CN113478110B - Protection film used for laser cutting of silver mirror glass and not compounded from release film - Google Patents
Protection film used for laser cutting of silver mirror glass and not compounded from release film Download PDFInfo
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- CN113478110B CN113478110B CN202110811387.9A CN202110811387A CN113478110B CN 113478110 B CN113478110 B CN 113478110B CN 202110811387 A CN202110811387 A CN 202110811387A CN 113478110 B CN113478110 B CN 113478110B
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- laser cutting
- silver mirror
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- 239000011521 glass Substances 0.000 title claims abstract description 55
- 238000003698 laser cutting Methods 0.000 title claims abstract description 55
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 47
- 239000004332 silver Substances 0.000 title claims abstract description 47
- 230000001681 protective effect Effects 0.000 claims abstract description 136
- 239000010410 layer Substances 0.000 claims abstract description 79
- 239000002346 layers by function Substances 0.000 claims abstract description 41
- 239000000758 substrate Substances 0.000 claims abstract description 33
- 239000012790 adhesive layer Substances 0.000 claims abstract description 31
- 229920002050 silicone resin Polymers 0.000 claims abstract description 29
- 239000000463 material Substances 0.000 claims abstract description 25
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 24
- HLXDKGBELJJMHR-UHFFFAOYSA-N methyl-tri(propan-2-yloxy)silane Chemical group CC(C)O[Si](C)(OC(C)C)OC(C)C HLXDKGBELJJMHR-UHFFFAOYSA-N 0.000 claims abstract description 24
- 150000004756 silanes Chemical class 0.000 claims abstract description 24
- 239000002131 composite material Substances 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 11
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- 238000002360 preparation method Methods 0.000 claims description 25
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- 238000001035 drying Methods 0.000 claims description 11
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 10
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- XOFYZVNMUHMLCC-ZPOLXVRWSA-N prednisone Chemical compound O=C1C=C[C@]2(C)[C@H]3C(=O)C[C@](C)([C@@](CC4)(O)C(=O)CO)[C@@H]4[C@@H]3CCC2=C1 XOFYZVNMUHMLCC-ZPOLXVRWSA-N 0.000 description 16
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- JNVLFUCEKYADLU-UHFFFAOYSA-N 3,4,6-trimethoxy-3h-2-benzofuran-1-one Chemical compound COC1=CC(OC)=C2C(OC)OC(=O)C2=C1 JNVLFUCEKYADLU-UHFFFAOYSA-N 0.000 description 10
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- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 229910052782 aluminium Inorganic materials 0.000 description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 6
- 229910021641 deionized water Inorganic materials 0.000 description 6
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- 229910002027 silica gel Inorganic materials 0.000 description 6
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 6
- 239000007787 solid Substances 0.000 description 6
- 229910052727 yttrium Inorganic materials 0.000 description 6
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 6
- 238000005520 cutting process Methods 0.000 description 5
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 5
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- WOBHKFSMXKNTIM-UHFFFAOYSA-N Hydroxyethyl methacrylate Chemical compound CC(=C)C(=O)OCCO WOBHKFSMXKNTIM-UHFFFAOYSA-N 0.000 description 3
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 239000002390 adhesive tape Substances 0.000 description 3
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 description 3
- 239000003431 cross linking reagent Substances 0.000 description 3
- LQZZUXJYWNFBMV-UHFFFAOYSA-N dodecan-1-ol Chemical compound CCCCCCCCCCCCO LQZZUXJYWNFBMV-UHFFFAOYSA-N 0.000 description 3
- 125000004494 ethyl ester group Chemical group 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000003999 initiator Substances 0.000 description 3
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- LVQPBIMCRZQQBC-UHFFFAOYSA-N methoxymethyl 2-methylprop-2-enoate Chemical compound COCOC(=O)C(C)=C LVQPBIMCRZQQBC-UHFFFAOYSA-N 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
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- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
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- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
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Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K26/00—Working by laser beam, e.g. welding, cutting or boring
- B23K26/70—Auxiliary operations or equipment
- B23K26/702—Auxiliary equipment
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K26/00—Working by laser beam, e.g. welding, cutting or boring
- B23K26/36—Removing material
- B23K26/38—Removing material by boring or cutting
Landscapes
- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Plasma & Fusion (AREA)
- Mechanical Engineering (AREA)
- Laminated Bodies (AREA)
- Adhesive Tapes (AREA)
Abstract
The invention discloses a protective film for laser cutting of silver mirror glass, which is a non-composite release film; the film comprises a functional layer, a film substrate layer, an adhesive layer and a silicone resin layer; the adhesive layer is covered on one side of the film substrate; the functional layer is covered on the other side of the film substrate layer; wherein, the surface of the glue layer is covered with a silicone resin layer formed by silicone resin containing a modified silane coupling agent; wherein the modified silane coupling agent is methyl triisopropoxysilane modified by N-benzoyl quinine tert-butyl ester; the obtained protective film has excellent heat resistance, water resistance and stain resistance, and can be used for laser cutting of silver mirror glass, so that the damage of pollutants such as gasification smoke dust, combustion melting slag and the like generated in the laser cutting process to the silver mirror glass can be effectively prevented, and a product with high excellent rate is obtained; meanwhile, the protective film can absorb low-energy light focused on the periphery of a light spot by a laser beam, so that the line width of a heat affected zone on the upper surface of a cut material is reduced, and the processing precision of a processed device is improved.
Description
Technical Field
The invention belongs to the technical field of packaging materials, and particularly relates to a protective film of a non-composite release film for laser cutting of silver mirror glass.
Background
At present, the laser cutting technology becomes a mature industrial processing technology. Metals are the main object of laser cutting, and other materials capable of laser cutting include plastics, ceramics, silicon wafers, glass and the like. As glass is increasingly widely used, requirements of certain applications on cutting quality and cutting yield are very strict, and the traditional glass cutting technology can not meet production requirements gradually. Such as high temperature resistant, high hardness borosilicate glass as a TFT-LCD substrate, and tempered glass for use in automobiles, etc. The laser cutting technology of glass is well researched, and the superiority of laser cutting is gradually known. Compared with the traditional cutting technology, the laser cutting technology for the glass has many advantages, the edge of the glass cut by the laser is smooth, has no transverse micro-crack and no fragment, the scratch on the plate is avoided, and the possibility of glass breakage is reduced to the minimum degree. However, pollutants such as gasified smoke dust, fuel melting slag and the like generated in the laser cutting process splash on the surface of the flexible film material to form a large number of polluted scars, and the large number of polluted scars are very difficult to remove, and even if the pollutants are blown or wiped by compressed gas after the laser cutting, the pollutants cannot be completely removed; therefore, it is important to coat a protective film on the surface of the glass material.
The prior art, for example, publication No. CN 108817700 a discloses a protective film and a laser cutting method; the laser absorption rate of the target area in the protective film is smaller than a preset threshold value, the protective film is configured to be attached to the target surface of the substrate, when the substrate is subjected to laser cutting, the protective film keeps the film layer complete and transmits laser beams through the target area, so that the substrate is split along the area irradiated by the laser beams, the problem that the excellent rate of the substrate obtained through laser cutting is low is solved, and the excellent rate of the substrate obtained through laser cutting is improved. l
Disclosure of Invention
The invention aims to provide a protective film with excellent heat resistance, water resistance and stain resistance, which is used for laser cutting of silver mirror glass and can effectively prevent the silver mirror glass from being damaged by pollutants such as gasified smoke dust, combustion melting slag and the like generated in the laser cutting process, so that a product with high excellent rate is obtained; meanwhile, the protective film can absorb low-energy light focused on the periphery of a light spot by a laser beam, so that the line width of a heat affected zone on the upper surface of a cut material is reduced, and the processing precision of a processed device is improved.
The technical scheme adopted by the invention for realizing the purpose is as follows:
a protective film, comprising: the functional layer, the film substrate layer, the adhesive layer and the silicone resin layer; the adhesive layer is covered on one side of the film substrate; the functional layer is covered on the other side of the film substrate layer; wherein,
the surface of the adhesive layer is coated with a silicone resin layer formed by silicone resin containing a modified silane coupling agent;
the modified silane coupling agent is methyl triisopropoxysilane modified by N-benzoyl quinine tert-butyl ester.
According to the invention, N-benzoyl quinine tert-butyl ester modified methyl triisopropoxysilane is adopted as a silicone resin layer component on the upper surface of a glue layer in a protective film, and the protective film is prepared from the silicone resin layer component, the film substrate layer component, the glue layer component and a functional layer; the silver mirror glass laser cutting device is used for laser cutting of silver mirror glass, and can effectively prevent the silver mirror glass from being damaged by pollutants such as gasified smoke dust and combustion melting slag generated in the laser cutting process, so that the line width of a heat affected zone on the upper surface of a cut material is reduced, the processing precision of a processed device is improved, and a product with high yield is obtained; meanwhile, the protective film can absorb low-energy light focused on the periphery of a light spot by a laser beam, so that the line width of a heat affected zone on the upper surface of a cut material is reduced, the processing precision of a processed device is improved, and the protective film has good waterproof stain resistance and heat resistance; by adopting a special anti-sticking technology, after the protective film is stuck on the silver mirror glass, the back surface of the protective film is fixed by a double-sided adhesive tape without falling off, and the protective film has better service performance.
Preferably, in some embodiments of the present invention, the functional layer is a thin film formed by a mixture of an alumina/yttria composite sol and a thermoplastic resin, and the functional layer has an excellent absorption effect on a low-energy laser beam, so that a line width of a heat affected zone on the upper surface of the cut material is reduced, and the processing precision of the processed device is improved.
Preferably, in some embodiments of the present invention, the film substrate layer is at least one of polyethylene terephthalate, polyurethane, polyethylene, and polyimide.
Preferably, in some embodiments of the present invention, the adhesive layer is an acrylate pressure sensitive adhesive, so that it has a better adhesive effect with the film substrate.
The invention also discloses application of the protective film in laser cutting of silver mirror glass.
The invention also discloses a preparation method of the protective film for laser cutting of the silver mirror glass, which is a non-composite release film, and the preparation method comprises the following steps:
coating a coating mixed solution for preparing acrylate pressure-sensitive adhesive on one side of the film base material layer to obtain an adhesive layer;
coating the silicone resin emulsion containing the modified silane coupling agent on the upper surface of the adhesive layer, and drying to obtain a silicone resin layer;
preparing a coating mixed solution from the alumina/yttria composite sol and thermoplastic resin, coating the coating mixed solution on the other side of the membrane substrate layer, drying to obtain a functional layer, and finishing to obtain the protective membrane.
Preferably, in some embodiments of the present invention, the thickness of the protective film is 50 to 90 μm, and the thickness of the adhesive layer is 15 to 20 μm; the thickness of the silicone resin layer is 1-4 mu m; the thickness of the functional layer is 1.8-2.4 mu m.
Preferably, in some embodiments of the present invention, the modified silane coupling agent is prepared by: putting N-benzoyl quinine tert-butyl ester, a solvent and a catalyst in parts by weight into a reactor for catalyst activation; and adding methyl triisopropoxysilane into a reactor for reaction, and performing rotary evaporation and recrystallization to obtain the modified silane coupling agent.
More preferably, in some embodiments of the present invention, the N-benzoyl quinine tert-butyl ester is 4-7 parts by weight, the solvent is 150-200 parts by weight, the catalyst is 0.15-0.25 part by weight, and the methyl triisopropoxysilane is 2.5-4.5 parts by weight.
The invention also discloses application of the 3,4, 6-trimethoxy-1 (3H) -isobenzofuranone in improving the fingerprint resistance of the protective film.
According to the invention, N-benzoyl quinine tert-butyl ester modified methyl triisopropoxysilane is adopted as a silicone resin layer component on the upper surface of an adhesive layer in the protective film, and the protective film is prepared from the silicone resin layer component, the film substrate layer component, the adhesive layer component and a functional layer, so that the protective film has the following beneficial effects: the protective film is used for laser cutting of the silver mirror glass, and can effectively prevent the silver mirror glass from being damaged by pollutants such as gasified smoke dust, combustion melting slag and the like generated in the laser cutting process, so that a product with high excellent rate is obtained; meanwhile, the protective film can absorb low-energy light focused on the periphery of a light spot by a laser beam, so that the line width of a heat affected zone on the upper surface of a cut material is reduced, the processing precision of a processed device is improved, and the protective film has good waterproof stain resistance and heat resistance; by adopting a special anti-sticking technology, after the protective film is stuck on the silver mirror glass, the back surface of the protective film is fixed by a double-sided adhesive tape without falling off, and the protective film has better service performance.
Therefore, the protective film with excellent heat resistance, water resistance and stain resistance is used for laser cutting of the silver mirror glass, can effectively prevent the silver mirror glass from being damaged by pollutants such as gasified smoke dust, fuel slag and the like generated in the laser cutting process, and can obtain a product with high excellent rate; meanwhile, the protective film can absorb low-energy light focused on the periphery of a light spot by a laser beam, so that the line width of a heat affected zone on the upper surface of a cut material is reduced, and the processing precision of a processed device is improved.
Drawings
FIG. 1 is a schematic structural diagram of a protective film;
FIG. 2 is an infrared spectrum of the modified silane coupling agent of example 1;
FIG. 3 is a surface topography of the protective film of example 2;
FIG. 4 shows the line width change rate of the heat affected zone of the silver mirror glass laser cutting.
Reference numerals: 1. a functional layer; 2. a film substrate layer; 3. a glue layer; 4. a silicone layer.
Detailed Description
The experimental methods described in the following examples of the present invention are all conventional methods unless otherwise specified; the reagents and materials are commercially available, unless otherwise specified.
Specifically, a method for producing each component of the protective film according to the present invention will be described.
Preferably, in some embodiments of the present invention, the acrylate pressure sensitive adhesive is prepared as follows:
placing 2-4 parts by weight of acrylic acid, 5-10 parts by weight of butyl acrylate, 3-5 parts by weight of lauryl alcohol methacrylate, 2.5-4.5 parts by weight of methyl methacrylate, 2-3 parts by weight of hydroxyethyl methacrylate, 3-6 parts by weight of methoxy methyl methacrylate, 5-9 parts by weight of isoprene rubber containing double bonds and 40-70 parts by weight of solvent (10-25 parts by weight of acetone, 15-25 parts by weight of toluene and 15-20 parts by weight of ethyl ester) in a reaction container, and continuously stirring and raising the temperature to 70-85 ℃ for reaction for 2-4 hours; and then uniformly mixing 0.25-0.55 part of BPO initiator with the rest of solvent, slowly dripping the mixture into the reaction container, continuously stirring, continuously reacting for 3-4 h under the condition of keeping the reaction temperature unchanged, and cooling to room temperature to obtain the acrylate pressure-sensitive adhesive.
More preferably, the preparation method of the glue layer comprises the following steps: uniformly mixing the obtained acrylate pressure-sensitive adhesive and a cross-linking agent according to a weight ratio of 90-105: 1, coating one side of a film substrate by adopting a coating rod coating method, curing for 20-30 min at 70-85 ℃, and cooling to room temperature to obtain a glue layer, wherein the thickness of the glue layer is 15-20 mu m.
Preferably, in some embodiments of the present invention, the silicone layer is prepared by: according to parts by weight, 80-90 parts of hydroxyl-terminated dimethylvinyl (siloxane and polysiloxane) (purchased from Hubei ferry chemical Co., Ltd.), 2.5-4.5 parts of hydrogen-terminated poly (dimethylsiloxane) (purchased from Hubei ferry chemical Co., Ltd.), and 0.65-1.5 parts of modified silane coupling agent are placed in 200-250 parts of toluene to be diluted to obtain a silica gel emulsion, the silica gel emulsion is coated on the surface of a glue layer by adopting a coating rod coating method, and the glue layer is dried at 70-85 ℃ for 20-30 min until water is completely volatilized to obtain a silica resin layer, wherein the thickness of the silica resin layer is 1-4 mu m, and the silica resin layer is in contact with a product to be processed.
Further preferably, in some embodiments of the present invention, the modified silane coupling agent is prepared by: adding 4-7 parts by weight of N-benzoyl quinine tert-butyl ester into a reaction container, introducing nitrogen for protection reaction, adding 150-200 parts by weight of toluene as a solvent, raising the reaction temperature to 50-60, adding 0.15-0.25 part by weight of karstedt catalyst, and continuing stirring for 30-60 min to activate the catalyst; and then 2.5-4.5 parts of methyl triisopropoxysilane (purchased from Hangzhou tin chemical Co., Ltd., content of more than or equal to 99%) is added into a constant-pressure dropping funnel, and then the mixture is slowly dripped into the solution, after the dripping is finished, the temperature is raised to 60-80 ℃ to react for 1-3 days, impurities in the liquid are filtered off by suction when the solution is hot, then the solution is cooled to room temperature, toluene is removed by rotary evaporation, and recrystallization is carried out to obtain the modified silane coupling agent, wherein the yield is 36.9-43.7%.
Preferably, in some embodiments of the present invention, the functional layer is prepared by: uniformly mixing aluminum sol (purchased from Zibo Sime chemical engineering Co., Ltd.), silica sol (purchased from Shandong Liong New Material science and technology Co., Ltd., content of more than or equal to 99%), yttrium sol (purchased from Dalian Snoo chemical New Material science and technology Co., Ltd., content of more than or equal to 99%) and deionized water according to the weight ratio of 2-4: 1-1.5: 0.5-1: 20-30 to obtain an inorganic metal oxide mixed solution, uniformly mixing 10-20 parts of the mixed solution and 5-8 parts of polyamide aqueous dispersion (solid content of 12.5-17.5%), coating the mixed solution on the other side (opposite to the adhesive layer and the silicon resin layer) of a film substrate by a coating rod coating method, and drying the mixed solution at 70-85 ℃ for 20-30 min until water is completely volatilized to obtain a functional layer, wherein the thickness of the functional layer is 1.8-2.4 mu m. The functional layer can prevent the protective film from being adhered to a processing device on one hand; on the other hand, during laser cutting, certain laser can be absorbed, peripheral low-energy beams can be absorbed, the diameter of a laser focusing spot can be reduced, and the width of a cutting line can be reduced.
More preferably, in order to further improve the absorption of the laser beam and the water-and stain-resistant properties of the protective film while providing the protective film with excellent fingerprint resistance, preferable measures are taken which further comprise:
0.2-0.5 part of 3,4, 6-trimethoxy-1 (3H) -isobenzofuranone is added into the functional layer, and is uniformly mixed with the inorganic metal oxide mixed solution and the polyamide aqueous dispersion liquid, so that the absorption effect on laser beams is further improved; meanwhile, the protective film has better waterproof stain resistance and fingerprint resistance; the reason is probably that the 3,4, 6-trimethoxy-1 (3H) -isobenzofuranone is mixed with the inorganic metal oxide mixed solution and the polyamide aqueous dispersion liquid, so that the dispersion uniformity is improved, and the three have synergistic action, so that the comprehensive performance of the protective film is improved.
The schematic structural diagram of the protective film of the present invention is shown in fig. 1, and includes: functional layer 1, membrane substrate layer 2, glue film 3 and silicone layer 4.
The technical solution of the present invention is further described in detail below with reference to the following detailed description and the accompanying drawings:
example 1
A preparation method of a protective film of a non-composite release film for laser cutting of silver mirror glass comprises the following steps:
preparing an adhesive layer: according to parts by weight, 2.2 parts of acrylic acid, 6.5 parts of butyl acrylate, 3.5 parts of lauryl alcohol methacrylate, 2.5 parts of methyl methacrylate, 2 parts of hydroxyethyl methacrylate, 3 parts of methoxy methyl methacrylate, 5 parts of isoprene rubber containing double bonds and 55 parts of solvent (15 parts of acetone, 20 parts of toluene and 20 parts of ethyl ester) are placed in a reaction vessel and continuously stirred until the temperature is raised to 75 ℃ for reaction for 3 hours; and then uniformly mixing 0.25 part of BPO initiator with the rest of solvent, slowly dripping the mixture into the reaction container, continuously stirring, continuously reacting for 3 hours under the condition of keeping the reaction temperature unchanged, and cooling to room temperature to obtain the acrylate pressure-sensitive adhesive. Uniformly mixing the obtained acrylate pressure-sensitive adhesive with a Bayer RE cross-linking agent according to a weight ratio of 100:1, coating one side of a film substrate (made of polyethylene terephthalate) by a coating rod coating method, curing for 25min at 75 ℃, and cooling to room temperature to obtain an adhesive layer, wherein the thickness of the adhesive layer is 15.7 mu m.
Preparation of the silicone resin layer: placing 80 parts of hydroxyl-terminated dimethylvinyl (siloxane and polysiloxane), 2.5 parts of hydrogen-terminated poly (dimethylsiloxane) and 0.65 part of modified silane coupling agent in 200 parts of toluene for dilution to obtain a silica gel emulsion, coating the silica gel emulsion on the surface of a glue layer by adopting a coating rod coating method, and drying at 75 ℃ for 30min until moisture is completely volatilized to obtain a silica resin layer, wherein the thickness of the silica resin layer is 1.2 mu m;
preparation of the functional layer: uniformly mixing aluminum sol, silica sol, yttrium sol and deionized water according to the weight ratio of 2:1:0.5:20 to obtain an inorganic metal oxide mixed solution, uniformly mixing 10 parts of the mixed solution with 5 parts of a polyamide aqueous dispersion (the solid content is 12.5%), coating the mixed solution on the other side (opposite to the glue layer and the silicon resin layer) of a membrane substrate by adopting a coating rod coating method, and drying at 75 ℃ for 30min until the moisture is completely volatilized to obtain a functional layer, wherein the thickness of the functional layer is 2.1 mu m; the protective film was obtained after completion of the fabrication, and had a thickness of 55 μm.
In this embodiment, the preparation method of the modified silane coupling agent comprises: adding 4.5 parts of N-benzoyl quinine tert-butyl ester into a reaction vessel, introducing nitrogen for protection reaction, then adding 150 parts of toluene as a solvent, raising the reaction temperature to 55 ℃, then adding 0.15 part of karstedt catalyst, and continuing stirring for 40min to activate the catalyst; and adding 2.5 parts of methyl triisopropoxysilane into a constant-pressure dropping funnel, slowly dropwise adding into the solution, heating to 60 ℃ after dropwise adding, reacting for 2 days, filtering to remove impurities in the liquid by suction while the liquid is hot, cooling to room temperature, removing toluene by rotary evaporation, and recrystallizing to obtain the modified silane coupling agent with the yield of 37.2%.
Example 2
The preparation method of the protective film for laser cutting of the silver mirror glass is characterized in that the other steps of the protective film are the same as those of the embodiment 1, and the protective film is different from the embodiment 1 in that:
preparing an adhesive layer: according to the parts by weight, 3.6 parts of acrylic acid, 6.5 parts of butyl acrylate, 4.5 parts of lauryl alcohol methacrylate, 3.2 parts of methyl methacrylate, 2.5 parts of hydroxyethyl methacrylate, 3.5 parts of methoxy methyl methacrylate, 6 parts of isoprene rubber containing double bonds and 60 parts of solvent (wherein 15 parts of acetone, 25 parts of toluene and 20 parts of ethyl ester) are placed in a reaction container, and are continuously stirred and heated to 80 ℃ for reaction for 3 hours; and then uniformly mixing 0.45 part of BPO initiator with the rest solvent, slowly dripping the mixture into the reaction container, continuously stirring, continuously reacting for 3 hours under the condition of keeping the reaction temperature unchanged, and cooling to room temperature to obtain the acrylate pressure-sensitive adhesive. Uniformly mixing the obtained acrylate pressure-sensitive adhesive with a Bayer RE cross-linking agent according to a weight ratio of 100:1, coating the mixture on one side of a film substrate (made of polyethylene), curing the mixture for 20min at 80 ℃, and cooling the mixture to room temperature to obtain an adhesive layer, wherein the thickness of the adhesive layer is 17.2 mu m.
Example 3
The preparation method of the protective film for laser cutting of the silver mirror glass, which is not a composite release film, comprises the following steps of the same steps as those in the embodiment 2, and is different from the embodiment 2:
preparation of the silicone resin layer: 90 parts of hydroxyl-terminated dimethylvinyl (siloxane and polysiloxane), 3.5 parts of hydrogen-terminated poly (dimethylsiloxane) and 1 part of modified silane coupling agent are diluted in 230 parts of toluene to obtain a silica gel emulsion, the silica gel emulsion is coated on the surface of a glue line by a coating rod coating method, and the glue line is dried at 80 ℃ for 20min until the moisture is completely volatilized to obtain a silica resin layer, wherein the thickness of the silica resin layer is 2.6 mu m.
Example 4
The preparation method of the protective film for laser cutting of the silver mirror glass, which is not a composite release film, comprises the following steps of the same steps as those in the embodiment 2, and is different from the embodiment 2:
in this embodiment, the preparation method of the modified silane coupling agent comprises: adding 6.5 parts of N-benzoyl quinine tert-butyl ester into a reaction vessel, introducing nitrogen for protection reaction, then adding 200 parts of toluene as a solvent, raising the reaction temperature to 60 ℃, then adding 0.25 part of karstedt catalyst, and continuing stirring for 60min to activate the catalyst; and adding 4.5 parts of methyl triisopropoxysilane into a constant pressure dropping funnel, slowly dropwise adding into the solution, heating to 70 ℃ after dropwise adding, reacting for 2 days, filtering to remove impurities in the liquid by suction while the liquid is hot, cooling to room temperature, removing toluene by rotary evaporation, and recrystallizing to obtain the modified silane coupling agent with the yield of 42.5%.
Example 5
The preparation method of the protective film for laser cutting of the silver mirror glass, which is not a composite release film, comprises the following steps of the same steps as those in the embodiment 2, and is different from the embodiment 2:
preparation of the functional layer: uniformly mixing aluminum sol, silica sol, yttrium sol and deionized water according to a weight ratio of 3:1:1:30 to obtain an inorganic metal oxide mixed solution, uniformly mixing 20 parts of the mixed solution with 7 parts of a polyamide aqueous dispersion liquid (the solid content is 15%), coating the mixed solution on the other side (opposite to the glue layer and the silica resin layer) of a film substrate (made of polyethylene terephthalate) by adopting a coating rod coating method, and drying at 80 ℃ for 20min until the moisture is completely volatilized to obtain a functional layer, wherein the thickness of the functional layer is 2.3 mu m; the protective film was obtained after the completion of the production, and had a thickness of 64.9 μm.
Example 6
The preparation method of the protective film for laser cutting of the silver mirror glass, which is not a composite release film, comprises the following steps of the same steps as those in the embodiment 2, and is different from the embodiment 2:
preparation of the functional layer: uniformly mixing aluminum sol, silica sol, yttrium sol and deionized water according to a weight ratio of 2:1:0.5:20 to obtain an inorganic metal oxide mixed solution, uniformly mixing 10 parts of the mixed solution with 5 parts of polyamide aqueous dispersion (with the solid content of 12.5%) and 0.2 part of 3,4, 6-trimethoxy-1 (3H) -isobenzofuranone, coating the mixed solution on the other side (opposite to the adhesive layer and the silica resin layer) of a film substrate (made of polyethylene terephthalate) by a coating rod coating method, and drying at 75 ℃ for 30min until the moisture is completely volatilized to obtain a functional layer, wherein the thickness of the functional layer is 1.9 mu m; the protective film was obtained after completion of the fabrication, and had a thickness of 55 μm.
Example 7
The preparation method of the protective film for laser cutting of the silver mirror glass, which is not a composite release film, comprises the following steps of the same steps as those in the embodiment 2, and is different from the embodiment 2:
preparation of the functional layer: uniformly mixing aluminum sol, silica sol, yttrium sol and deionized water according to a weight ratio of 2:1:0.5:20 to obtain an inorganic metal oxide mixed solution, uniformly mixing 10 parts of the mixed solution with 5 parts of polyamide aqueous dispersion (with the solid content of 12.5%) and 0.35 part of 3,4, 6-trimethoxy-1 (3H) -isobenzofuranone, coating the mixed solution on the other side (opposite to the adhesive layer and the silica resin layer) of a film substrate (made of polyethylene terephthalate) by a coating rod coating method, and drying at 75 ℃ for 30min until the moisture is completely volatilized to obtain a functional layer, wherein the thickness of the functional layer is 2.3 mu m; the protective film was obtained after completion of the fabrication, and had a thickness of 55 μm.
Example 8
The preparation method of the protective film for laser cutting of the silver mirror glass, which is not a composite release film, comprises the following steps of the same steps as those in the embodiment 2, and is different from the embodiment 2:
preparation of the functional layer: uniformly mixing aluminum sol, silica sol, yttrium sol and deionized water according to a weight ratio of 2:1:0.5:20 to obtain an inorganic metal oxide mixed solution, uniformly mixing 10 parts of the mixed solution with 5 parts of polyamide aqueous dispersion (with the solid content of 12.5%) and 0.5 part of 3,4, 6-trimethoxy-1 (3H) -isobenzofuranone, coating the mixed solution on the other side (opposite to the adhesive layer and the silica resin layer) of a film substrate (made of polyethylene terephthalate) by a coating rod coating method, and drying at 75 ℃ for 30min until the moisture is completely volatilized to obtain a functional layer, wherein the thickness of the functional layer is 2.3 mu m; the protective film was obtained after completion of the fabrication, and had a thickness of 55 μm.
Example 9
The preparation method of the protective film for laser cutting of the silver mirror glass, which is not a composite release film, comprises the following steps of the same steps as those in the embodiment 7, and is different from the embodiment 7:
preparation of the silicone resin layer: 80 parts of hydroxyl-terminated dimethylvinyl (siloxane and polysiloxane), 2.5 parts of hydrogen-terminated poly (dimethylsiloxane) and 0.65 part of methyl triisopropoxysilane were diluted in 200 parts of toluene to obtain a silicone emulsion, which was coated on the surface of a rubber layer by a coating bar coating method, and dried at 75 ℃ for 30min until the moisture was completely volatilized to obtain a silicone layer, wherein the thickness of the silicone layer was 1.2. mu.m.
Comparative example 1
The preparation method of the protective film for laser cutting of the silver mirror glass, which is not a composite release film, comprises the following steps of the same steps as those in the embodiment 2, and is different from the embodiment 2:
preparation of the silicone resin layer: 80 parts of hydroxyl-terminated dimethylvinyl (siloxane and polysiloxane), 2.5 parts of hydrogen-terminated poly (dimethylsiloxane) and 0.65 part of methyl triisopropoxysilane were diluted in 200 parts of toluene to obtain a silicone emulsion, which was coated on the surface of a rubber layer by a coating bar coating method, and dried at 75 ℃ for 30min until the moisture was completely volatilized to obtain a silicone layer, wherein the thickness of the silicone layer was 1.2. mu.m.
Test example 1
Infrared spectroscopic measurement of modified silane coupling agent
Fourier transform Infrared Spectroscopy (FTS-3000 Fourier Infrared absorption Spectroscopy, Bio-Rad, UK) was used. The wave number range used in the test is 4000--1。
FIG. 2 shows a modification of example 1Infrared spectra of front and back methyl triisopropoxysilane. Curves a and b are respectively infrared spectrograms of the methyl triisopropoxysilane and the modified methyl triisopropoxysilane; as can be seen from FIG. 2, the infrared spectrum of the modified methyltriisopropoxysilane was 2894.6cm relative to that of the unmodified methyltriisopropoxysilane-1The nearby characteristic absorption peak is enhanced, which is the stretching vibration of the alkane; at 1734.7cm-1The characteristic absorption peak appearing nearby is the stretching vibration of the ester group; at 1705.3cm-1The characteristic absorption peak appearing nearby is stretching vibration of a ketone group; thus, it was found that a modified silane coupling agent was obtained by modifying methyl triisopropoxysilane with N-benzoyl quinine tert-butyl ester.
Test example 2
Measurement of surface morphology of protective film
The surface morphology of the sample of the protective film material was analyzed using a model SSX-550 scanning electron microscope.
FIG. 3 is a surface topography of the protective film of example 2. As can be seen from FIG. 3, the surface of the protective film material in example 2 has no obvious holes, and the structure is dense and uniform.
Test example 3
Determination of Heat resistance of protective film
Heating and baking the protective film in a hot-blast stove at 300 deg.C for 30min, measuring the color difference values delta L, delta a and delta b before and after heating and baking by a color difference meter, and calculating delta E (delta L)2+△a2+△b2)1/2And judging the heat resistance of the protective film according to the value of Delta E, wherein the Delta E<4, the film material has excellent heat resistance; the test results are shown in table 1.
Table 1 Δ E value test results for protective films
As can be seen from Table 1, the Δ E values of the protective films of examples 1 to 5 were less than 0.5 at 250 ℃, and the color of the protective film was not substantially changed; at 300 ℃, the delta E value of the protective film is lower than 1.3, and the color does not change obviously or turn yellow slightly, namely the protective film has excellent heat resistance; comparing example 2 with comparative example 1, the delta E value of the protective film in example 2 is lower than that in comparative example 1 at 250 ℃ and 300 ℃, which shows that N-benzoyl quinine tert-butyl ester modified methyl triisopropoxysilane is used as a silicone resin layer component on the upper surface of the glue layer in the protective film, the heat resistance of the protective film is improved, and the protective film can bear the temperature below 300 ℃; the Δ E values of the protective films of examples 6 to 8 were not higher than 0.12 at 250 ℃, the Δ E values of the protective films were lower than 0.4 at 300 ℃, the colors of the protective films were hardly changed, comparative examples 2 and 7, and examples 9 and 1, the Δ E values of the protective films of example 7 were not significantly different from example 2 at 250 ℃ and 300 ℃, and the Δ E values of the protective films of example 9 were also not significantly different from comparative example 1, which indicates that the addition of 3,4, 6-trimethoxy-1 (3H) -isobenzofuranone to the functional layers of the protective films had no significant effect on the heat resistance of the protective films.
Test example 4
Measurement of fingerprint resistance of protective film
Dipping a small amount of clean cotton balls on about one half of the surface of a protective film sample, wiping vaseline on the surface of the protective film sample after 1h by using the clean cotton balls, measuring trichroin coordinate values ((L, a and b) of the non-coated part and the coated part of the protective film sample by using a color difference tester, calculating delta L, delta a and delta b before and after the protective film sample is coated with white vaseline, and calculating a formula delta E (delta L) according to the color difference2+△a2+△b2)1/2Calculating Delta E, Delta E<0.25 is an ideal matching range with very little or no chromatic aberration, i.e., the film material is excellent in fingerprint resistance. The calculation results are shown in table 2.
Table 2 protective film Δ E value test results
| Experimental group | Delta E value |
| Example 1 | 0.13 |
| Example 2 | 0.11 |
| Example 3 | 0.21 |
| Example 4 | 0.17 |
| Example 5 | 0.23 |
| Example 6 | 0.06 |
| Example 7 | 0.03 |
| Example 8 | 0.05 |
| Example 9 | 0.21 |
| Comparative example 1 | 0.27 |
As can be seen from Table 2, the protective films of examples 1 to 5 had a Δ E value of less than 0.22, and satisfied a Δ E of less than 0.25, and had very little or no color difference in the fingerprint test, and excellent fingerprint resistance; comparing example 2 with comparative example 1, the delta E value of the protective film in example 2 is lower than that of comparative example 1, which shows that N-benzoyl quinine tert-butyl ester modified methyl triisopropoxysilane is used as a silicone resin layer component on the upper surface of the adhesive layer in the protective film, and the protective film is compounded with other layer materials to prepare the protective film, so that the protective film has excellent fingerprint resistance; comparing example 2 with example 7, and example 9 with comparative example 1, the Δ E value of the protective film in example 7 is lower than that of example 2, and the Δ E value of the protective film in example 9 is lower than that of comparative example 1, which shows that the addition of 3,4, 6-trimethoxy-1 (3H) -isobenzofuranone in the functional layer of the protective film improves the fingerprint resistance of the protective film.
Test example 5
Determination of water-proof and stain-resistant performance of protective film
The protective film material was cut into 50mm × 50mm, and a water drop was dropped on the surface of the film material, and contact angle measurement was performed after 10 seconds, and the test results are shown in table 3.
Table 3 water contact angle of protective film
As can be seen from Table 3, the water contact angle of the protective films of examples 1-5 was higher than 127 °; comparing the example 2 with the comparative example 1, the contact angle of the protective film in the example 2 is higher than that in the comparative example 1, which shows that the N-benzoyl quinine tert-butyl ester modified methyl triisopropoxysilane is used as the silicone resin layer component on the upper surface of the adhesive layer in the protective film and is compounded with other layer materials to prepare the protective film, so that the waterproof performance of the protective film is improved; the water contact angles of the examples 6 to 8 are higher than 143 degrees, the water contact angles of the protective films of the comparative examples 2 and 7, and the water contact angles of the protective films of the example 9 and 1 are higher than those of the example 2 and the protective film of the example 9 and 1, respectively, which shows that the addition of 3,4, 6-trimethoxy-1 (3H) -isobenzofuranone in the functional layer of the protective film improves the water and stain resistance of the protective film.
Test example 6
The protective film is used for measuring the laser cutting performance of the silver mirror glass; attaching the silicone resin layer on the lower surface of the protective film prepared in each embodiment on silver mirror glass (the silicone resin layer on the lower surface of the protective film is in contact with the silver mirror glass) according to a conventional technology, fixing the back surface of the protective film by using a double-sided adhesive tape without falling off, and performing laser cutting according to a conventional technical scheme and technical parameters; wherein the laser irradiation conditions are as follows: the wavelength is 355nm, the repetition frequency is 90kHz, the average power is 6W, the irradiation frequency is 5 times/1 line, the pulse width is 50ns, and the light-gathering point is elliptical (the major axis is 100 μm, and the minor axis is 20 μm); the laser cutting speed is 50 m/min; the line width change rate of the heat affected zone of laser cutting (the test conditions of each example are the same) relative to the situation of not sticking the protective film for protection is measured, and the calculation formula is as follows:
rate of change (%) - (L)0-L1)/L0
FIG. 4 shows the line width change rate of the heat affected zone of the silver mirror glass laser cutting. As can be seen from fig. 4, the line width change rate of the heat affected zone of the laser cutting of silver mirror glass in examples 1-5 is higher than 60%, the line width change rate of the heat affected zone of comparative example 2 and comparative example 1 is higher than that of comparative example 1, which shows that the N-benzoyl quinine tert-butyl ester modified methyl triisopropoxysilane is used as the silicone resin layer component on the upper surface of the adhesive layer in the protective film, so that the absorption of the protective film on the laser beam is improved, the diameter of the focused spot is reduced, and the line width of the heat affected zone on the upper surface of the cut material is reduced. In examples 6 to 8, the line width change rate of the laser cutting heat affected zone of the silver mirror glass is higher than 68%, the line width change rate of the heat affected zone of the silver mirror glass is higher than that of example 2 and example 7, and the line width change rate of the heat affected zone of example 9 is higher than that of comparative example 1 compared with example 7, example 9 and comparative example 1, which shows that the addition of 3,4, 6-trimethoxy-1 (3H) -isobenzofuranone in the functional layer further improves the absorption effect of the protective film on the laser beam, and further reduces the line width of the heat affected zone on the upper surface of the cut material.
The observation results of the surface quality of the silver mirror glass after laser cutting by uncovering the protective film are shown in table 2:
TABLE 4 surface quality of silver mirror glass after laser cutting
| Experimental group | Surface quality |
| Example 2 | Almost free of contaminating particles |
| Example 7 | Almost free of contaminating particles |
| Example 9 | Almost free of contaminating particles |
| Comparative example 1 | Almost free of contaminating particles |
As can be seen from table 4, the silver mirror glass coated with the protective film in examples 2, 7, 9 and comparative example 1 was laser cut and then the protective film was peeled off, and the surface of the silver mirror glass was almost free from particle contamination, i.e., the silver mirror glass with good surface quality was obtained.
Conventional operations in the operation steps of the present invention are well known to those skilled in the art and will not be described herein.
The above embodiments are merely illustrative, and not restrictive, and those skilled in the art can make various changes and modifications without departing from the spirit and scope of the invention. Therefore, all equivalent technical solutions also belong to the scope of the present invention, and the protection scope of the present invention should be defined by the claims.
Claims (9)
1. A protective film, comprising: the functional layer (1), the film substrate layer (2), the adhesive layer (3) and the silicone resin layer (4); the adhesive layer (3) is covered on one side of the film substrate layer (2); the functional layer (1) is covered on the other side of the film substrate layer (2); wherein,
the surface of the adhesive layer (3) is covered with a silicone resin layer (4) formed by silicone resin containing a modified silane coupling agent;
the modified silane coupling agent is methyl triisopropoxysilane modified by N-benzoyl quinine tert-butyl ester.
2. The protective film according to claim 1, wherein: the functional layer (1) is a film formed by a mixture of alumina/yttria composite sol and thermoplastic resin.
3. The protective film according to claim 1, wherein: the film base material layer (2) is at least one of polyethylene terephthalate, polyurethane, polyethylene and polyimide.
4. The protective film according to claim 1, wherein: the adhesive layer (3) is an acrylic pressure-sensitive adhesive.
5. Use of the protective film according to claim 1 for the production of protective films for laser cutting of silver mirror glass.
6. A preparation method of a protective film of a non-composite release film for laser cutting of silver mirror glass comprises the following steps:
coating a coating mixed solution for preparing acrylate pressure-sensitive adhesive on one side of the film substrate layer (2) to obtain an adhesive layer (3);
coating a silicone resin emulsion containing the modified silane coupling agent described in claim 1 on the upper surface of the adhesive layer, and drying to obtain a silicone resin layer (4);
preparing a coating mixed solution from the alumina/yttria composite sol and thermoplastic resin, coating the coating mixed solution on the other side of the membrane substrate layer (2), drying to obtain the functional layer (1), and preparing to obtain the protective membrane.
7. The method for preparing the protective film for laser cutting of silver mirror glass, which is not a composite release film, according to claim 6, is characterized in that: the thickness of the protective film is 50-90 mu m; the thickness of the adhesive layer (3) is 15-20 mu m; the thickness of the silicone resin layer (4) is 1-4 mu m; the thickness of the functional layer (1) is 1.8-2.4 mu m.
8. The method for preparing the protective film, which is not a composite release film, for the laser cutting of the silver mirror glass according to claim 6, wherein the method for preparing the modified silane coupling agent comprises the following steps: putting N-benzoyl quinine tert-butyl ester, a solvent and a catalyst in parts by weight into a reactor for catalyst activation; and then adding methyl triisopropoxysilane into the reactor for reaction, and performing rotary evaporation and recrystallization to obtain the modified silane coupling agent.
9. The method for preparing the protective film for laser cutting of silver mirror glass, which is a non-composite release film, according to claim 8, wherein the N-benzoyl quinine tert-butyl ester is 4-7 parts by weight, the solvent is 150-200 parts by weight, the catalyst is 0.15-0.25 part by weight, and the methyl triisopropoxysilane is 2.5-4.5 parts by weight.
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| CN106799548B (en) * | 2017-02-06 | 2019-04-26 | 京东方科技集团股份有限公司 | The method of protective film, laser cutting |
| CN107815257A (en) * | 2017-11-08 | 2018-03-20 | 苏州赛伍应用技术股份有限公司 | A kind of chip cutting diaphragm and preparation method thereof and application method |
| CN110079233B (en) * | 2019-05-24 | 2023-05-05 | 深圳昌茂粘胶新材料有限公司 | Glass processing process protective film capable of being directly cut and preparation method thereof |
| CN212269967U (en) * | 2020-04-28 | 2021-01-01 | 广东硕成科技有限公司 | Protective film for wafer cutting |
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2021
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