593 A CN114874593 A CN 114874593A
- Authority
- CN
- China
- Prior art keywords
- parts
- silver
- pet
- silver film
- stretching
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 84
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 43
- 239000004332 silver Substances 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229920000728 polyester Polymers 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims abstract description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 45
- 229920000139 polyethylene terephthalate Polymers 0.000 claims description 32
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 30
- 238000000498 ball milling Methods 0.000 claims description 27
- 239000007864 aqueous solution Substances 0.000 claims description 15
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 15
- -1 polybutylene terephthalate Polymers 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 10
- 239000003963 antioxidant agent Substances 0.000 claims description 10
- 230000003078 antioxidant effect Effects 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 10
- 239000008213 purified water Substances 0.000 claims description 10
- 230000003647 oxidation Effects 0.000 claims description 8
- 238000007254 oxidation reaction Methods 0.000 claims description 8
- 238000011049 filling Methods 0.000 claims description 7
- 238000004381 surface treatment Methods 0.000 claims description 7
- 239000000243 solution Substances 0.000 claims description 6
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 5
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 5
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 5
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 5
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 5
- 239000005642 Oleic acid Substances 0.000 claims description 5
- 239000012752 auxiliary agent Substances 0.000 claims description 5
- 239000003638 chemical reducing agent Substances 0.000 claims description 5
- 238000001514 detection method Methods 0.000 claims description 5
- 238000007599 discharging Methods 0.000 claims description 5
- 238000001125 extrusion Methods 0.000 claims description 5
- 239000008098 formaldehyde solution Substances 0.000 claims description 5
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 5
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 5
- 229920003207 poly(ethylene-2,6-naphthalate) Polymers 0.000 claims description 5
- 229920001707 polybutylene terephthalate Polymers 0.000 claims description 5
- 239000011112 polyethylene naphthalate Substances 0.000 claims description 5
- 238000006722 reduction reaction Methods 0.000 claims description 5
- 238000005070 sampling Methods 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- KKEYFWRCBNTPAC-UHFFFAOYSA-L terephthalate(2-) Chemical compound [O-]C(=O)C1=CC=C(C([O-])=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-L 0.000 claims description 3
- 238000005260 corrosion Methods 0.000 abstract description 8
- 230000007797 corrosion Effects 0.000 abstract description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 5
- 239000001301 oxygen Substances 0.000 abstract description 5
- 229910052760 oxygen Inorganic materials 0.000 abstract description 5
- 150000004820 halides Chemical class 0.000 abstract description 4
- 230000002035 prolonged effect Effects 0.000 abstract description 4
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 abstract description 3
- 239000007789 gas Substances 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000004544 sputter deposition Methods 0.000 abstract description 3
- 229910052717 sulfur Inorganic materials 0.000 abstract description 3
- 239000011593 sulfur Substances 0.000 abstract description 3
- 230000003064 anti-oxidating effect Effects 0.000 abstract 1
- 239000011248 coating agent Substances 0.000 abstract 1
- 238000000576 coating method Methods 0.000 abstract 1
- 239000005020 polyethylene terephthalate Substances 0.000 description 23
- 239000010410 layer Substances 0.000 description 8
- 238000002161 passivation Methods 0.000 description 6
- 238000002310 reflectometry Methods 0.000 description 6
- 230000009286 beneficial effect Effects 0.000 description 5
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 description 4
- 238000007747 plating Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 230000002457 bidirectional effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
Classifications
-
- 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
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
-
- 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
-
- 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
- C08J2467/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
-
- 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
- C08J2467/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2467/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0806—Silver
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Laminated Bodies (AREA)
- Manufacture Of Macromolecular Shaped Articles (AREA)
- Shaping By String And By Release Of Stress In Plastics And The Like (AREA)
Abstract
The invention discloses a preparation method of a PET silver film, which comprises the following preparation steps: the method comprises the following steps: carrying out anti-oxidation treatment on the silver powder; step two: preparing raw materials; step three: and stretching by adopting a biaxial stretching method, and then heating to shape the stretched PET so as to obtain the PET silver film. Compared with the prior art, the PET silver film has the advantages that the service life is effectively prolonged, the surface friction resistance is improved, sputtering equipment is not needed, the preparation steps are saved, the production efficiency is improved, the polyester has better corrosion resistance to water vapor, oxygen, halide and sulfur-containing gas through the sandwich protection of the silver powder, the service life of the silver-plated reflecting film is prolonged, the layering phenomenon is effectively prevented, and the problems that the existing silver film is general in corrosion resistance, a coating is easy to fall off, large in equipment investment and easy to oxidize are solved.
Description
Technical Field
The invention relates to the technical field of reflecting materials, in particular to a preparation method of a PET silver film.
Background
With the demands for thinner, smaller and lower power consumption of LCDs for mobile phones, notebook computers, etc., high performance backlight technology must be compatible with them. The reflecting film in the backlight component is mainly used for improving the reflectivity of the optical surface and reflecting the light leaked out of the bottom of the light guide plate with high efficiency and no loss, thereby reducing the light loss, reducing the power consumption and improving the light saturation of the liquid crystal display surface. The silver-plated reflective film has the advantages of high reflectivity, thin thickness and the like, and is widely used for portable equipment such as mobile phones and tablet computers at present. However, the silver metal is unstable and reacts with water, oxygen, halide, sulfide and the like in the environment, so that the reflectivity is obviously reduced, and the whole display effect is influenced.
The silver film on the market at present is a composite material formed by plating a layer of extremely thin metal silver on the surface of PET by a special process, wherein the most common processing method is a magnetron sputtering silver plating method, namely, the silver film is deposited on the surface of PET by high-temperature precipitation in a high vacuum state. However, the penetration of water and oxygen also causes corrosion of the silver layer, which affects the service life of the reflective film, and an interlayer peeling phenomenon easily occurs between two layers, and element migration easily occurs between deposited layers to cause surface fogging, which affects the reflectivity of the reflective film.
In conclusion, silver films with oxidation resistance, long service life and excellent corrosion resistance are still the targets pursued in the industry.
Disclosure of Invention
The invention aims to provide a preparation method of a PET silver film, which solves the problems in practical use.
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation method of a PET silver film comprises the following preparation steps:
the method comprises the following steps: performing oxidation resistance treatment on silver powder
Chemical reduction: adding 300 parts of purified water into a reaction container, and adding 50 parts of silver nitrate under the stirring condition to completely dissolve the silver nitrate; then 60 parts of purified water is used for dissolving 15 parts of sodium hydroxide to prepare a sodium hydroxide aqueous solution; dropwise adding a sodium hydroxide aqueous solution into a silver nitrate aqueous solution, and after the dropwise adding is finished; immediately dripping 15 parts of formaldehyde solution to carry out chemical reaction for 1 hour, and washing the silver powder;
weighing 5 parts of the silver powder, adding 30 parts of zirconia with the diameter of phi 5mm, filling the silver powder into a ball milling tank, adding 7.5 parts of absolute ethyl alcohol as a ball milling solvent, simultaneously adding 0.05 part of oleic acid as an auxiliary agent, setting the rotating speed of 320rpm for ball milling for 16 hours, and stopping ball milling after the grain size is qualified through sampling detection;
dissolving 0.1 part of silver surface treatment passivator (phosphite) by using a small amount of absolute ethyl alcohol, adding the solution into a ball mill, continuously ball-milling for 30min, discharging, drying at 60 ℃, and dispersing to obtain antioxidant flaky silver powder;
step two: preparing raw materials
Respectively adding 65 parts of polyethylene terephthalate, 15 parts of polybutylene terephthalate, 10 parts of polyethylene naphthalate, 3 parts of copolymerized modified polyester and 20 parts of antioxidant silver powder into a double-screw blender;
step three: and stretching by adopting a biaxial stretching method, and then heating to shape the stretched PET so as to obtain the PET silver film.
Preferably: and the extrusion temperature in the single-screw extruder in the second step is 270 ℃, which is beneficial to improving the processability and facilitating the subsequent stretching process.
Preferably: the drying temperature in the third step was 165 ℃.
Preferably: the longitudinal stretching temperature in the two-way stretching in the third step is 85 ℃, and the transverse stretching temperature is 110 ℃.
Preferably: the thickness after stretching in the third step is 0.3 mm.
Preferably: the setting temperature in the third step is 230 ℃.
Compared with the prior art, the invention has the beneficial effects that:
the PET silver film effectively prolongs the service life, improves the surface friction resistance, does not need sputtering equipment, saves preparation steps, and improves the production efficiency, and the reflectivity of the PET silver film reflecting film at the position of 550nm wavelength is more than or equal to 99 percent. Silver surface treatment passivator is added to silver powder, and surface passivation is carried out on flake silver powder through ball-milling mechanical passivation technology, so that a passivation layer is formed on the surface of the silver powder, the oxidation resistance of the silver powder is improved, and the silver powder is protected by filling polyester, so that the silver powder has more excellent corrosion resistance to water vapor, oxygen, halide and sulfur-containing gas, the service life of a silver-plated reflecting film is prolonged, the layering phenomenon is effectively prevented, and the problems that the existing silver film is general in corrosion resistance, easy to drop a plating layer, large in equipment investment and easy to oxidize are solved.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below.
Example 1
In the embodiment of the invention, the preparation method of the PET silver film comprises the following preparation steps:
the method comprises the following steps: performing oxidation resistance treatment on silver powder
Chemical reduction: adding 300 parts of purified water into a reaction container, and adding 50 parts of silver nitrate under the condition of stirring to completely dissolve the silver nitrate; then 60 parts of purified water is used for dissolving 15 parts of sodium hydroxide to prepare a sodium hydroxide aqueous solution; dropwise adding a sodium hydroxide aqueous solution into a silver nitrate aqueous solution, and after the dropwise adding is finished; immediately dripping 15 parts of formaldehyde solution to carry out chemical reaction for 1 hour, and washing the silver powder;
weighing 5 parts of the silver powder, adding 30 parts of zirconia with the diameter of phi 5mm, filling the mixture into a ball milling tank, adding 7.5 parts of absolute ethyl alcohol as a ball milling solvent, simultaneously adding 0.05 part of oleic acid as an auxiliary agent, setting the rotating speed to 320rpm, carrying out ball milling for 16 hours, and stopping ball milling after the particle size is qualified through sampling detection;
dissolving 0.1 part of silver surface treatment passivator (phosphite) by using a small amount of absolute ethyl alcohol, adding the solution into a ball mill, continuously ball-milling for 30min, discharging, drying at 60 ℃, and dispersing to obtain antioxidant flaky silver powder;
step two: preparing raw materials
Respectively adding 65 parts of polyethylene terephthalate, 15 parts of polybutylene terephthalate, 10 parts of polyethylene naphthalate, 3 parts of copolymerized modified polyester and 20 parts of antioxidant silver powder into a double-screw blender;
step three: and stretching by adopting a biaxial stretching method, and then heating to shape the stretched PET so as to obtain the PET silver film.
And the extrusion temperature in the single-screw extruder in the second step is 270 ℃, which is beneficial to improving the processability and facilitating the subsequent stretching process.
The drying temperature in the third step was 165 ℃.
The longitudinal stretching temperature in the two-way stretching in the third step is 85 ℃, and the transverse stretching temperature is 110 ℃.
The thickness after stretching in the third step is 0.3mm
The setting temperature in the third step is 230 ℃.
The PET silver film effectively prolongs the service life, improves the surface friction resistance, does not need sputtering equipment, saves preparation steps and improves the production efficiency, and the reflectivity of the PET silver film reflecting film at the wavelength of 550nm is more than or equal to 99 percent. Silver surface treatment passivator is added to silver powder, and surface passivation is carried out on flake silver powder through ball-milling mechanical passivation technology, so that a passivation layer is formed on the surface of the silver powder, the oxidation resistance of the silver powder is improved, and the silver powder is protected by filling polyester, so that the silver powder has more excellent corrosion resistance to water vapor, oxygen, halide and sulfur-containing gas, the service life of a silver-plated reflecting film is prolonged, the layering phenomenon is effectively prevented, and the problems that the existing silver film is general in corrosion resistance, easy to drop a plating layer, large in equipment investment and easy to oxidize are solved.
Example 2
A preparation method of a PET silver film comprises the following preparation steps:
the method comprises the following steps: performing oxidation resistance treatment on silver powder
Chemical reduction: adding 200 parts of purified water into a reaction container, and adding 40 parts of silver nitrate under the condition of stirring to completely dissolve the silver nitrate; dissolving 10 parts of sodium hydroxide in 50 parts of purified water to prepare a sodium hydroxide aqueous solution; dropwise adding a sodium hydroxide aqueous solution into a silver nitrate aqueous solution, and after the dropwise adding is finished; immediately dripping 10 parts of formaldehyde solution to carry out chemical reaction for 1 hour, and washing the silver powder;
weighing 3 parts of the silver powder, adding 25 parts of zirconia with the diameter of phi 5mm, filling the mixture into a ball milling tank, adding 5 parts of absolute ethyl alcohol as a ball milling solvent, simultaneously adding 0.05 part of oleic acid as an auxiliary agent, setting the rotating speed to 320rpm, carrying out ball milling for 16 hours, and stopping ball milling after the particle size is qualified through sampling detection;
dissolving 0.1 part of silver surface treatment passivator (phosphite) by using a small amount of absolute ethyl alcohol, adding the solution into a ball mill, continuously ball-milling for 30min, discharging, drying at 60 ℃, and dispersing to obtain antioxidant flaky silver powder;
step two: preparing raw materials
Respectively adding 60 parts of poly (terephthalate), 10 parts of polybutylene terephthalate, 8 parts of polyethylene naphthalate, 2 parts of copolymerized modified polyester and 15 parts of antioxidant silver powder into a double-screw blender;
step three: and stretching by adopting a biaxial stretching method, and then heating to shape the stretched PET so as to obtain the PET silver film.
And the extrusion temperature in the single-screw extruder in the second step is 270 ℃, which is beneficial to improving the processability and facilitating the subsequent stretching process.
The drying temperature in the third step was 165 ℃.
The longitudinal stretching temperature in the bidirectional stretching in the third step is 85 ℃, and the transverse stretching temperature is 110 ℃.
The thickness after stretching in the third step is 0.3mm
The setting temperature in the third step is 230 ℃.
Example 3
A preparation method of a PET silver film comprises the following preparation steps:
the method comprises the following steps: performing oxidation resistance treatment on silver powder
Chemical reduction: adding 400 parts of purified water into a reaction container, and adding 60 parts of silver nitrate under the stirring condition to completely dissolve the silver nitrate; dissolving 20 parts of sodium hydroxide in 70 parts of purified water to prepare a sodium hydroxide aqueous solution; dropwise adding a sodium hydroxide aqueous solution into a silver nitrate aqueous solution, and after the dropwise adding is finished; immediately dropping 20 parts of formaldehyde solution to carry out chemical reaction for 1 hour, and then washing the silver powder;
weighing 7 parts of the silver powder, adding 35 parts of zirconia with the diameter of phi 5mm, filling the mixture into a ball milling tank, adding 10 parts of absolute ethyl alcohol as a ball milling solvent, simultaneously adding 0.05 part of oleic acid as an auxiliary agent, setting the rotating speed to 320rpm, carrying out ball milling for 16 hours, and stopping ball milling after the particle size is qualified through sampling detection;
dissolving 0.1 part of silver surface treatment passivator (phosphite) by using a small amount of absolute ethyl alcohol, adding the solution into a ball mill, continuously ball-milling for 30min, discharging, drying at 60 ℃, and dispersing to obtain antioxidant flaky silver powder;
step two: preparing raw materials
70 parts of poly terephthalate, 20 parts of polybutylene terephthalate, 12 parts of polyethylene naphthalate, 4 parts of copolymerized modified polyester and 25 parts of antioxidant silver powder are respectively added into a double-screw blender;
step three: and stretching by adopting a biaxial stretching method, and then heating to shape the stretched PET so as to obtain the PET silver film.
And the extrusion temperature in the single-screw extruder in the second step is 270 ℃, which is beneficial to improving the processability and facilitating the subsequent stretching process.
The drying temperature in the third step was 165 ℃.
The longitudinal stretching temperature in the two-way stretching in the third step is 85 ℃, and the transverse stretching temperature is 110 ℃. The thickness after stretching in the third step is 0.3mm, and the setting temperature in the third step is 230 ℃.
Claims (6)
1. The preparation method of the PET silver film is characterized by comprising the following preparation steps:
the method comprises the following steps: performing oxidation resistance treatment on silver powder
Chemical reduction: adding 200-400 parts of purified water into a reaction container, and adding 40-60 parts of silver nitrate under the stirring condition to completely dissolve the silver nitrate; dissolving 10-20 parts of sodium hydroxide by using 50-70 parts of purified water to prepare a sodium hydroxide aqueous solution; dropwise adding a sodium hydroxide aqueous solution into a silver nitrate aqueous solution, and after the dropwise adding is finished; immediately dropwise adding 10-20 parts of formaldehyde solution to carry out chemical reaction for 1 hour, and then washing the silver powder;
weighing 3-7 parts of the silver powder, adding 25-35 parts of zirconia with the diameter of phi 5mm, filling the mixture into a ball milling tank, adding 5-10 parts of absolute ethyl alcohol as a ball milling solvent, simultaneously adding 0.05 part of oleic acid as an auxiliary agent, setting the rotating speed of 320rpm for ball milling for 16 hours, and stopping ball milling after the particle size is qualified through sampling detection;
dissolving 0.1 part of silver surface treatment passivator by using a small amount of absolute ethyl alcohol, adding the solution into a ball mill, continuously ball-milling for 30min, discharging, drying at 60 ℃, and dispersing to obtain antioxidant flaky silver powder;
step two: preparing raw materials
Respectively adding 60-70 parts of poly terephthalate, 10-20 parts of polybutylene terephthalate, 8-12 parts of polyethylene naphthalate, 2-4 parts of copolymerized modified polyester and 15-25 parts of antioxidant silver powder into a double-screw blender;
step three: and stretching by adopting a biaxial stretching method, and then heating to shape the stretched PET so as to obtain the PET silver film.
2. The method for preparing a PET silver film according to claim 1, wherein the extrusion temperature in the single-screw extruder in the second step is 270 ℃.
3. The method for preparing a PET silver film according to claim 1, wherein the drying temperature in the third step is 165 ℃.
4. The method for preparing a PET silver film according to claim 1, wherein the longitudinal stretching temperature in the three-step biaxial stretching is 85 ℃ and the transverse stretching temperature is 110 ℃.
5. The method for preparing a PET silver film according to claim 1, wherein the thickness of the PET silver film after stretching in the third step is 0.3 mm.
6. The method for preparing a PET silver film according to claim 1, wherein the setting temperature in the third step is 230 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210661314.0A CN114874593A (en) | 2022-06-13 | 2022-06-13 | Preparation method of PET silver film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210661314.0A CN114874593A (en) | 2022-06-13 | 2022-06-13 | Preparation method of PET silver film |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN114874593A true CN114874593A (en) | 2022-08-09 |
Family
ID=82680653
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210661314.0A Pending CN114874593A (en) | 2022-06-13 | 2022-06-13 | Preparation method of PET silver film |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114874593A (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105880632A (en) * | 2016-06-14 | 2016-08-24 | 深圳市中金岭南科技有限公司 | Method for preparing oxidation-resistant flaky silver powder |
| CN113752514A (en) * | 2021-09-03 | 2021-12-07 | 宁波东旭成新材料科技有限公司 | Preparation method of Mini-LED backlight module optical reflection film |
-
2022
- 2022-06-13 CN CN202210661314.0A patent/CN114874593A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105880632A (en) * | 2016-06-14 | 2016-08-24 | 深圳市中金岭南科技有限公司 | Method for preparing oxidation-resistant flaky silver powder |
| CN113752514A (en) * | 2021-09-03 | 2021-12-07 | 宁波东旭成新材料科技有限公司 | Preparation method of Mini-LED backlight module optical reflection film |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| TW556005B (en) | Phase difference plate formed by a rod compound-containing polymer film | |
| EP3300084B1 (en) | Transparent conductor | |
| WO2008105597A1 (en) | Transparent electrode for solar cell and manufacturing method thereof | |
| CN113299426B (en) | Transparent conductive barrier film, preparation method and application thereof | |
| EP1905864A1 (en) | In Sm OXIDE SPUTTERING TARGET | |
| Dong et al. | Fabrication of high-quality flexible transparent conductive thin films with a Nb2O5/AgNWs/Nb2O5 sandwich structure | |
| CN114874593A (en) | Preparation method of PET silver film | |
| CN102168246A (en) | Large-area high-uniformity transparent conducting film deposited on flexible substrate and preparation method thereof | |
| CN111217539A (en) | Coating process of optical glass | |
| CN111018363A (en) | ITO thin film glass capable of improving electromagnetic shielding effect and preparation method thereof | |
| CN1171241C (en) | Conductive nitride film, process for producing the same, and antireflection object | |
| CN115050505A (en) | High-corrosion-resistance transparent conductive film and preparation method thereof | |
| CN111916252A (en) | Transparent conductive film with low sheet resistance | |
| JPH06251632A (en) | Transparent conductive film having high flexibility and manufacture thereof | |
| CN203535978U (en) | ITO (Indium Tin Oxide) conducting film for touch screen | |
| CN212392013U (en) | Transparent conductive film with low sheet resistance | |
| CN212392012U (en) | Low sheet resistance transparent conductive film | |
| CN114574820A (en) | Indium-zinc-tin oxide sputtering target and conductive film thereof | |
| CN111883287A (en) | Low-sheet-resistance transparent conductive film | |
| JP2000082337A (en) | Transparent conductive film, transparent touch panel, and liquid crystal display element | |
| JPH10208554A (en) | Transparent conductive film and liquid crystal element using the same | |
| KR101060994B1 (en) | Method for manufacturing ito thin film with high-transmittance | |
| CN114188446B (en) | Conductive glass and preparation method and application thereof | |
| KR20030031809A (en) | Method for manufacturing polarization plate, and liquid crystal display device | |
| CN115074666B (en) | Preparation method of multilayer composite ITO film |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20220809 |