WO2022132417A1 - Structures stratifiées avec couche intermédiaire polymère adhésive comprenant des zones de décollement cohésives de performance améliorée - Google Patents
Structures stratifiées avec couche intermédiaire polymère adhésive comprenant des zones de décollement cohésives de performance améliorée Download PDFInfo
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- WO2022132417A1 WO2022132417A1 PCT/US2021/060810 US2021060810W WO2022132417A1 WO 2022132417 A1 WO2022132417 A1 WO 2022132417A1 US 2021060810 W US2021060810 W US 2021060810W WO 2022132417 A1 WO2022132417 A1 WO 2022132417A1
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- zones
- api
- peel strength
- debonding
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- LKKPNUDVOYAOBB-UHFFFAOYSA-N naphthalocyanine Chemical class N1C(N=C2C3=CC4=CC=CC=C4C=C3C(N=C3C4=CC5=CC=CC=C5C=C4C(=N4)N3)=N2)=C(C=C2C(C=CC=C2)=C2)C2=C1N=C1C2=CC3=CC=CC=C3C=C2C4=N1 LKKPNUDVOYAOBB-UHFFFAOYSA-N 0.000 description 1
- 229920003052 natural elastomer Polymers 0.000 description 1
- 229920001194 natural rubber Polymers 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- GYHFUZHODSMOHU-UHFFFAOYSA-N nonanal Chemical compound CCCCCCCCC=O GYHFUZHODSMOHU-UHFFFAOYSA-N 0.000 description 1
- JFNLZVQOOSMTJK-KNVOCYPGSA-N norbornene Chemical compound C1[C@@H]2CC[C@H]1C=C2 JFNLZVQOOSMTJK-KNVOCYPGSA-N 0.000 description 1
- 239000002667 nucleating agent Substances 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- HMZGPNHSPWNGEP-UHFFFAOYSA-N octadecyl 2-methylprop-2-enoate Chemical compound CCCCCCCCCCCCCCCCCCOC(=O)C(C)=C HMZGPNHSPWNGEP-UHFFFAOYSA-N 0.000 description 1
- SSDSCDGVMJFTEQ-UHFFFAOYSA-N octadecyl 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CCCCCCCCCCCCCCCCCCOC(=O)CCC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 SSDSCDGVMJFTEQ-UHFFFAOYSA-N 0.000 description 1
- FSAJWMJJORKPKS-UHFFFAOYSA-N octadecyl prop-2-enoate Chemical compound CCCCCCCCCCCCCCCCCCOC(=O)C=C FSAJWMJJORKPKS-UHFFFAOYSA-N 0.000 description 1
- NUJGJRNETVAIRJ-UHFFFAOYSA-N octanal Chemical compound CCCCCCCC=O NUJGJRNETVAIRJ-UHFFFAOYSA-N 0.000 description 1
- NZIDBRBFGPQCRY-UHFFFAOYSA-N octyl 2-methylprop-2-enoate Chemical compound CCCCCCCCOC(=O)C(C)=C NZIDBRBFGPQCRY-UHFFFAOYSA-N 0.000 description 1
- 229940065472 octyl acrylate Drugs 0.000 description 1
- ANISOHQJBAQUQP-UHFFFAOYSA-N octyl prop-2-enoate Chemical compound CCCCCCCCOC(=O)C=C ANISOHQJBAQUQP-UHFFFAOYSA-N 0.000 description 1
- 229940049964 oleate Drugs 0.000 description 1
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 239000012766 organic filler Substances 0.000 description 1
- RPQRDASANLAFCM-UHFFFAOYSA-N oxiran-2-ylmethyl prop-2-enoate Chemical compound C=CC(=O)OCC1CO1 RPQRDASANLAFCM-UHFFFAOYSA-N 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- QNGNSVIICDLXHT-UHFFFAOYSA-N para-ethylbenzaldehyde Natural products CCC1=CC=C(C=O)C=C1 QNGNSVIICDLXHT-UHFFFAOYSA-N 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 238000007719 peel strength test Methods 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- HGBOYTHUEUWSSQ-UHFFFAOYSA-N pentanal Chemical compound CCCCC=O HGBOYTHUEUWSSQ-UHFFFAOYSA-N 0.000 description 1
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 229940031826 phenolate Drugs 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- DOIRQSBPFJWKBE-UHFFFAOYSA-N phthalic acid di-n-butyl ester Natural products CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 description 1
- IEQIEDJGQAUEQZ-UHFFFAOYSA-N phthalocyanine Chemical class N1C(N=C2C3=CC=CC=C3C(N=C3C4=CC=CC=C4C(=N4)N3)=N2)=C(C=CC=C2)C2=C1N=C1C2=CC=CC=C2C4=N1 IEQIEDJGQAUEQZ-UHFFFAOYSA-N 0.000 description 1
- 238000009832 plasma treatment Methods 0.000 description 1
- 229920001084 poly(chloroprene) Polymers 0.000 description 1
- 229920000747 poly(lactic acid) Polymers 0.000 description 1
- 229920002589 poly(vinylethylene) polymer Polymers 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920002530 polyetherether ketone Polymers 0.000 description 1
- 229920000139 polyethylene terephthalate Polymers 0.000 description 1
- 239000005020 polyethylene terephthalate Substances 0.000 description 1
- 229920001195 polyisoprene Polymers 0.000 description 1
- 239000004626 polylactic acid Substances 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 150000003077 polyols Chemical class 0.000 description 1
- 235000013824 polyphenols Nutrition 0.000 description 1
- 229920001451 polypropylene glycol Polymers 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 229920000909 polytetrahydrofuran Polymers 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000002028 premature Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- BOQSSGDQNWEFSX-UHFFFAOYSA-N propan-2-yl 2-methylprop-2-enoate Chemical compound CC(C)OC(=O)C(C)=C BOQSSGDQNWEFSX-UHFFFAOYSA-N 0.000 description 1
- LYBIZMNPXTXVMV-UHFFFAOYSA-N propan-2-yl prop-2-enoate Chemical compound CC(C)OC(=O)C=C LYBIZMNPXTXVMV-UHFFFAOYSA-N 0.000 description 1
- NHARPDSAXCBDDR-UHFFFAOYSA-N propyl 2-methylprop-2-enoate Chemical compound CCCOC(=O)C(C)=C NHARPDSAXCBDDR-UHFFFAOYSA-N 0.000 description 1
- PNXMTCDJUBJHQJ-UHFFFAOYSA-N propyl prop-2-enoate Chemical compound CCCOC(=O)C=C PNXMTCDJUBJHQJ-UHFFFAOYSA-N 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000010526 radical polymerization reaction Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000002310 reflectometry Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 229940100486 rice starch Drugs 0.000 description 1
- 229910052701 rubidium Inorganic materials 0.000 description 1
- YGSDEFSMJLZEOE-UHFFFAOYSA-M salicylate Chemical compound OC1=CC=CC=C1C([O-])=O YGSDEFSMJLZEOE-UHFFFAOYSA-M 0.000 description 1
- 229960001860 salicylate Drugs 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 229910052706 scandium Inorganic materials 0.000 description 1
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 description 1
- SCPYDCQAZCOKTP-UHFFFAOYSA-N silanol Chemical compound [SiH3]O SCPYDCQAZCOKTP-UHFFFAOYSA-N 0.000 description 1
- 150000004819 silanols Chemical class 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 239000013464 silicone adhesive Substances 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 239000004945 silicone rubber Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000000235 small-angle X-ray scattering Methods 0.000 description 1
- 239000001488 sodium phosphate Substances 0.000 description 1
- 239000012321 sodium triacetoxyborohydride Substances 0.000 description 1
- KKDONKAYVYTWGY-UHFFFAOYSA-M sodium;2-(methylamino)ethanesulfonate Chemical compound [Na+].CNCCS([O-])(=O)=O KKDONKAYVYTWGY-UHFFFAOYSA-M 0.000 description 1
- HUAUNKAZQWMVFY-UHFFFAOYSA-M sodium;oxocalcium;hydroxide Chemical compound [OH-].[Na+].[Ca]=O HUAUNKAZQWMVFY-UHFFFAOYSA-M 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 229940114926 stearate Drugs 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- 150000003440 styrenes Chemical class 0.000 description 1
- 150000003871 sulfonates Chemical class 0.000 description 1
- 150000003462 sulfoxides Chemical class 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- SJMYWORNLPSJQO-UHFFFAOYSA-N tert-butyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OC(C)(C)C SJMYWORNLPSJQO-UHFFFAOYSA-N 0.000 description 1
- ISXSCDLOGDJUNJ-UHFFFAOYSA-N tert-butyl prop-2-enoate Chemical compound CC(C)(C)OC(=O)C=C ISXSCDLOGDJUNJ-UHFFFAOYSA-N 0.000 description 1
- 229920003046 tetrablock copolymer Polymers 0.000 description 1
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 1
- 229910052716 thallium Inorganic materials 0.000 description 1
- 239000003017 thermal stabilizer Substances 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 239000005341 toughened glass Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003623 transition metal compounds Chemical class 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical class [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 description 1
- 229940086542 triethylamine Drugs 0.000 description 1
- XUHUMYVYHLHMCD-UHFFFAOYSA-N tris(2-cyclohexylphenyl) phosphite Chemical compound C1CCCCC1C1=CC=CC=C1OP(OC=1C(=CC=CC=1)C1CCCCC1)OC1=CC=CC=C1C1CCCCC1 XUHUMYVYHLHMCD-UHFFFAOYSA-N 0.000 description 1
- WGKLOLBTFWFKOD-UHFFFAOYSA-N tris(2-nonylphenyl) phosphite Chemical compound CCCCCCCCCC1=CC=CC=C1OP(OC=1C(=CC=CC=1)CCCCCCCCC)OC1=CC=CC=C1CCCCCCCCC WGKLOLBTFWFKOD-UHFFFAOYSA-N 0.000 description 1
- HBYRZSMDBQVSHO-UHFFFAOYSA-N tris(2-tert-butyl-4-methylphenyl) phosphite Chemical compound CC(C)(C)C1=CC(C)=CC=C1OP(OC=1C(=CC(C)=CC=1)C(C)(C)C)OC1=CC=C(C)C=C1C(C)(C)C HBYRZSMDBQVSHO-UHFFFAOYSA-N 0.000 description 1
- WRSPWQHUHVRNFV-UHFFFAOYSA-N tris[3,5-di(nonyl)phenyl] phosphite Chemical compound CCCCCCCCCC1=CC(CCCCCCCCC)=CC(OP(OC=2C=C(CCCCCCCCC)C=C(CCCCCCCCC)C=2)OC=2C=C(CCCCCCCCC)C=C(CCCCCCCCC)C=2)=C1 WRSPWQHUHVRNFV-UHFFFAOYSA-N 0.000 description 1
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 1
- 229910000406 trisodium phosphate Inorganic materials 0.000 description 1
- 235000019801 trisodium phosphate Nutrition 0.000 description 1
- SOLUNJPVPZJLOM-UHFFFAOYSA-N trizinc;distiborate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-][Sb]([O-])([O-])=O.[O-][Sb]([O-])([O-])=O SOLUNJPVPZJLOM-UHFFFAOYSA-N 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 description 1
- KRLHYNPADOCLAJ-UHFFFAOYSA-N undecyl 2-methylprop-2-enoate Chemical compound CCCCCCCCCCCOC(=O)C(C)=C KRLHYNPADOCLAJ-UHFFFAOYSA-N 0.000 description 1
- RRLMGCBZYFFRED-UHFFFAOYSA-N undecyl prop-2-enoate Chemical compound CCCCCCCCCCCOC(=O)C=C RRLMGCBZYFFRED-UHFFFAOYSA-N 0.000 description 1
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 1
- KOZCZZVUFDCZGG-UHFFFAOYSA-N vinyl benzoate Chemical class C=COC(=O)C1=CC=CC=C1 KOZCZZVUFDCZGG-UHFFFAOYSA-N 0.000 description 1
- 238000011179 visual inspection Methods 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
- 239000004636 vulcanized rubber Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/10—Adhesives in the form of films or foils without carriers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
- B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
- B32B17/10—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
- B32B7/04—Interconnection of layers
- B32B7/12—Interconnection of layers using interposed adhesives or interposed materials with bonding properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2367/00—Polyesters, e.g. PET, i.e. polyethylene terephthalate
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
- B32B7/04—Interconnection of layers
- B32B7/05—Interconnection of layers the layers not being connected over the whole surface, e.g. discontinuous connection or patterned connection
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/20—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive itself
- C09J2301/204—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive itself the adhesive coating being discontinuous
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/20—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive itself
- C09J2301/208—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive itself the adhesive layer being constituted by at least two or more adjacent or superposed adhesive layers, e.g. multilayer adhesive
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/20—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive itself
- C09J2301/21—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive itself the adhesive layer being formed by alternating adhesive areas of different nature
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/40—Additional features of adhesives in the form of films or foils characterized by the presence of essential components
- C09J2301/414—Additional features of adhesives in the form of films or foils characterized by the presence of essential components presence of a copolymer
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2423/00—Presence of polyolefin
- C09J2423/04—Presence of homo or copolymers of ethene
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2433/00—Presence of (meth)acrylic polymer
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2459/00—Presence of polyacetal
Definitions
- the present invention relates to rigid substrate-laminates comprising polymeric interlayers that provide enhanced properties to rigid substrates using controlled debonding zone treatments.
- Laminated glass is generally made by laminating two pieces of glass onto a polymeric interlayer ( Figure 1).
- Figure 1 One particular advantage of laminated glass versus solid glass sheets is impact and shatter resistance due to adhesion of the glass to the interlayer sheet.
- polymeric interlayer Many different materials have been used as the polymeric interlayer.
- sheets containing a polyvinyl acetal, also known as polyvinyl butyral, and a plasticizer are widely utilized as an interlayer for laminated glass because they have excellent adhesion-to-glass properties.
- Laminated glass containing such interlayers can be made with good transparency, mechanical strength, flexibility, acoustic damping, and shatter resistance.
- At least partially neutralized ethylene acid copolymers have also been used as interlayers for preparing laminated safety glass, for example, as disclosed in U.S. Pat. Nos. 3,404,134; 3,344,014; 7,445,683; 7,763,360; 7,951,865; 7,960,017; 8,399,097; 8,399,098; U.S. Pat. App. Pub. Nos. 2018/0117883, and 2019/0030863; Int. Pat. App. Nos.
- ionomer resins can be chosen to produce interlayers having excellent flexural strength and optical properties, the adhesion properties to glass may not be optimal.
- ionomers are generally neutralized acid copolymers, they may develop lamination defects, particularly in high moisture environments.
- interlayers or portions of interlayers for float glass including polyvinyl butyral and thermoplastic elastomers. These, too, can exhibit difficulties with adhesion, laminate toughness, and durability.
- Patent references also discuss approaches on enhancing adhesion through the use of primers.
- U.S. Pat. No. 3,445,423 discloses using a solution of gamma-aminopropyl- triethoxysilane as a primer for bonding the outside marginal portion of a windshield to a metal receiving member using a polyurethane composition.
- U.S. Pat. No. 3,881,043 discloses the application of an adhesion primer to the perimeter of a windshield to reduce the tendency for premature delamination.
- Another embodiment involves the application of the adhesion promoting composition to be applied in a pattern of dots throughout the extent of the interfacial surface to increase the overall magnitude of adhesion.
- U.S. Pat. Nos. 5,342,653; 5,478,412; and 5,5477,36 disclose a method of applying antiadhesion projections to the surface of the sheet to counteract the high adhesion of the sheet to glass between the projections. These projections are said to operate on a physical blocking of adhesion means and by preference, do not rely on chemical means.
- U.S. Pat. No. 10,022,908 discloses application of a primer to the surface of the interlayer which raises the adhesion between the interlayer and glass surface and can provide increased adhesion retention under exposure to high humidity conditions.
- U.S. Pat. No. 3,505,160 discloses the application of an adhesion reducing substance (“a poor adhesive”) in the interior portion of a windshield to increase the impact performance in a region where occupant impact could likely occur in an accident scenario.
- a poor adhesive an adhesion reducing substance
- U.S. Pat. App. Pub. No. 2019/0030863 discloses that a certain class of silanes can successfully and advantageously be used in very specific amounts and under limited conditions as glass adhesion promoters for sodium-neutralized ionomers, allowing the optimal use of such ionomers in the preparation of interlayers and glass laminates having enhanced interlayer-to-glass adhesion properties.
- the present invention addresses the above-described problems by providing a means where the integrity of the laminate prepared with the multi-modal bonding robustness of the interlayer/glass laminate assembly is improved while retaining adequate laminate integrity and durability but providing improved impact performance. This is carried out by providing a substantially cohesive discrete debonding region within the interlayer near the glass substrate.
- FEP fluorinated-ethylene-propylene
- this invention relates to an adhesive polymeric interlayer (API), comprising: a first polymeric material, a first and a second surface, cohesive debonding zones that are discrete and/or continuous debonding zones, wherein the cohesive debonding zones comprise a first debonding zone that is discrete or continuous and having a maximum mean peel strength, wherein the cohesive debonding zones comprise a second cohesive debonding zone that is discrete or continuous with a minimum mean peel strength greater than about 0.01 kJ/m 2 , wherein the maximum mean peel strength is at least about 2 times greater than the minimum mean peel strength.
- API adhesive polymeric interlayer
- this invention relates to an API as recited above, wherein: the debonding zones are located within 10% thickness of the API from the first and/or the second surface of the API, and the first debonding zone and the second debonding zone are within the 10% thickness of the API proximate to the first surface.
- this invention relates to an API as recited above, wherein one of the first or second debonding zones comprises the first polymeric material, and the other of the first and second discrete zones comprises a first material chemically and/or physically different from the first polymeric material.
- this invention relates to an API as recited above, wherein the first material is characterized by: (i) a molecular weight different than that of the first polymeric material, (ii) a crystallinity different than that of the first polymeric material, (iii) a density different than that of the first polymeric material, (iv) a glass transition temperature different than that of the first polymeric material, (v) a melt flow index different than that of the first polymeric material, or (vi) a Young’s modulus different than that of the first polymeric material, (vii) or a combination of one or more of said characteristics.
- this invention relates to an API as recited above, wherein at least one of the first debonding zone and the second debonding zone is coplanar to the API.
- this invention relates to an API as recited above, wherein the first debonding zone and the second debonding zone are discrete, and are located in one plane or in more than one plane.
- this invention relates to an API as recited above, wherein the cohesive discrete debonding zones are distributed in an ordered pattern.
- this invention relates to an API as recited above, wherein the cohesive discrete debonding zones are distributed stochastically.
- this invention relates to an API as recited above, wherein at least one of the first debonding zone or the second debonding zone is characterized by:
- this invention relates to an API as recited above, wherein the effective diameter of the regular shaped discrete debonding zone, the random shaped discrete debonding zone, or the cluster discrete zone is from about 1 multiple to about 150,000,000-multiples of the thickness of the discrete debonding zone.
- this invention relates to an API as recited above, wherein the weight content of one of said first and second debonding zones as a percentage of the total of the API is in the range of from about 0.00001% to about 30%.
- this invention relates to an API as recited above, wherein the first debonding zone with maximum mean peel strength has a mean peel strength that is from about 2 times to about 250 times greater than a mean peel strength of the second debonding zone with minimum mean peel strength.
- this invention relates to an API as recited above, wherein the API comprises at least two zones, wherein at least one of the zones has a mean peel strength of from about 0.01 to about 12.0 kJ/m 2 .
- this invention relates to an API as recited above, wherein the first polymeric material comprises a polyvinylacetal, an ionomer, a thermoplastic elastomer, an ethyl vinylacetate, or combinations thereof.
- this invention relates to an API as recited above, wherein the first material comprises a polyvinylacetal, an ionomer, a thermoplastic elastomer, a silane, an ethyl vinylacetate, a fluoropolymer, a polyvinyl-alcohol, or combinations thereof.
- this invention relates to an API as recited above, wherein at least one of the cohesive debonding zones comprises the ionomer, wherein the ionomer resin is a sodium- neutralized ethylene-a,P-unsaturated carboxylic acid copolymer.
- this invention relates to an API as recited above, wherein the polyvinylacetal is a polyvinylbutyral.
- this invention relates to an API as recited above, wherein the second debonding zone is the first polymeric material, and the first polymeric material is an ionomer resin.
- this invention relates to an API as recited above, wherein the first debonding zone is the first polymeric material, and the first polymeric material is a polyvinylacetal.
- this invention relates to an API as recited above, wherein the first material is an adhesion modifying agent.
- this invention relates to an API as recited above, wherein the adhesion modifying agent is present in a range of from about 0.001% to about 75% by weight of the first polymeric material.
- this invention relates to an API as recited above, wherein one of the first or second debonding zones has a thickness of from about 0.001 mm to about 10.0 mm.
- this invention relates to an API as recited above, wherein the adhesion modifying agent is a silane, an alkali metal salt, an alkaline earth metal salt or a carboxylic group- containing olefinic polymer. In another embodiment, this invention relates to an API as recited above, wherein the adhesion modifying agent is a silane.
- this invention relates to an API as recited above, wherein the adhesion modifying agent is present in a range of from about 0.001% to about 75% by weight of the first polymeric material.
- this invention relates to an API as recited above, wherein one of the first or second debonding zones has a thickness of from about 0.001 mm to about 10.0 mm.
- this invention relates to an API as recited above, wherein each discrete debonding zone is shaped as a dot, a circle, a partial circle, an oval, a partial oval, a triangle, a square, a rectangle, a pentagon, a hexagon; a heptagon, a polygon, or is amorphous shaped.
- this invention relates to an API as recited above, wherein an effective diameter of the discrete zone debonding is in a range of from about 0.1 mm to about 50 mm.
- this invention relates to an API as recited above, wherein the peel strength ratio of the zone with maximum peel strength (Zmax) to the zone with the minimum peel strength (Zmin), that is, (Zmax/Zmin) is greater than or equal to 5.
- this invention relates to an API as recited above, wherein: all debonding zones have different peel strength; one or more debonding zones have the same peel strength; or one or more debonding zones have different peel strength.
- this invention relates to a laminate structure, comprising a stack of:
- this invention relates to a laminate structure as recited above, comprising a stack of:
- this invention relates to a laminate structure, wherein at least one rigid substrate is a glass substrate.
- this invention relates to a laminate structure as recited above, wherein the discrete debonding zones have a surface area on one side that is:
- this invention relates to a laminate structure as recited above, wherein said adhesive polymeric interlayer comprises at least two zones, wherein at least one of the zones has a mean peel strength of:
- this invention relates to a laminate structure as recited above, wherein the adhesive polymeric interlayer comprises from 2 to 100 zones per cm 2 .
- this invention relates to a laminate structure as recited above, wherein the thicknesses on either side of the adhesive polymeric interlayer (API) in which the cohesive debonding zones are located are independently from about 0.5% to about 10% of the total thickness of the API.
- API adhesive polymeric interlayer
- interlayer and laminate performance is enhanced by providing a debonding region within the adhesive polymeric interlayer near the interface of the adhesive polymeric interlayer and the glass sheet, which allows for controlled debonding, as exemplified by employing less adhesion-promoting material. Additionally, it has been shown that non-uniform, controlled adhesion produces unique combinations of debonding region-glass adhesion, laminate tear resistance, and laminate post-breakage durability.
- the enhanced performance is measured by different ways, including ball-on-ring, cyclic weathering, and other tests as described herein. The improved adhesion leads to improved durability of the laminates comprising such debonding regions.
- Controlled debonding zone treatments have been found to allow further optimization of laminate performance characteristics; primarily laminate tear resistance at a given unit thickness of the debonding region at the interface of the glass and the API within the API compared with conventional art.
- the durability of laminates can also be optimized to balance aspects of laminate integrity with that of energy absorbing capability under impact or other extreme applied forces acting to breach the laminate.
- the CDZT approach involves defining both a range and boundary limits for the energy required to effectuate a debonding ‘event’ at or near the interface between the debonding region and the API beneath the region in the API. These boundary conditions would have at least a lower limit and an upper limit.
- Each lower and upper limit would be generated through the application of a treatment such that at least a bimodal or multi-modal adhesion level is created, wherein the cohesion/debonding characteristics are defined by the applied treatment.
- the CDZT technology has been found to provide superior laminate performance over that of the conventional art. This can be accomplished in various modes and possessing some or all of the characteristics listed herein.
- a treatment can alternatively consist of the application of an energetic ‘beam’, such as electron beam, gamma, plasma, electron discharge, laser, ion-beam or other energetic means such as, plasma, flame-treatment, UV/VIS/IR radiation, microwaves or chemical alteration, via, coating techniques, chemical vapor deposition, and the like.
- an energetic ‘beam’ such as electron beam, gamma, plasma, electron discharge, laser, ion-beam or other energetic means such as, plasma, flame-treatment, UV/VIS/IR radiation, microwaves or chemical alteration, via, coating techniques, chemical vapor deposition, and the like.
- Combinations of a chemical substance(s) with energetic sources can also be employed as a treatment.
- the treatment may be of an infinitesimally small dimension (i.e. only surface atomic or molecular monolayer affected by the treatment or the treatment may be of a finite thickness (approaching up to 30%) of the API layer thickness.
- the treatment may be applied to the rigid substrate.
- debonding zone treatments and/or cohesive treatments can be made to be invisible or nearly imperceptible so as to not interfere with the clarity and transparency of said laminate, these techniques can be combined with other features of the resulting laminate structure; these would not be limited to the creation of decorative, gradients, visible patterns, obscuration, tinting/coloration, alteration of transparency and reflectiveness (for example, creation of translucency or opaqueness), energy management, solar control, photovoltaic generation and passive and active systems.
- the design of the applied treatment can be defined by various descriptors.
- the surface coverage (or volume fraction) is one aspect that can be adjusted to achieve a desired effect or outcome.
- the CZDT provides for enhanced laminate performance with respect to the energy level required to breach the laminate and/or the durability of the laminate to withstanding various harsh environmental factors (wide-temperature swings/exposures and high moistures) or imposed stress (flexure, dead or live loads, lamination stress, etc.). Additionally, it can provide improved robustness in performance over a broad range of manufacturing variations; such as, rigid substrate composition, substrate surface cleanliness (e.g. glass washing conditions), moisture conditions, improper lamination temperature and dwell time, etc.
- Fig. 1 shows a standard laminate structure with two glass substrates and an interlayer.
- Fig. 2 shows a schematic construction of the present invention with one glass substrate and an interlayer with the 10 %-thickness regions comprising cohesive discrete debonding zones.
- Fig. 3 shows a schematic construction of the present invention with only one glass substrate and an interlayer with the 10% thickness regions comprising cohesive continuous debonding zones.
- Fig. 4 shows a schematic construction of the present invention with only one glass substrate and an interlayer with the 10% thickness regions comprising cohesive discrete and continuous debonding zones.
- Fig. 5 shows a schematic construction of the present invention with two glass substrates and an interlayer with the 10 %-thickness regions comprising cohesive discrete debonding zones.
- Fig. 6 shows a schematic construction of the present invention with two glass substrates and an interlayer with the 10% thickness regions comprising cohesive continuous debonding zones.
- FIG. 7 shows a schematic construction of the present invention with two glass substrates and an interlayer with the 10% thickness regions comprising cohesive discrete and continuous debonding zones.
- Figure 8 shows the peel force of a typical interlayer/glass ‘laminate’ possessing relatively uniform adhesion - this is representative of the conventional art.
- Figure 9 shows a schematic construction of the present invention, where one glass substrate, the debonding zone treatment and the adhesive polymeric interlayer are shown.
- Fig. 10 shows a laminate with two glass substrates and an interlayer (API) with a cohesive discrete debond zone treatment comprising of a fluorinated-ethylene-propylene copolymer (FEP) debond layer with ionomer pillars connecting ionomer phase.
- API interlayer
- FEP fluorinated-ethylene-propylene copolymer
- Fig. 11 shows a laminate with two glass substrates and an interlayer (API) with a cohesive continuous debond zone treatment comprising of an FEP continuous debond layer.
- API interlayer
- Fig. 12 shows a picture of the Laminate Breakage: Ball-on-Ring test.
- Fig. 13 depicts the graphical representation of the change in Load in N as a function of crosshead displacement in mm.
- Ur is the laminate tear energy.
- glass substrate has been used as an example of rigid substrate.
- Rigid substrate has been discussed infra in later sections.
- the present invention relates to a laminate structure comprising at least one glass substrate and an adhesive polymeric interlayer (API) that comprises cohesive debonding zones that are substantially discrete and/or substantially continuous in their layout.
- API adhesive polymeric interlayer
- Such debonding zones are located preferably within the 10% thickness of API from the interface of said API and the glass substrate. These zones allow for a unique combination of modified API-glass debonding, laminate toughness, and laminate durability. Various spatial patterns and densities of debonding are described, as well as the resulting material properties.
- controlled debonding is meant a zonal variability in the generally planar direction, in cohesion, in the vicinity of the interfacial region and the API. Stated another way, the cohesion strength within the region comprising the debonding zones varies generally in the planar direction in the vicinity of the interface of the glass substrate and the API. This variation is described in the multiple exemplary embodiments, infra.
- debonding zones is meant that if the glass substrates and the adhesive polymeric interlayer debond, there is substantial likelihood that the debonding is primarily within the “debonding zones.”
- cohesive discrete debonding zones are meant that the debonding zones are contained in the API but are substantially discrete, that is, the zones, which may or may not cover generally the entire area of the adhesive polymeric interlayer (API), in the planar direction, are substantially separate from each other with defined boundaries.
- the discrete zones may be co-planar or may not be co-planar.
- the discrete zones in a given plane may be co-planar to at least one of the glass substrate, and/or to the API layer.
- cohesive continuous debonding zones is meant that the debonding zones are contained in the API but are substantially continuous, that is, the zones, may cover generally the entire area of the adhesive polymeric interlayer (API), in the planar direction, are substantially separate from each other with defined boundaries.
- API adhesive polymeric interlayer
- the continuous zones may be co-planar or may not be coplanar.
- the continuous zones in a given plane may be co-planar to at least one of the glass substrate, and/or to the API layer.
- the crack path resides within the bulk material, defined here as a substantial portion of the crack area being at a distance greater than 100 nm from the interface, for example, a glass substrate-API interface, or a superbonding layer API interface. In one embodiment, from about 51% to about 100% of the crack area is found at a at a distance greater than 100 nm from the interface. Stated differently, the crack area percentage is selected from a range defined by any one number below, including the endpoints:
- Patterned cohesion is meant that the debonding treatment is arranged in some geometric fashion with the disposition within the interfacial region of the interlayer and rigid substrate. There is some regularity with a patterned treatment. This treatment will create debonding discontinuities that differ from the interstitial spaces adjoining the pattern. There may be more than one pattern treatment applied, either differing in pattern type, geometry parameters and can be made to be overlapping or imposed upon the underlying pattern treatment or falling within the interstitial space or any combination thereof.
- stochastic is meant that an item or pattern is randomly determined and generally cannot be predicted precisely. Therefore, as used herein, a stochastic pattern is a random one. Stochastically Varying Cohesion
- “stochastically varying cohesion” is meant that the debonding treatment is approaching a ‘random-like’ disposition within the debond region of the API and rigid substrate. This treatment will create debonding discontinuities from that of a more uniform field of cohe- sion/debonding.
- uniform cohesion is meant that the debonding in the near-interfacial region occurs substantially in a manner that does not vary more than +/- 10% from location-to-location as measured on an interfacial area basis. In one embodiment, the uniform cohesion covers from 5% to 100% of the near-interfacial region thickness.
- linear positioning is meant the cohesion modifier is applied to either the glass or the adhesive polymeric interlayer (API) or both, in a manner that allows the glass panels to be laid out onto the without regard to orientation, thus allowing the API to be cut with a minimal amount of waste.
- API adhesive polymeric interlayer
- Circularity, C is defined as the degree to which the zone is similar to a circle, taking into consideration the smoothness of the perimeter, length P. This means circularity is a measurement of both the zone and roughness. Thus, the further away from a perfectly round, smooth circle a zone becomes, the lower the circularity value. Circularity is a dimensionless value. Where A is the feature area, ISO9276-6 defines circularity as:
- Solidity, S is the measurement of the overall concavity of a zone. It is defined as the image area, A, divided by the convex hull area, Ac, as given below. Thus, as the zone becomes more solid, the image area and convex hull area approach each other, resulting in a solidity value of one. However, as the zone digresses from a closed circle, the convex hull area increases and the calculated solidity decreases. Solidity is a dimensionless value.
- effective diameter is meant the diameter of a circle with an area equivalent to the area of a zone having any shape as described herein.
- pressures expressed in psi units would be gauge, and pressures expressed in kPa units would be absolute. Pressure differences, however, are expressed as absolute (for example, pressure 1 is 25 psi higher than pressure 2).
- copolymer refers to polymers comprising copolymerized units resulting from copolymerization of two or more comonomers.
- a copolymer may be described herein with reference to its constituent comonomers or to the amounts of its constituent comonomers, for example “a copolymer comprising ethylene and 15 weight % of acrylic acid”, or a similar description.
- Such a description may be considered informal in that it does not refer to the comonomers as copolymerized units; in that it does not include a conventional nomenclature for the copolymer, for example International Union of Pure and Applied Chemistry (IUPAC) nomenclature; in that it does not use product-by-process terminology; or for another reason.
- IUPAC International Union of Pure and Applied Chemistry
- a description of a copolymer with reference to its constituent comonomers or to the amounts of its constituent comonomers means that the copolymer contains copolymerized units (in the specified amounts when specified) of the specified comonomers. It follows as a corollary that a copolymer is not the product of a reaction mixture containing given comonomers in given amounts, unless expressly stated in limited circumstances to be such.
- dipolymer refers to polymers consisting essentially of two monomers
- terpolymer refers to polymers comprising at least three monomers
- acid copolymer refers to a copolymer comprising copolymerized units of an a-olefin, an a,P-ethylenically unsaturated carboxylic acid, and optionally other suitable comonomer(s) such as, for example, an a,P-ethylenically unsaturated carboxylic acid ester.
- (meth)acrylic refers to acrylic or methacrylic, for example, “acrylic acid or methacrylic acid”, or “alkyl acrylate or alkyl methacrylate”.
- ionomer generally refers to a polymer that comprises ionic groups that are carboxylate salts, for example, ammonium carboxylates, alkali metal carboxylates, alkaline earth carboxylates, transition metal carboxylates and/or combinations of such carboxylates.
- carboxylate salts for example, ammonium carboxylates, alkali metal carboxylates, alkaline earth carboxylates, transition metal carboxylates and/or combinations of such carboxylates.
- Such polymers are generally produced by partially or fully neutralizing the carboxylic acid groups of precursor or parent polymers that are acid copolymers, as defined herein, for example by reaction with a base.
- the alkali metal ionomer as used herein is a sodium ionomer, for example a copolymer of ethylene and methacrylic acid, wherein all or a portion of the carboxylic acid groups of the copolymerized methacrylic acid units are neutralized, and substantially all of the neutralized carboxylic acid groups are in the form of sodium carboxylates.
- the interfacial region within the adhesive polymeric interlayer comprises more than one controlled debonding zones, alternatively called debonding zones, such that the difference in mean peel strength between the zone with minimum peel strength (Zmin) and the zone with maximum peel strength (Zmax) is at least about 2 multiples. Stated differently, (Zmax/Zmin) > 2.
- a laminate comprises the interfacial region within the API with multiple debonding zones, such that the difference in peel strength or mean peel strength between any two zones Zi and Z2 is greater than or equal to 0, or their ratio is greater than or equal to 1. In other words, Z1-Z2 > 0, or Z1/Z2 > 1.
- the (Zmax/Zmin) > 2 condition is maintained.
- the peel strength ratio of the zone with maximum peel strength (Zmax) to the zone with the minimum peel strength (Zmin), that is, (Zmax/Zmin) is greater than or equal to 5.
- all zones have different peel strengths; one or more zones have the same peel strength; or one or more zones have different peel strengths.
- this invention encompasses the embodiment, wherein more than one discrete and/or continuous zones demonstrate different peel strength, but the (Zmax/Zmin) > 2 condition is maintained.
- Zi is the zone with maximum peel strength
- Z3 is the zone with minimum peel strength.
- Zones Zi, Z2, Z3, and Z4 have different peel strengths.
- the interfacial region within the API comprises more than one discrete and/or continuous zones substantially planar to each other but in different planes within the interfacial region within the API that demonstrate the same peel strength, or different peel strength, but the (Zmax/Zmin) > 2 condition is maintained.
- FEP fluorinated-eth- ylene-propylene
- Z4 is the zone with maximum peel strength and Zs is the zone with minimum peel strength.
- Zones Z2, Z6, and Z9 have the same peel strength.
- Zones Zi, Z2, and Z7 have different peel strengths.
- the polymeric interlayer comprises more than one debonding zones, such that the debonding zones have regular shapes.
- the debonding zone is defined according to the peel strength. Stated another way, to a normal eye an interlayer may appear homogeneous and uniform, but for the purposes of the present invention, the debonding zones are defined by the difference in their peel strengths.
- Regular shapes include for example, circles, triangles, square, rectangles, trapezoid, rhombus, pentagons, hexagons, heptagons, and other polygons that may or may not approximate a circle, ovals, and such other shapes, with an effective area generally greater than the thickness of the interlayer in one embodiment.
- This invention also envisions irregular-shaped debonding zones for example, circles, triangles, square, rectangles, trapezoid, rhombus, pentagons, hexagons, heptagons, and other polygons that may or may not approximate a circle, ovals, and such other shapes.
- Irregular shapes include random shapes with closed boundaries, with effective area generally greater than the thickness of the interlayer in another embodiment.
- the debonding zones are spaced adjacent one another.
- the debonding zones are separated by interstitial space.
- some debonding zones are spaced adjacent one another, and other debonding zones are separated by interstitial space.
- Other shapes include one-dimensionally oriented patterns such as gridlines, crisscross lines, lattice, interweave, random lines, concentric and eccentric circles, spaghetti patterns, flat strips, etc.
- a cluster of smaller shapes would form a zone, with a second cluster of smaller shapes that would form a second zone.
- the aggregate peel strength of each cluster is measured, and the cluster of shapes is considered a debonding zone.
- the shapes within the cluster could be random shapes, regular, mixed regular shapes, mixed random shapes, or mixed random and regular shapes.
- the debonding zones as clusters could also comprise one-dimensionally oriented patterns such as gridlines, crisscross lines, random lines, concentric and eccentric circles, spaghetti patterns, flat strips, etc.
- the difference in peel strength between a gridline and the adjacent debonding zone may be measured by preparing a separate interlayer debonding zone with the strength of the gridline, and comparing it with the debonding zone on the interlayer of interest in between two gridlines, that is, in the interstitial spaces between two gridlines. Even in case of one-dimensionally oriented patterns, the area of such shapes may determine the peel-strength difference between a controlled debonding zone and the interstitial spaces or the difference between two adjacent controlled debonding zones.
- the debonding zone is defined according to the peel strength. Stated another way, to a normal eye the interfacial region within the API may appear homogeneous and uniform, but for the purposes of the present invention, the debonding zones are defined by the difference in their peel strengths.
- glass substrates are used as exemplars.
- rigid substrates include conventional glasses, such as soda lime and borosilicate glass, typically manufactured using the float process, crystalline materials such as aluminum oxynitride (A10N), single crystal aluminum oxide (Sapphire), spinel (MgAhCh), and glass-ceramic materials, such as TransArmTM, and lithium disilicate glass-ceramic.
- materials that could be utilized as the rigid substrate (or glass) as cited in this disclosure may include for example, commercial plate glass, float or sheet glass compositions, annealed glass, tempered glass, chemically strengthened glass, quartz and fused silica, borosilicate glasses, lithium containing glasses, PYROCERAM®, lithium containing ceramics, and nucleated ceramics.
- Glass compositions that can be produced as glass-ceramic materials include lithium zinc silicates, lithium aluminosilicates, lithium zinc aluminosilicates, lithium magnesium silicates, lithium magnesium aluminosilicates, magnesium aluminosilicates, calcium magnesium aluminosilicates, magnesium zinc silicates, calcium magnesium zinc silicates, zinc aluminosilicate systems calcium phosphates, calcium silicophosphates and barium silicate.
- other high-performance materials can consist of, aluminum oxide, zirconium oxide, silicon carbide, silicon nitride, aluminum nitride and machinable glasses.
- Rigid substrates such a glass may also contain a variety of surface coatings and treatments to afford solar control properties, reflectivity, decorative features, frit coatings, opacifying treatments, gradients or masking.
- the patent art herein can be employed as a universal feature for these and all broad and contemplated anticipations.
- a variety of polymeric materials that have a modulus suited for the for rigid substrate purpose and sufficient mechanical performance can include, polycarbonates, acrylic or polymethyl methacrylate, polyethylene, polypropylene, polyethylene terephthalate, polyvinyl chloride, acrylonitrile-bu- tadiene- styrene, polyamides, polyaramids, polyvinyl chloride, polystyrene, polylactic acid, polyoxymethylene, polyetheretherketone, and thermosets, such as phenolics, polyesters, epoxies and crosslinked systems such as vulcanized rubber.
- this invention relates to a laminate structure comprising a stack of at least one glass substrate adhered to an adhesive polymeric interlayer.
- the interfacial region or zone of the adhesive polymeric interlayer (API) comprises continuous and/or discrete debonding zones.
- the cohesive discrete debonding zones are substantially discrete, that is, the zones, which may or may not cover generally the entire area of the adhesive polymeric interlayer (API), in the planar direction, are substantially separate from each other with defined boundaries.
- the likely random imperfections in discreteness of the zones given the limitations of the materials, and/or the process of making the materials — for example, two zones that are substantially discrete may “bleed into” each other, de minimis— are acknowledged in the present invention.
- the discrete zones may be co-planar or may not be co-planar.
- the discrete zones in a given plane may be co-planar to at least one of the glass substrate, or to the API layer.
- the cohesive discrete debonding zones are different from the API in at least one physical and/or one chemical characteristic.
- continuous debonding zones means that the debonding zones are substantially continuous, that is, the zones cover generally the entire area of the API in the planar direction, acknowledging the likely random imperfections in continuity of the zones given the limitations of the materials, and/or the process of making the materials of the present invention.
- continuous debonding zones are coplanar to the API or to the glass substrate.
- the continuous debonding zones are different from the API in at least one physical and/or one chemical characteristic.
- FIG. 1 depicts a general laminate structure with two glass substrates (10 and 20) with an adhesive polymeric interlayer or API (30) in between the two glass substrates.
- FIG. 2 depicts an embodiment of the present invention wherein only one glass substrate (110) adheres to the adhesive polymeric interlayer (130) to form the stack (1000).
- the adhesive polymeric interlayer (API; 130) comprises discrete debonding zones (140) within the API (130) such that the debonding zones (140) are located in a region that begins at the interface (150) of the API (130) and the glass substrate (110) and extends about 10% in thickness into the API (130).
- the debonding zone’s (140) thickness is much lower than the thickness of the API (130).
- FIG. 3 depicts an embodiment of the present invention wherein only one glass substrate
- the adhesive polymeric interlayer (API; 131) comprises continuous debonding zones (141) within the API (131) such that the continuous debonding zones (141) are located in a region that begins at the interface (151) of the API (131) and the glass substrate (111) and extends about 10% in thickness into the API (131).
- the debonding zone’s (141) thickness is much lower than the thickness of the API (131).
- FIG. 4 depicts an embodiment of the present invention wherein only one glass substrate
- the adhesive polymeric interlayer (API; 132) comprises discrete debonding zones (142) and continuous debonding zones (143) within the API (132) such that the debonding zones (142 and 143) are located in a region that begins at the interface (152) of the API (132) and the glass substrate (112) and extends about 10% in thickness into the API (132).
- the debonding zone’s (142) thickness is much lower than the thickness of the API (132).
- the laminate structure can comprise more than one glass substrate and corresponding polymeric interlayers in between.
- the number of glass substrates can be 1, 2, 3, 4, 5, 6, 7,8 ,9, 10. . . 20.
- the number of API, in alternation with the glass, or in series with itself, can range from 1-20.
- Embodiments described below use a two-glass substrate with one API layer, but only as an example. It is understood that the description applies to multiple glass substrates with corresponding multiple API layers.
- this invention relates to a laminate structure comprising a stack of two glass substrates adhered to each other through an adhesive polymeric interlayer.
- the interfacial region or zone of the adhesive polymeric interlayer (API) comprises cohesive debonding zones discrete and/or continuous.
- cohesive discrete and/or continuous debond- ing zones are coplanar to the API or to both glass substrates.
- the cohesive discrete and/or continuous debonding zones are different from the API in at least one physical and/or one chemical characteristic.
- FIG. 5 depicts an embodiment of the present invention wherein two glass substrates (210 and 220) adhere to the adhesive polymeric interlayer (230) to form the stack (2000).
- the adhesive polymeric interlayer (API; 230) comprises discrete debonding zones (240) within the API (230) such that the debonding zones (240) are located in a region that begins at the interface (250) of the API (230) and the glass substrate (210) and extends about 10% in thickness into the API (230).
- the debonding zone’s (240) thickness is much lower than the thickness of the API (230).
- FIG. 6 depicts an embodiment of the present invention wherein two glass substrates (211 and 221) adhere to the adhesive polymeric interlayer (231) to form the stack (2001).
- the adhesive polymeric interlayer (API; 231) comprises continuous debonding zones (241) within the API (231) such that the continuous debonding zones (241) are located in a region that begins at the interface (251) of the API (231) and the glass substrate (211) and extends about 10% in thickness into the API (231).
- the debonding zone’s (241) thickness is much lower than the thickness of the API (231).
- FIG. 7 depicts an embodiment of the present invention wherein two glass substrates (212 and 222) adhere to the adhesive polymeric interlayer (232) to form the stack (2002).
- the adhesive polymeric interlayer (API; 232) comprises discrete debonding zones (242) and continuous debonding zones (243) within the API (232) such that the debonding zones (242 and 243) are located in a region that begins at the interface (252) of the API (232) and the glass substrate (212) and extends about 10% in thickness into the API (232).
- the debonding zone’s (242) thickness is much lower than the thickness of the API (232).
- FIG. 8 shows the peel force of a typical interlay er/glass ‘laminate’ possessing relatively uniform adhesion - this is representative of the conventional art.
- FIG. 9 shows a schematic construction of the present invention, where one glass substrate, the debonding zone treatment and the adhesive polymeric interlayer are shown.
- FIG. 10 depicts an embodiment of the present invention wherein two glass substrates (214 and 224) adhere to the adhesive polymeric interlayer (234), which is an ionomer, to form the stack (2004).
- the adhesive polymeric interlayer (API; 234) comprises FEP cohesive discrete debonding zones (244) within the API (234) such that the discrete debonding zones (244) are located in a region that begins at the interface (254) of the API (234) and the glass substrate (214) and extends about 10% in thickness into the API (234).
- the debonding zone’s (244) thickness is much lower than the thickness of the API (234).
- FIG. 11 depicts an embodiment of the present invention wherein two glass substrates (215 and 225) adhere to the adhesive polymeric interlayer (235) to form the stack (2005).
- the adhesive polymeric interlayer (API; 235) comprises FEP continuous debonding zones (245) within the API (235) such that the continuous debonding zones (245) are located in a region that begins at the interface (255) of the API (235) and the glass substrate (215) and extends about 10% in thickness into the API (235).
- the debonding zone’s (245) thickness is much lower than the thickness of the API (235).
- the laminate structure can comprise more than one glass substrate with corresponding layers in between.
- the number of glass substrates can be 1, 2, 3, 4, 5, 6, 7,8 ,9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, and 20.
- the number interlayers (API) can also be from 1-20.
- the laminated structure of the present invention comprises more than one cohesive discrete and/or continuous debonding zones.
- the cohesive discrete and/or continuous debonding zones comprise a polymeric material chemically and/or physically different from that of the API.
- the cohesive discrete and/or continuous debonding zone and the API differ in terms of molecular weight, crystallinity, density, Young’s modulus, glass transition temperature, melt-flow index, chemical composition, additive, chemical modification, or a combination of one or more of such characteristics.
- the invention provides a debonding region comprising a controlled debonding zone which, when combined with one or more layers of glass and adhesive polymeric interlayer (API) forms a laminate, provides a combination of improved toughness, adhesion, and durability.
- the invention provides a debonding zone with a controlled debonding treatment that is substantially uniform and creates substantially discrete and/or continuous debonding zones with variable fracture toughness so that debonding occurs at a prescribed fracture energy level.
- the invention provides debonding region with a controlled debonding treatment that is substantially discrete and/or continuous and creates debonding zones with variable fracture toughness with higher and lower fracture energy.
- the weight content of the discrete and/or continuous debonding zones is in the range of 1% to about 30%. Stated differently, the weight content is any one of the following numbers, as measured in percentage of the API: 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20, 21, 22, 23, 24, 25, 26, 27, 28, 29, and 30.
- the weight content can be any number within a range defined by any two numbers herein, including the endpoints of the range.
- the weight content of the discrete zones is in the range of 0.00001% to about 30%. Stated differently, the weight content is any one of the following numbers, as measured in percentage of the API: 0.00001, 0.00002, 0.00005, 0.00008, 0.00010, 0.001, 0.005, 0.008, 0.010, 0.05, 0.1, 0.5, 1, , , 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20, 21, 22, 23, 24, 25, 26, 27, 28, 29, and 30.
- the weight content of the discrete debonding zones is in the range of 0.000011% to about 1%.
- the weight content is any one of the following numbers, as measured in percentage of the API: 0.001, 0.10, 0.020, 0.030, 0.040, 0.050, 0.060, 0.070, 0.080, 0.090, and 1.00.
- the weight content can be any number within a range defined by any two numbers herein, including the endpoints of the range.
- the interfacial region comprises at least two zones, wherein the zone with maximum mean peel strength has a mean peel strength that is at least about 2 times greater than a mean peel strength of the zone with minimum mean peel strength.
- the zone with maximum mean peel strength has a mean peel strength that is from about 2 times to about 250 times greater than a mean peel strength of the zone with minimum mean peel strength.
- the interfacial region comprises at least two zones, wherein at least one of the zones has a mean peel strength of from about 0.1 to about 4.0 kJ/m 2 .
- the mean peel strength is from about 0.5 to about 3.0 kJ/ m 2 .
- the at least one of the zones has a mean peel strength of from about 8.0 to about 12.0 kJ/ m 2 .
- the mean peel strength is from about 9.0 to about 11.0 kJ/ m 2 .
- the effective diameter of the regular shaped discrete debonding zone, the random shaped discrete debonding zone, or the cluster discrete zone is from about 1 multiple to about 150,000,000-multiples of the thickness of the discrete debonding zone.
- the thickness and the size in terms of effective diameter of the discrete debonding zone can the same, or the can range in multiples of 2, 3, 4, 5, . . 100, 200, 300, . . 1000, 2000, 3000, .
- the polymeric adhesive interlayer comprises a polyvinyl acetal, an ionomer, a thermoplastic elastomer, a silane, an ethyl vinyl acetate, or combinations thereof.
- the physical and/or chemical composition of the discrete debonding zone and the API layer is different at least in one substantial aspect.
- the discrete debonding zones within said interfacial region also comprise a polyvinyl acetal, an ionomer, a thermoplastic elastomer, a silane, an ethyl vinyl acetate, or combinations thereof.
- the discrete debonding zones comprises the ionomer, wherein the ionomer resin is a sodium-neutralized ethylene-a, P-unsatu- rated carboxylic acid copolymer.
- the polyvinyl acetal is a polyvinyl butyral. Polyvinyl acetal is described infra.
- the laminate structure further comprising an adhesion modifying agent.
- the adhesion modifying agent is a silane, an alkali metal salt, an alkaline earth metal salt or a carboxylic group-containing olefinic polymer.
- the adhesion modifying agent is present in a range of from about 0.001% to about 25% by weight of the adhesive polymeric interlayer.
- the discrete and/or continuous debonding zones have a thickness of from about 0.001 mm to about 1.0 mm.
- the shape of the discrete and/or continuous debonding zone is a circle that has an area that is 30-100% of the area of the API.
- the mean peel strength of the Glass/Treatment interface zone (ZG-T) is at least 2 times greater than the mean peel strength of the API/Treatment interface zone (ZAPI-T). This provides the benefit of having high glass adhesion and durability with controlled bonding of the API (hence improved laminate toughness).
- one or more discrete and/or continuous debonding zones in each laminated structure are coplanar to said API and/or to said glass substrate/s.
- the discrete and/or continuous debonding zones are nominally coplanar and in others, they are substantially coplanar.
- one or more discrete and/or continuous debonding zones are not coplanar to at least one glass substrate.
- the interlayer sheeting will have a surface texture/roughness and the cohesive layer may fluctuate in thickness with some of these ‘bumps’ or may not completely ‘undulate’ with this roughness. Then, although the glass is reasonably flat/smooth, the final laminated composite structure may have a textured thickness.
- a plasticized polyvinyl acetal composition preferably a polyvinyl butyral composition
- the composition comprises (a) a polyvinyl acetal resin having a hydroxyl number of from about 12 to about 34, preferably of from about 15 to about 34, as determined according to ASTM D1396-92; (b) a plasticizer in an amount of from about 20, or from about 30, to about 60, or to about 50, parts per hundred (pph), based on the dry weight of the polyvinyl acetal resin; and (c) a light stabilizer/antioxidant additive package comprising an oligomeric hindered amine light stabilizer with antioxidant functionality (HALS); wherein substantially no additional antioxidant is present.
- the plasticized polyvinyl acetal composition is a plasticized polyvinyl butyral composition.
- Suitable polyvinyl acetal resins and processes for their preparation are in a general sense well known to those of ordinary skill in the relevant art, as exemplified by previously incorporated US8329793B2, US2016/0214354A1, US2016/0214352A1, US2017/0253704A1,
- the polyvinyl acetal resin can be produced by conventionally known methods of acet- alization of polyvinyl alcohol with an aldehyde.
- the polyvinyl alcohol is produced by hydrolysis of a corresponding polyvinyl acetate.
- a viscosity average polymerization degree of polyvinyl alcohol serving as a raw material of the polyvinyl acetal resin is typically 100 or more, or 300 or more, or 400 or more, or 600 or more, or 700 or more, or 750 or more, or 900 or more, or 1200 or more.
- the viscosity average polymerization degree of polyvinyl alcohol is too low, there is a concern that the penetration resistance or creep resistance properties, particularly creep resistance properties under high- temperature and high-humidity conditions, such as those at 85°C and at 85% RH, are lowered.
- the viscosity average polymerization degree of polyvinyl alcohol is typically 5000 or less, or 3000 or less, or 2500 or less, or 2300 or less, or 2000 or less.
- the viscosity average polymerization degree of polyvinyl alcohol is more than 5000, there is a concern that the extrusion of a resin film is difficult.
- the polyvinyl acetal resin is generally constituted of vinyl acetal units, vinyl alcohol units and vinyl acetate units, and these respective units can be, for example, measured by the “Testing Methods for Polyvinyl Butyral” of JIS K 6728, or a nuclear magnetic resonance method (NMR).
- a polyvinyl acetal resin is used having a hydroxyl number of from about 12 to about 34, preferably of from about 15 to about 34 (as determined according to ASTM D1396- 92).
- the polyvinyl acetal resin contains a unit other than the vinyl acetal unit
- the remaining vinyl acetal unit quantity can be calculated.
- the aldehyde which is used for acetalization of polyvinyl alcohol is preferably an aldehyde having 1 or more and 12 or less carbon atoms.
- the carbon number of the aldehyde is more than 12, the reactivity of the acetalization is lowered, and moreover, blocking of the resin is liable to be generated during the reaction, and the synthesis of the polyvinyl acetal resin is liable to be accompanied with difficulties.
- the aldehyde is not particularly limited, and examples thereof include aliphatic, aromatic, or alicyclic aldehydes, such as formaldehyde, acetaldehyde, propionaldehyde, n-butyl aldehyde, isobutyl aldehyde, valeraldehyde, n-hexyl aldehyde, 2-ethylbutyl aldehyde, n-heptyl aldehyde, n-octyl aldehyde, n-nonyl aldehyde, n-decyl aldehyde, benzaldehyde, cinnamaldehyde, etc.
- aldehyde such as formaldehyde, acetaldehyde, propionaldehyde, n-butyl aldehyde, isobutyl aldehyde, valeraldehyde, n-hexy
- aliphatic aldehydes having 2 or more and 6 or less carbon atoms are preferred, and above all, butyl aldehyde is especially preferred.
- the above-described aldehydes may be used solely or may be used in combination of two or more thereof.
- a small amount of a polyfunctional aldehyde or an aldehyde having other functional group, or the like may also be used in combination in an amount in the range of 20% by mass or less.
- the polyvinyl acetal resin is most preferably polyvinyl butyral.
- the polyvinyl acetal resin compositions of the present invention contain a plasticizer.
- Suitable plasticizers can be chosen from any that are known or used conventionally in the manufacture of plasticized PVB sheeting compositions.
- a plasticizer suitable for use herein can be a plasticizer or a mixture of plasticizers selected from the group consisting of: diesters obtained from the chemical reaction of aliphatic diols with carboxylic acids, including diesters of polyether diols or polyether polyols; and esters obtained from polyvalent carboxylic acids and aliphatic alcohols.
- plasticizer For convenience, when describing the sheet compositions of the present invention, a mixture of plasticizers can be referred to herein as "plasticizer". That is, the singular form of the word "plasticizer” as used herein can represent the use of either one plasticizer or the use of a mixture of two or more plasticizers in a given sheet composition. The intended use will be apparent to a reader skilled in the art.
- Preferred plasticizers for use herein are diesters obtained by the reaction of triethylene glycol or tetraethylene glycol with aliphatic carboxylic acids having from 6 to 10 carbon atoms; and diesters obtained from the reaction of sebacic acid with aliphatic alcohols having from 1 to 18 carbon atoms.
- the plasticizer is either tetraethylene glycol di(2-heptanoate) (4G7), tri ethyleneglycol di-(2-ethyl hexanoate) (3 GO), dihexyl adipate (DHA), triethylene glycol di(2-ethylbutyrate (3GH) or dibutyl sebacate (DBS). Most preferably the plasticizer is 3 GO.
- the poly(vinyl) acetal resins of present invention may include a surfactant.
- a surfactant suitable for use herein can be any that is known to be useful in the art of polyvinyl acetal manufacture.
- surfactants suitable for use herein include: sodium lauryl sulfate; ammonium lauryl sulfate; sodium dioctyl sulfosuccinate; ammonium perfluorocarboxylates having from 6 to 12 carbon atoms; sodium aryl sulfonates, adducts of chlorinated cyclopentadiene and maleic anhydride; partially neutralized polymethacrylic acid; alkylaryl sulfonates; sodium N-oleyl-N-me- thyl laurate; sodium alkylaryl polyether sulfonates; triethanolamine lauryl sulfate; diethyl dicyclohexyl ammonium lauryl sulfate; sodium
- Preferable surfactants include sodium lauryl sulfate, sodium dioctyl sulfosuccinate, sodium cocomethyl tauride, and decyl(sulfophenoxy)benzenesulfonic acid disodium salt. It has been found that sodium dodecyl sulfate (SDS) and sodium lauryl sulfate (SLS) are particularly useful.
- the surfactant can be included in any effective amount for the particular set of process conditions practiced.
- the surfactant can be included in an amount of from about 0.01, or from about 0.10, or from about 0.15, to about 0.85, or to about 0.80, or to about 0.75, or to about 0.70, pph by weight, based on the weight of polyvinyl acetate resin ultimately used to prepare the polyvinyl acetal.
- adhesion modifiers include, for example, those disclosed in International Patent Application Publication No. WO03/033583 Al .
- Alkali metal salts and alkaline earth metal salts are typically used, for example, salts of potassium, sodium, magnesium, and the like.
- the salt include salts of organic acids, such as octanoic acid, hexanoic acid, butyric acid, acetic acid and formic acid; inorganic acids, such as hydrochloric acid and nitric acid; and the like. Magnesium compounds are preferred.
- the ionomer resin is a sodium-neutralized eth- ylene-a,P-unsaturated carboxylic acid copolymer, which includes resins having constituent units derived from ethylene, constituent units derived from an a,P-unsaturated carboxylic acid and optionally other constituent units as described below, in which at least a part of the constituent units derived from the a,P-unsaturated carboxylic acid are neutralized with a sodium ion.
- a content proportion of the constituent units derived from an a,P-unsaturated carboxylic acid is typically 2% by mass or more, or 5% by mass or more (based on total copolymer mass).
- the content proportion of the constituent units derived from an a,P-unsaturated carboxylic acid is typically 30% by mass or less (based on total copolymer mass).
- Examples of the a,P-unsaturated carboxylic acid constituting the ionomer include, without limitation, acrylic acid, methacrylic acid, itaconic acid, maleic acid, fumaric acid, and mixtures of two or more thereof.
- the a,P-ethylenically unsaturated carboxylic acid is selected from acrylic acid, methacrylic acid, and mixtures thereof.
- the a,P-ethylenically unsaturated carboxylic acid is methacrylic acid.
- the ethylene acid copolymer may further comprise copolymerized units of one or more additional comonomer(s), such as an a,P-ethylenically unsaturated carboxylic acid ester.
- additional comonomer(s) such as an a,P-ethylenically unsaturated carboxylic acid ester.
- alkyl esters having 3 to 10, or 3 to 8 carbons are typically used.
- esters of unsaturated carboxylic acids include, without limitation, methyl acrylate, methyl methacrylate, ethyl acrylate, ethyl methacrylate, propyl acrylate, propyl methacrylate, isopropyl acrylate, isopropyl methacrylate, n-butyl acrylate, n-butyl methacrylate, isobutyl acrylate, isobutyl methacrylate, tert-butyl acrylate, tert-butyl methacrylate, octyl acrylate, octyl methacrylate, undecyl acrylate, undecyl methacrylate, octadecyl acrylate, octadecyl methacrylate, dodecyl acrylate, dodecyl methacrylate, 2-ethylhexyl acrylate, 2-ethylhexyl methyl
- the additional comonomers are selected from methyl acrylate, methyl methacrylate, n-butyl acrylate, n-butyl methacrylate, isobutyl acrylate, isobutyl methacrylate, glycidyl methacrylate, vinyl acetate, and mixtures of two or more thereof.
- the additional comonomer is one or more of n-butyl acrylate, n-butyl methacrylate, isobutyl acrylate and isobutyl methacrylate.
- the additional comonomer is one or both of n-butyl acrylate and isobutyl acrylate.
- Suitable ethylene acid copolymers have a melt flow rate (MFR) of from about 1, or from about 2, to about 4000 g/10 min, or to 1000 g/10 min, or to about 400 g/10 min, as determined in accordance with ASTM method D1238-89 at 190°C and 2.16 kg.
- MFR melt flow rate
- suitable ethylene acid copolymers may be synthesized as described, for example, in US Patent Nos. 3404134, 5028674, 6500888, 6518365, 8334033 and 8399096.
- a method described in US Patent No. 8399096 is used, and a sufficiently high level and complementary amount of the derivative of the second a,P-ethylenically unsaturated carboxylic acid is present in the reaction mixture.
- the ethylene acid copolymers are partially neutralized by reaction with one or more bases.
- An example of a suitable procedure for neutralizing the ethylene acid copolymers is described in US PatentNos. 3404134 and 6518365.
- the acid groups are neutralized to a level of about 1%, or about 10%, or about 15%, or about 20%, to about 90%, or to about 60%, or to about 55%, or to about 30%, based on the total content of carboxylic acid groups present in the ethylene acid copolymers as calculated or measured for the non-neutralized ethylene acid copolymers.
- the neutralization level can be tailored for the specific end-use.
- the counterions to the carboxylate anions in the ionomer are sodium cations. While ionomers used in the present invention are sodium-neutralized ionomers, counterions other than sodium cations may be present in small amounts of less than 5 equivalent %, or less than 3 equivalent %, or less than 2 equivalent %, or less than 1 equivalent %, based on the total equivalents of carboxylate groups in the ionomer. In one embodiment, the counterions are substantially sodium ions.
- Suitable cations other than sodium include any positively charged species that is stable under the conditions in which the ionomer composition is synthesized, processed, and used. Suitable cations may be used in combinations of two or more. Typically, such other cations are metal cations, which may be monovalent, divalent, trivalent, or multivalent. Monovalent metal cations include but are not limited to cations of potassium, lithium, silver, mercury, copper, and the like. Divalent metal cations include but are not limited to cations of beryllium, magnesium, calcium, strontium, barium, copper, cadmium, mercury, tin, lead, iron, cobalt, nickel, zinc, and the like.
- Trivalent metal cations include but are not limited to cations of aluminum, scandium, iron, yttrium, and the like.
- Multivalent metal cations include but are not limited to cations of titanium, zirconium, hafnium, vanadium, tantalum, tungsten, chromium, cerium, iron, and the like.
- complexing agents such as stearate, oleate, salicylate, and phenolate radicals may be included, as described in US Patent No. 3404134.
- the metal cations used are monovalent or divalent metal cations, such as lithium, magnesium, zinc, potassium, and combinations of one or more of these metal cations.
- counterions other than sodium are present in at most “contaminant” amounts, as one would typically find in industrial situations, as would be recognized by persons of ordinary skill in the relevant art.
- the resulting sodium-neutralized ethylene acid copolymer has a melt index, as determined in accordance with ASTM method D1238-89 at 190°C and 2.16 kg, that is lower than that of the corresponding ethylene acid copolymer.
- the ionomer’s melt index depends on a number of factors, including the melt index of the ethylene acid copolymer, the amount of copolymerized acid, the neutralization level, the identity of the cation and its valency. Moreover, the desired value of the ionomer’s melt index may be determined by its intended end use.
- the ionomer has a melt index of about 1000 g/10 min or less, or about 750 g/10 min or less, or about 500 g/10 min or less, or about 250 g/10 min or less, or about 100 g/10 min or less, or about 50 g/10 min or less, or about 25 g/10 min or less, or about of 20 g/10 min or less, or about 10 g/10 min or less, or about 7.5 g/10 min or less, as determined in accordance with ASTM method D1238-89 at 190°C and 2.16 kg.
- the ionomer is an at least partially sodium-neutralized ethylene acid dipolymer comprising (consisting essentially of) copolymerized units of:
- the ionomer is an at least partially sodium-neutralized ethylene acid terpolymer comprising copolymerized units of:
- Such terpolymer ionomers are generally disclosed in International Patent Application Nos. WO 2015/199750A1 and WO 2014/100313A1, as well as in previously incorporated US Provisional Application Ser. No. 62/333,371 (filed 9 May 2016).
- the a,P-unsatu- rated carboxylic acid is methacrylic acid.
- the a,P-unsaturated carboxylic acid ester is n-butyl acrylate, isobutyl acrylate or a mixture thereof.
- the copolymer consists essentially of copolymerized units of (i), (ii) and (iii).
- Thermoplastic elastomers can be used in the multilayer polymeric interlayer described above. These materials generally provide polymeric interlayer sheets and laminates comprising these sheets with improved acoustic properties, as described in US Published Patent Application No. 2017/0320297A1.
- these materials also referred to as “elastomers”, generally include materials with soft and hard segments, such as a polystyrene-based elastomer (soft segment: polybutadiene, polyisoprene/hard segment: polystyrene), a polyolefin-based elastomer (soft segment: ethylene propylene rubber/hard segment: polypropylene), a polyvinyl chloridebased elastomer (soft segment: polyvinyl chloride/hard segment: polyvinyl chloride), a polyurethane-based elastomer (soft segment: polyether, polyester, or polycarbonate/hard segment: polyurethane), a polyester-based elastomer (soft segment: aliphatic polyester/hard segment: aromatic polyester), a polyether ester-based elastomer (soft segment: polyether/hard segment: polyester), a polyamide-based elastomer (soft segment: polypropylene glycol, polytetramethylene ether
- a content of the hard segment in the thermoplastic elastomer is preferably about 5% by mass or more, or about 7% by mass or more, or about 8% by mass or more, or about 10% by mass or more, or about 14% by mass or more, or about 16% by mass or more, or about 18% by mass or more, relative to the total amount of the thermoplastic elastomer.
- a content of the hard segment is preferably about 40% by mass or less, or about 30% by mass or less, or about 20% by mass or less, relative to the total amount of the thermoplastic elastomer.
- the content of the hard segment is less than about 5% by mass, there is a tendency for the molding of the layer B to be difficult, the height of the peak of tan 6 is small, the flexural rigidity of the laminate is small, or the sound insulating properties in a high-frequency region is lowered.
- the content of the hard segment is more than about 40% by mass, there is a tendency for the characteristics of the thermoplastic elastomer to be hardly exhibited, the stability of sound insulating performance is lowered, or the sound insulating characteristics in the vicinity of room temperature are lowered.
- a content of the soft segment in the thermoplastic elastomer is preferably about 60% by mass or more, or about 70% by mass or more, or about 80% by mass or more, relative to the total amount of the thermoplastic elastomer.
- the content of the soft segment is preferably about 95% by mass or less, or about 92% by mass or less, or about 90% by mass or less, or about 88% by mass or less, or about 86% by mass or less, or about 84% by mass or less, or about 82% by mass or less relative to the total amount of the thermoplastic elastomer.
- the content of the soft segment is less than about 60% by mass, the characteristics of the thermoplastic elastomer tend to be hardly exhibited.
- the content of the soft segment is more than about 95% by mass, there is a tendency that the molding of the layer B is difficult, the height of the peak of tan 6 is small, the flexural rigidity of the laminate is small, or the sound insulating properties in a high-frequency region are lowered.
- the contents of the hard segment and the soft segment in the thermoplastic elastomer are each considered as an average value of the mixture.
- thermoplastic elastomer From the viewpoint of making both the moldability and the sound insulating properties compatible with each other, it is more preferred to use a block copolymer having a hard segment and a soft segment as the thermoplastic elastomer. Furthermore, from the viewpoint of further improving the sound insulating properties, it is preferred to use a polystyrene-based elastomer.
- crosslinked rubbers of natural rubber, isoprene rubber, butadiene rubber, chloroprene rubber, nitrile rubber, butyl rubber, ethylene propylene rubber, urethane rubber, silicone rubber, chlorosulfonated polyethylene rubber, acrylic rubber, fluorine rubber, and the like may be used as the thermoplastic elastomer.
- the thermoplastic elastomer is preferably a copolymer of an aromatic vinyl monomer and a vinyl monomer or a conjugated diene monomer, or a hydrogenated product of the copolymer.
- the copolymer is preferably a block copolymer having an aromatic vinyl polymer block and an aliphatic unsaturated hydrocarbon polymer block, for example, a polystyrene-based elastomer.
- the binding form of these polymer blocks is not particularly limited, and it may be any of a linear binding form, a branched binding form, a radial binding form, and a combined binding form of two or more thereof. Of those, a linear binding form is preferred.
- examples of the linear binding form include a diblock copolymer expressed by a-b, a triblock copolymer expressed by a-b-a or b-a-b, a tetrablock copolymer expressed by a-b-a-b, a pentablock copolymer expressed by a-b-a-b-a or b-a-b- a-b, an (a-b)nX type copolymer (X represents a coupling residual group, and n represents an integer of 2 or more), and a mixture thereof.
- a sum total of an aromatic vinyl monomer unit and an aliphatic unsaturated hydrocarbon monomer unit in the block copolymer is preferably about 80% by mass or more, or about 95% by mass or more, or about 98% by mass or more relative to the whole of the monomer units. It is to be noted that a part or the whole of the aliphatic unsaturated hydrocarbon polymer blocks in the block copolymer may be hydrogenated.
- a content of the aromatic vinyl monomer unit in the block copolymer is preferably about 5% by mass or more, or about 7% by mass or more, or about 8% by mass or more, or about 14% by mass or more, or about 16% by mass or more, or about 18% by mass or more, relative to the whole of the monomer units of the block copolymer.
- a content of the aromatic vinyl monomer unit is preferably about 40% by mass or less, or about 30% by mass or less, or about 25% by mass or less, or about 20% by mass or less, relative to the whole of the monomer units of the block copolymer.
- the content of the aromatic vinyl monomer unit in the block copolymer can be determined from a charge ratio of the respective monomers in synthesizing the block copolymer, or the measurement results of X H-NMR or the like of the block copolymer.
- the content of the aromatic vinyl monomer unit in the block copolymer is considered as an average value of the mixture.
- a monomer other than the aromatic vinyl monomer may be copolymerized so long as its amount is small.
- a proportion of the aromatic vinyl monomer unit in the aromatic vinyl polymer block is preferably about 80% by mass or more, or about 95% by mass or more, or about 98% by mass or more relative to the whole of the monomer units in the aromatic vinyl polymer block.
- aromatic vinyl monomer constituting the aromatic vinyl polymer block examples include styrene; alkyl styrenes, such as a-methyl styrene, 2-m ethyl styrene, 3 -methyl styrene, 4-me- thylstyrene, 4-propyl styrene, 4-cyclohexylstyrene and 4-dodecylstyrene; arylstyrenes, such as 2- ethyl-4-benzylstyrene, 4-(phenylbutyl)styrene, 1-vinylnaphthalene and 2-vinylnaphthalene; halogenated styrenes; alkoxystyrenes; vinylbenzoate esters; and the like. These aromatic vinyl monomers may be used solely or may be used in combination of two or more thereof.
- a content of the aliphatic unsaturated hydrocarbon monomer unit in the block copolymer is preferably about 60% by mass or more, or about 70% by mass or more, or about 75% by mass or more, or 80% by mass or more, relative to the whole of the monomer units of the block copolymer.
- the content of the aliphatic unsaturated hydrocarbon monomer unit in the block copolymer is preferably about 95% by mass or less, or about 92% by mass or less, or about 90% by mass or less, or about 88% by mass or less, or about 86% by mass or less, or about 84% by mass or less, or about 82% by mass or less, relative to the whole of the monomer units of the block copolymer.
- the content of the aliphatic unsaturated hydrocarbon monomer unit in the block copolymer can be determined from a charge ratio of the respective monomers in synthesizing the block copolymer, or the measurement results of 'H-NMR or the like of the block copolymer.
- the content of the aliphatic unsaturated hydrocarbon monomer unit in the block copolymer is considered as an average value of the mixture.
- a monomer other than the aliphatic unsaturated hydrocarbon monomer may be copolymerized so long as its amount is small.
- a proportion of the aliphatic unsaturated hydrocarbon monomer unit in the aliphatic unsaturated hydrocarbon polymer block is preferably about 80% by mass or more, or about 95% by mass or more, or about 98% by mass or more, relative to the whole of the monomer units in the aliphatic unsaturated hydrocarbon polymer block.
- Examples of the aliphatic unsaturated hydrocarbon monomer constituting the aliphatic unsaturated hydrocarbon polymer block include ethylene, propylene, 1 -butene, 1 -pentene, 1 -hexene, 1 -heptene, 1 -octene, 1 -nonene, 1 -decene, 4-phenyl-l -butene, 6-phenyl-l -hexene, 3-methyl- 1 -butene, 4-methyl-l -butene, 3 -methyl- 1 -pentene, 4-m ethyl- 1 -pentene, 3 -methyl- 1 -hexene, 4-me- thyl-1 -hexene, 5-methyl-l -hexene, 3, 3 -dimethyl- 1 -pentene, 3,4-dimethyl-l -pentene, 4,4-dime- thyl-1 -pentene, vinylcyclo
- the aliphatic unsaturated hydrocarbon monomer is preferably an aliphatic unsaturated hydrocarbon having 2 or more carbon atoms, or an aliphatic hydrocarbon having 4 or more carbon atoms, and is preferably an aliphatic unsaturated hydrocarbon having 12 or less carbon atoms, or an aliphatic hydrocarbon having 8 or less carbon atoms.
- butadiene, isoprene, and a combination of butadiene and isoprene are preferred.
- the aliphatic unsaturated hydrocarbon monomer is preferably a conjugated diene.
- the conjugated diene is preferably a hydrogenated product resulting from hydrogenating a part or the whole thereof.
- a hydrogenation ratio is preferably 80% or more, or 90% or more.
- the hydrogenation ratio as referred to herein is a value obtained by measuring an iodine value of the block copolymer before and after the hydrogenation reaction.
- a weight average molecular weight of the block copolymer is preferably about 30,000 or more, or about 50,000 or more and preferably about 400,000 or less, or about 300,000 or less.
- a ratio (Mw/Mn) of weight average molecular weight to number average molecular weight of the block copolymer is preferably about 1.0 or more, and preferably about 2.0 or less, or about 1.5 or less.
- the weight average molecular weight refers to a weight average molecular weight as reduced into polystyrene as determined by the gel permeation chromatography (GPC) measurement
- the number average molecular weight refers to a number average molecular weight as reduced into polystyrene as determined by the GPC measurement.
- the block copolymer can be, for example, produced by an anionic polymerization method, a cationic polymerization method, a radical polymerization method, or the like.
- anionic polymerization specific examples thereof include:
- thermoplastic elastomer in the case of using a conjugated diene as the aliphatic unsaturated hydrocarbon monomer, by adding an organic Lewis base on the occasion of anionic polymerization, a 1,2-bond quantity and a 3,4-bond quantity of the thermoplastic elastomer can be increased, and the 1,2-bond quantity and the 3,4-bond quantity of the thermoplastic elastomer can be easily controlled by the addition amount of the organic Lewis base. By controlling them, the peak temperature or height of tan 6 can be adjusted.
- Examples of the organic Lewis base include esters, such as ethyl acetate; amines, such as tri ethylamine, N,N,N’,N’ -tetramethylethylenediamine (TMEDA) and N-m ethylmorpholine; ni- trogen-containing heterocyclic aromatic compounds, such as pyridine; amides, such as dimethylacetamide; ethers, such as dimethyl ether, diethyl ether, tetrahydrofuran (THF) and dioxane; glycol ethers, such as ethylene glycol dimethyl ether and diethylene glycol dimethyl ether; sulfoxides, such as dimethyl sulfoxide; ketones, such as acetone and methyl ethyl ketone; and the like.
- esters such as ethyl acetate
- amines such as tri ethylamine, N,N,N’,N’ -tetramethylethylenedi
- the hydrogenation reaction can be conducted by dissolving the obtained unhydrogenated polystyrene-based elastomer in a solvent inert to a hydrogenation catalyst, or allowing the unhydrogenated polystyrene-based elastomer to react directly with hydrogen without being isolated from a reaction liquid in the presence of a hydrogenation catalyst.
- the hydrogenation ratio is preferably about 60% or more, or about 80% or more, or about 90% or more.
- Examples of the hydrogenation catalyst include Raney nickel; heterogeneous catalysts in which a metal, such as Pt, Pd, Ru, Rh and/or Ni, is supported on a carrier, such as carbon, alumina and/or diatomaceous earth; Ziegler-based catalysts composed of a combination of a transition metal compound with an alkylaluminum compound and/or an alkyllithium compound; metallocene-based catalysts; and the like.
- the hydrogenation reaction can be generally conducted under conditions at a hydrogen pressure of about 0.1 MPa or more and about 20 MPa or less and at a reaction temperature of about 20°C or higher and about 250°C or lower for a reaction time of about 0.1 hours or more and about 100 hours or less.
- the thermoplastic elastomer has a sea-island phase separated structure in which the hard segment block is included as an island component and the soft segment block is included as a sea component. It has been found that the phase separation size of an island component is sometimes increased in a layer to be used in an interlayer for a laminated glass, and therefore, the interlayer for a laminated glass shrinks when producing a laminated glass or the haze of the laminated glass is decreased, and also found that a laminated glass using an interlayer for a laminated glass having a specific structure has excellent sound insulating properties even when the thickness is reduced and also has low shrinkability.
- the thermoplastic elastomer includes a hard segment block and a soft segment block
- the layer B has a sea-island phase separated structure in which the hard segment block is included as an island component and the soft segment block is included as a sea component
- the degree of orientation (1) is defined by the following formula (I) based on the maximum intensity value and the minimum intensity value in an arbitrary azimuth range of 180° including the azimuth at which the intensity reaches the maximum in the azimuthal intensity distribution of periodic scattering or coherent scattering by the hard segment block or the soft segment block obtained for the layer A by small-angle X-ray scattering measurement
- the degree of orientation (1) is about 0.9 or less.
- the degree of orientation (2) is about 10 or less.
- Degree of orientation (2) maximum intensity value/minimum intensity value (II) [0231] It is also preferred that, when an island component having a largest major axis size is selected from the island components having a substantially elliptical shape or a substantially continuous linear shape in each phase image obtained by observation with an atomic force microscope of a region in the range of 200 nm x 200 nm at arbitrary 5 sites on a sliced surface obtained by slicing a central area in the thickness direction of the layer B along a plane substantially parallel to the layer B, the average of the major axis size of the selected island components is about 100 nm or less.
- thermoplastic elastomers [0232] Specific examples of suitable thermoplastic elastomers can be found, for example, by reference to US Published Patent Application No. 2010/0239802.
- the thermoplastic elastomer is a hydrogenated block copolymer formed by hydrogenating a block copolymer comprising at least a polymer block (A) constituted predominantly from an aromatic vinyl compound unit and a polymer block (B) constituted predominantly from a 1,3-butadiene unit or constituted predominantly from an isoprene unit and a 1,3-butadiene unit, wherein a content of the polymer block (A) is from about 5% to about 40% mass on the basis of a total amount of the hydrogenated block copolymer, wherein the polymer block (B) has a hydrogenation rate of about 70% or more, and wherein the hydrogenated block copolymer has a glass transition temperature of from about -45°C to about 30°C.
- the thermoplastic elastomer is a hydrogenated block copolymer formed by hydrogenating a block copolymer comprising at least a polymer block (C) constituted predominantly from an aromatic vinyl compound unit and a polymer block (D) constituted predominantly from a 1,3-butadiene unit or constituted predominantly from an isoprene unit and a 1,3-butadiene unit, wherein a content of the polymer block (C) is from about 10% to about 40% mass on the basis of a total amount of the hydrogenated block copolymer, wherein the polymer block (D) has a hydrogenation rate of about 80% or more, and wherein the hydrogenated block copolymer has a glass transition temperature of less than about -45°C.
- the aromatic vinyl compound is styrene
- the polymer block (B) and (D) are constituted predominantly from an isoprene unit and a 1,3-butadiene unit
- the hydrogenated block copolymer is a tri-block copolymer having an A1-B-A2 or C1-D-C2 type structure.
- EVA Ethylene Vinyl Acetate
- the API can be an ethylene vinyl acetate (EVA)-type material, such as disclosed in US Published Patent Application No. 2016/0167348A1.
- EVA material comprises ethylene vinyl acetate having a vinyl acetate content of greater than about 25 wt.%, or from about 30 wt.%, to about 40 wt.%, or to about 35 wt.%, or about 33 wt.%; an initial melt flow index of at least about 14 g/10 min, and a final melt flow index of about 2 g/10 min or lower, or about 1.5 g/10 min or lower, after the material is cross-linked by one or more methods known to those of ordinary skill in the relevant art (for example, thermally crosslinked with the aid of a peroxide crosslinker).
- Silanes suitable for use in accordance with the present invention are dialkoxysilanes. Without being held to theory, it is believed that the hydrolyzed silanol portion of the silane can form an adhesive bond with the glass surface (silanols), thereby enhancing the adhesive force at the interface between the polymer and glass surface. The remaining portion of the silane molecule should then ‘anchor’ in some fashion and to some degree, with the surrounding ionomer resin ‘matrix’.
- each of the alkoxy groups individually contains from 1 to 3 carbon atoms.
- Suitable examples include diethoxydimethylsilane, diethoxyl(methyl)vinylsilane, 1,3-di- ethoxy-l,l,3,3-tertramethyldisiloxane, dimethoxy dimethylsilane, dimethoxylmethylvinylsilane, methyldiethoxysilane, diisopropyldimethoxysilane, dicyclopentyldimethoxysilane, y-aminopro- pyl-N-cy cl ohexylmethyldimethoxy silane, 3 -aminopropylmethyldimethoxy silane, N-phenyl-3- aminopropylmethyldimethoxy silane, N-phenyl-3 -aminopropylmethyldi ethoxy silane, N-P-(ami- noethyl)-y-amino
- the silane in addition to the alkoxy groups also contains an “active” chemical group for bonding into the ionomer resin matrix, for example, a carboxylic acid- reactive group such as an amino group or a glycidyl group.
- an “active” chemical group for bonding into the ionomer resin matrix for example, a carboxylic acid- reactive group such as an amino group or a glycidyl group.
- Suitable examples include y-aminopro- pyl-N-cy cl ohexylmethyldimethoxy silane, 3 -aminopropylmethyldimethoxy silane, N-phenyl-3 - aminopropylmethyldimethoxy silane, N-phenyl-3 -aminopropylmethyldi ethoxy silane, N-P-(ami- noethyl)-y-aminopropylmethyldimethoxy silane and 3-glycidoxypropylmethyl di ethoxy silane.
- the silane is a liquid under ambient conditions (for example, at 20°C).
- specific such examples include N-P-(aminoethyl)-y-aminopropylmethyldimethoxysilane (CAS #3069-29-2) and 3-glycidoxypropylmethyldiethoxysilane (CAS #2897-60-1).
- the resin composition and masterbatch of the present invention may contain one or more other additives including, for example, an antioxidant, an ultraviolet ray absorber, a photostabilizer, an antiblocking agent, a pigment, a dye, a heat shielding material (infrared ray absorber) and the like, or mixtures thereof.
- an antioxidant for example, an antioxidant, an ultraviolet ray absorber, a photostabilizer, an antiblocking agent, a pigment, a dye, a heat shielding material (infrared ray absorber) and the like, or mixtures thereof.
- the antioxidant include phenol-based antioxidants, phosphorus-based antioxidants, sulfur-based antioxidants, and the like. Of those, phenol-based antioxidants are preferred, and alkyl-substituted phenol-based antioxidants are especially preferred.
- phenol-based antioxidant examples include acrylate-based compounds, such as 2-t-butyl-6-(3-t-butyl-2-hydroxy-5-methylbenzyl)-4-methylphenyl acrylate and 2,4-di-t-amyl-6- (l-(3,5-di-t-amyl-2-hydroxyphenyl)ethyl)phenyl acrylate; alkyl-substituted phenol-based compounds, such as 2,6-di-t-butyl-4-methylphenol, 2,6-di-t-butyl-4-ethylphenol, octadecyl-3-(3,5-di- t-butyl-4-hydroxyphenyl)propionate, 2,2’-methylene-bis(4-methyl-6-t-butylphenol), 4,4’-butyli- dene-bis(4-methyl-6-t-butylphenol), 4,4’-butylidene-bis(6-t-
- Examples of the phosphorus-based antioxidant include monophosphite-based compounds, such as triphenyl phosphite, diphenylisodecyl phosphite, phenyldiisodecyl phosphite, tris(nonylphenyl) phosphite, tris(dinonylphenyl) phosphite, tris(2-t-butyl-4-methylphenyl) phosphite, tris(2,4-di-t-butyl) phosphite, tris(cyclohexylphenyl) phosphite, 2,2-methylenebis(4,6-di-t- butylphenyl)octyl phosphite, 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, 10-(3,5-di- t-butyl-4-hydroxybenzyl)-9
- sulfur-based antioxidant examples include dilauryl 3,3 ’-thiodipropionate, dis- tearyl 3,3-thiodipropionate, lauryl stearyl 3,3 ’-thiodipropionate, pentaerythritol-tetrakis-(P-lauryl- thiopropionate), 3,9-bis(2-dodecylthioethyl)-2,4,8,10-tetraoxaspiro[5.5]undecane, and the like.
- antioxidants can be used solely or in combination of two or more thereof.
- the antioxidant utilized is typically about 0.001 parts by weight or more, or about 0.01 parts by weight or more, based on 100 parts by weight of the ionomer resin.
- the amount of antioxidant utilized is typically about 5 parts by weight or less, or about 1 part by weight or less, based on 100 parts by weight of the ionomer resin.
- ultraviolet ray absorber examples include benzotriazole-based ultraviolet ray absorbers, such as 2-(5-methyl-2- hydroxyphenyl)benzotriazole, 2-[2-hydroxy-3,5-bis(a,a’-dimethylbenzyl)phenyl]-2H-benzotria- zole, 2-(3,5-di-t-butyl-2-hydroxyphenyl)benzotriazole, 2-(3-t-butyl-5-methyl-2-hydroxyphenyl)- 5-chlorobenzotriazole, 2-(3,5-di-t-butyl-5-methyl-2-hydroxyphenyl)-5-chlorobenzotriazole and 2- (3,5-di-t-amyl-2-hydroxyphenyl)benzotriazole, 2-(2’ -hydroxy-5 ’-t-octylphenyl)triazole.; hindered amine-based ultraviolet ray absorbers, such as 2,2,6,6-tetramethyl-4-piperidyl be
- ultraviolet ray absorbers can be used solely or in combination of two or more thereof.
- the amount of ultraviolet ray absorber utilized is typically about 10 ppm by weight or more, or about 100 ppm by weight or more, based on the weight of the ionomer resin.
- the amount of ultraviolet ray absorber utilized is typically about 50,000 ppm or less, or about 10,000 ppm or less, based on the weight of the ionomer resin.
- UV absorbers In some embodiments, it is also possible to use two or more types of UV absorbers in combination.
- no UV absorber is added, or the laminate is substantially UV absorber additive free.
- Examples of the photostabilizer include hindered amine-based materials, such as “ADEKA STAB LA-57” (a trade name) manufactured by Adeka Corporation, and “TINUVIN 622” (a trade name) manufactured by Ciba Specialty Chemicals Inc.
- a transmittance at a wavelength of 1,500 nm can be regulated to about 50% or less, or the TDS value (calculated from ISO 13837:2008) can be regulated to less than about 43%.
- Examples of the heat-shielding fine particle include a metal-doped indium oxide, such as tin-doped indium oxide (ITO), a metal-doped tin oxide, such as antimony-doped tin oxide (ATO), a metal-doped zinc oxide, such as aluminum-doped zinc oxide (AZO), a metal element adhesive polymeric tungsten oxide represented by a general formula: MmWOn (M represents a metal element; m is about 0.01 or more and about 1.0 or less; and n is about 2.2 or more and about 3.0 or less), zinc antimonate (ZnSb20s), lanthanum hexaboride, and the like.
- ITO tin-doped indium oxide
- ATO antimony-doped tin oxide
- AZO aluminum-doped zinc oxide
- MmWOn M represents a metal element
- m is about 0.01 or more and about 1.0 or less
- n is about 2.2
- ITO, ATO, and a metal element adhesive polymeric tungsten oxide are preferred, and a metal element adhesive polymeric tungsten oxide is more preferred.
- the metal element represented by M in the metal element adhesive polymeric tungsten oxide include Cs, Tl, Rb, Na, K, and the like, and in particular, Cs is preferred.
- m is preferably about 0.2 or more, or about 0.3 or more, and it is preferably about 0.5 or less, or about 0.4 or less.
- an average particle diameter of the heat shielding fine particle is preferably about 100 nm or less, or about 50 nm or less.
- the average particle diameter of the heat shielding particle as referred to herein means one measured by a laser diffraction instrument.
- a content of the heat shielding fine particle is preferably about 0.01% by weight or more, or about 0.05% by weight or more, or about 0.1% by weight or more, or about 0.2% by weight or more relative to the weight of the ionomer resin.
- the content of the heat shielding fine particle is preferably about 5% by weight or less, or about 3% by weight or less.
- the heat shielding compound include phthalocyanine compounds, naphthalocyanine compounds, and the like. From the viewpoint of further improving the heat shielding properties, it is preferred that the heat shielding compound contains a metal.
- a content of the heat shielding compound is preferably about 0.001% by weight or more, or about 0.005% by weight or more, or about 0.01% by weight or more, based on the weight of the ionomer resin. In addition, the content of the heat shielding compound is preferably about 1% by weight or less, or about 0.5% by weight or less.
- the dispersion coating composition may include other additives known in the art.
- the composition may include a wax additive, such as a microcrystalline wax or a polyethylene wax, which serves as an anti-blocking agent as well as to improve the coefficient of friction of the final coated substrate.
- additives include fumed silica, which reduces the tack of the coating at room temperature, fillers, cross-linking agents, anti-static agents, defoamers, dyes, brighteners, processing aids, flow enhancing additives, lubricants, dyes, pigments, flame retardants, impact modifiers, nucleating agents, anti-blocking agents, thermal stabilizers, UV absorbers, UV stabilizers, surfactants, chelating agents, and coupling agents and the like.
- Inorganic fillers include calcium carbonate, titanium dioxide, silica, talc, barium sulfate, carbon black, ceramics, chalk, or mixtures thereof.
- Organic fillers include natural starch, modified starch, chemically modified starch, rice starch, corn starch, wood flour, cellulose, and mixtures thereof.
- Coating methods include embodiments where the blend combination is in the form of an extrusion coating wherein the blend combination is in molten form and lamination methods wherein the blend combination is in the form of a preformed film.
- the coating composition can be applied to one or both sides of the substrate, as well as to the surface of the glass or other rigid substrate.
- Fluorinated-ethylene-propylene (FEP) layers described herein can be disposed on within the adhesive polymeric interlayer (API) such as sheets of an interlayer resin composition.
- API adhesive polymeric interlayer
- Such interlayers can be prepared by conventional melt extrusion or melt molding processes suitable for making interlayers for glass laminates. Such processes are well-known to those of ordinary skill in the relevant art, as exemplified by the previously incorporated publications.
- the API can be monolayer or multilayer sheets.
- multilayer sheets can be formed having a functional core layer sandwiched between two exterior layers and other optional interior layers.
- at least one (or both) of the exterior layers of the multilayer interlayer is a sheet of the resin composition in accordance with the present invention.
- an acoustic damping layer such as a polystyrene copolymer intermediate film (see JP2007-91491 A), a polyvinyl acetal layer (see US Published Patent Application No. 2013/0183507, US Patent No. 8741439, JP Published Patent Application No. 2012-214305A and US Patent No. 8883317), a viscoelastic acrylic layer (see US Patent No. 7121380), a layer containing a copolymer of styrene and a rubber-based resin monomer (see JP Published Patent Application No. 2009-256128A), a layer containing a polyolefin (see US Published Patent Application No.
- the intermediate layer is thermoplastic elastomer resin, such as disclosed in International Patent Application Nos. WO 2016/076336A1, WO 2016/076337A1, WO 2016/076338A1 WO 2016/076339A1 and WO 2016/076340 Al, as well as United States Patent Application No. 15/588986 (filed 8 May 2017).
- the thermoplastic elastomer resin is a hydrogenated product of a block copolymer having: (i) an aromatic vinyl polymer block (a) containing about 60 mol% or more of an aromatic vinyl monomer unit, based on the aromatic vinyl polymer block, and
- the interlayer as a whole can be symmetric having a substantially consistent thickness, or can be asymmetric wherein a portion of the interlayer has a thickness greater than another portion (for example, partial or full “wedge”, as discussed in United States Patent Application No. 15/588986 (filed 8 May 2017) and United States Provisional Application No. 62/414015 (filed 28 October 2016)).
- the laminate can be substantially clear or having coloring in all or a portion (for example, “shadeband” as discussed in United States Patent Application No. 15/588986 (filed 8 May 2017) and United States Provisional Application No. 62/414015 (filed 28 October 2016)).
- the thinner portion of the interlayer should possess the thicknesses of a symmetric construction, while the thickness of the thick portion will depend on various parameters such as wedge angle.
- the thicker edge has a thickness of about 1850 pm or less, or about 1600 pm or less, or about 1520 pm or less, or about 1330 pm or less, or about 1140 pm or less; and the thinner edge has a thickness of about 600 pm or more, or about 700 pm or more, or about 760 pm or more.
- a concave and convex structure such as an embossing
- an embossing can be formed on the surface of the interlayer of the present invention by conventionally known methods for assistance in deairing in laminate production.
- the shape of the embossing is not particularly limited, and those which are conventionally known can be adopted.
- At least one surface (and preferably both surfaces) of the interlayer for a laminated glass is shaped.
- an air bubble present at an interface between the interlayer for a laminated glass and a glass easily escapes to the outside of the laminated glass, and thus, the appearance of the laminated glass can be made favorable.
- An embossing roll to be used in the embossing roll method can be produced, for example, by using an engraving mill (mother mill) having a desired concave-convex pattern and transferring the concave-convex pattern to the surface of a metal roll. Further, an embossing roll can also be produced using laser etching. Further, after forming a fine concave-convex pattern on the surface of a metal roll as described above, the surface with the fine concave-convex pattern is subjected to a blast treatment using an abrasive material such as aluminum oxide, silicon oxide, or glass beads, whereby a finer concave-convex pattern can also be formed.
- the embossing roll to be used in the embossing roll method is preferably subjected to a release treatment.
- a release treatment In the case where an embossing roll which is not subjected to a release treatment is used, it becomes difficult to release the interlayer for a laminated glass from the embossing roll.
- Examples of a method for the release treatment include known methods such as a silicone treatment, a Teflon (registered trademark) treatment, and a plasma treatment.
- the depth of the concave portion and/or the height of the convex portion (hereinafter sometimes referred to as “the height of the embossed portion”) of the surface of the interlayer for a laminated glass shaped by an embossing roll method or the like are/is typically about 5 pm or more, or about 10 pm or more, or about 20 pm or more.
- the height of the embossed portion is typically about 150 pm or less, or about 100 pm or less, or about 80 pm or less.
- the height of the embossed portion refers to a maximum height roughness (Rz) defined in JIS B 0601 (2001).
- the height of the embossed portion can be measured by, for example, utilizing the confocal principle of a laser microscope or the like.
- the height of the embossed portion that is, the depth of the concave portion or the height of the convex portion may vary within a range that does not depart from the gist of the invention.
- Examples of the form of the shape imparted by an embossing roll method or the like include a lattice, an oblique lattice, an oblique ellipse, an ellipse, an oblique groove, and a groove.
- the inclination angle of such form is typically from about 10° to about 80° with respect to the film flow direction (MD direction).
- the shaping pattern may be a regular pattern or an irregular pattern such as a random matte pattern, or a pattern such as disclosed in US Patent No. 7351468.
- the shaping by an embossing roll method or the like may be performed on one surface of the interlayer for a laminated glass, or may be performed on both surfaces, but is more typically performed on both surfaces.
- a fluorinated-ethylene-propylene (FEP) layer is present within the API in the 10% depth of the API, as discussed previously.
- FEP fluorinated-ethylene-propylene
- a method can be used in which, after temporary contact bonding, the resultant laminate is put into an autoclave for final bonding. Further description of these methods can be found in, for example, US Patent No. 7642307.
- a vacuum laminator for example, a known instrument which is used for production of a solar cell can be used, and the assembly is laminated under a reduced pressure of about 1 x 10' 6 MPa or more and about 3 x 10' 2 MPa or less at a temperature of about 100°C or higher, or about 130°C or higher, and about 200°C or lower, or about 170°C or lower.
- the method of using a vacuum bag or a vacuum ring is, for example, described in EP Published Patent Application No. 1235683A1 (CA Published Patent Application No. 2388107A1) and, for example, the assembly is laminated under a pressure of about 2 x 10' 2 MPa at about 130°C or higher and about 145°C or lower.
- the autoclave process which is supplementarily conducted after the temporary contact bonding is variable depending upon the thickness or constitution of a module, it is, for example, carried out under a pressure of about 1 MPa or more and about 15 MPa or less at a temperature of about 120°C or higher and about 160°C or lower for about 0.5 hours or more and about 2 hours or less.
- the glass to be used for preparing a laminated glass is not particularly limited.
- Inorganic glasses such as a float sheet glass, a polished sheet glass, a figured glass, a wired sheet glass, a heat-ray absorbing glass, and conventionally known organic glasses, such as polymethyl methacrylate and polycarbonate, and the like can be used. These glasses may be any of colorless, colored, transparent, or non-transparent glasses. These glasses may be used solely, or may be used in combination of two or more thereof.
- the laminated glass of the present invention can be suitably used for a windshield for automobile, a side glass for automobile, a sunroof for automobile, a rear glass for automobile, or a glass for head-up display; a building member for a window, a wall, a roof, a sunroof, a sound insulating wall, a display window, a balcony, a handrail wall, or the like; a partition glass member of a conference room; a solar panel; and the like. Further information on such uses can be found by reference to the previously incorporated publication.
- the separation between two debonding zones is clearly demarcated. Stated another way, the difference in peel strength is sufficiently drastic to show a difference. In another embodiment, the difference between two zones is more diffuse. In one embodiment, there is a spatial distance between two debonding zones of at least about 0.01 mm; or about 0.1 mm; or about 1.0 mm; or about 2.0 mm; or about 3.0 mm; or about 4.0 mm; or about 5.0 mm; or about 10.0 mm; or about 25.0 mm; or about 50.0 mm; or about 100.0 mm.
- the debonding zones’ peel strengths are engendered by using different polymer or the same polymer to form the API layer.
- the present invention envisages the scenario where the molecular weight of the polymer is used to generate the debonding zones.
- the thickness of the interfacial zone is used to generate the debonding zones.
- external treatment of the interfacial zone is used to generate the debonding zones.
- the debonding zones are generated by treatment of the adhesive polymeric adhesive and/or the laminate glass adhering to the API layer.
- the debonding treatment can include the application of a chemically active substance or mixture which can alter the adhesive/debonding characteristics at or near the interface between the rigid substrate and the API layer.
- a treatment can alternatively include the application of an energetic ‘beam’, such as electron beam, gamma, plasma, electron discharge, laser, ion-beam or other energetic means such as, plasma, flame-treatment, UV/VIS/IR radiation, microwaves or chemical alteration, via, coating techniques, chemical vapor deposition, and the like.
- an energetic ‘beam’ such as electron beam, gamma, plasma, electron discharge, laser, ion-beam or other energetic means such as, plasma, flame-treatment, UV/VIS/IR radiation, microwaves or chemical alteration, via, coating techniques, chemical vapor deposition, and the like.
- Combinations of a chemical substance ⁇ ) with energetic sources can also be employed as a treatment.
- the treatment may be of an infinitesimally small dimension (i.e., only surface atomic or molecular monolayer affected by the treatment or the treatment may be of a finite thickness (approaching up to 10% of the interlayer thickness.
- the treatment may be applied to either the rigid substrate or to the polymeric interlayer or
- the invention provides a interfacial region layer comprising at least two zones, wherein the zone with maximum mean peel strength has a mean peel strength that is at least about 2 times greater than a mean peel strength of the zone with minimum mean peel strength; or about 3 times greater than a mean peel strength of the zone with minimum mean peel strength; or about 4 times greater than a mean peel strength of the zone with minimum mean peel strength; or about 5 times greater than a mean peel strength of the zone with minimum mean peel strength; or about 6 times greater than a mean peel strength of the zone with minimum mean peel strength; or about 7 times greater than a mean peel strength of the zone with minimum mean peel strength; or about 8 times greater than a mean peel strength of the zone with minimum mean peel strength; or about 9 times greater than a mean peel strength of the zone with minimum mean peel strength.
- the invention provides an interfacial region comprising at least two zones, wherein the zone with maximum mean peel strength has a mean peel strength that is at least about 10 times greater than a mean peel strength of the zone with minimum mean peel strength; or wherein the zone with maximum mean peel strength has a mean peel strength that is at least about 15 times greater than a mean peel strength of the zone with minimum mean peel strength; or wherein the zone with maximum mean peel strength has a mean peel strength that is at least about 20 times greater than a mean peel strength of the zone with minimum mean peel strength; or wherein the zone with maximum mean peel strength has a mean peel strength that is at least about 25 times greater than a mean peel strength of the zone with minimum mean peel strength; or wherein the zone with maximum mean peel strength has a mean peel strength that is at least about 30 times greater than a mean peel strength of the zone with minimum mean peel strength; or wherein the maximum mean peel strength is at least about 35 times greater than the minimum mean peel strength; or wherein the maximum mean peel strength is at least about 40 times greater
- the maximum mean peel strength is at least about 10 times greater than the minimum mean peel strength. In an embodiment, the maximum mean peel strength is at least about 20 times greater than the minimum mean peel strength. In an embodiment, the maximum mean peel strength is at least about 30 times greater than the minimum mean peel strength. In an embodiment, the maximum mean peel strength is at least about 40 times greater than the minimum mean peel strength. In an embodiment, the maximum mean peel strength is at least about 50 times greater than the minimum mean peel strength. In an embodiment, the maximum mean peel strength is at least about 60 times greater than the minimum mean peel strength. In an embodiment, the maximum mean peel strength is at least about 70 times greater than the minimum mean peel strength. In an embodiment, the maximum mean peel strength is at least about 80 times greater than the minimum mean peel strength.
- the maximum mean peel strength is at least about 90 times greater than the minimum mean peel strength. In an embodiment, the maximum mean peel strength is at least about 100 times greater than the minimum mean peel strength. In an embodiment, the maximum mean peel strength is at least about 110 times greater than the minimum mean peel strength. In an embodiment, the maximum mean peel strength is at least about 120 times greater than the minimum mean peel strength. In an embodiment, the maximum mean peel strength is at least about 130 times greater than the minimum mean peel strength. In an embodiment, the maximum mean peel strength is at least about 140 times greater than the minimum mean peel strength. In an embodiment, the maximum mean peel strength is at least about 150 times greater than the minimum mean peel strength. In an embodiment, the maximum mean peel strength is at least about 160 times greater than the minimum mean peel strength.
- the maximum mean peel strength is at least about 170 times greater than the minimum mean peel strength. In an embodiment, the maximum mean peel strength is at least about 180 times greater than the minimum mean peel strength. In an embodiment, the maximum mean peel strength is at least about 190 times greater than the minimum mean peel strength. In an embodiment, the maximum mean peel strength is at least about 200 times greater than the minimum mean peel strength. In an embodiment, the maximum mean peel strength is at least about 210 times greater than the minimum mean peel strength. In an embodiment, the maximum mean peel strength is at least about 220 times greater than the minimum mean peel strength. In an embodiment, the maximum mean peel strength is at least about 230 times greater than the minimum mean peel strength. In an embodiment, the maximum mean peel strength is at least about 240 times greater than the minimum mean peel strength. In an embodiment, the maximum mean peel strength is at least about 250 times greater than the minimum mean peel strength.
- the invention provides an interfacial region comprising at least two zones, wherein the zone with maximum mean peel strength has a mean peel strength that is from about 2 times to about 250 times greater than a mean peel strength of the zone with minimum mean peel strength; or wherein the maximum mean peel strength is from about 3 times to about 225 times greater than the minimum mean peel strength; or wherein or wherein the maximum mean peel strength is from about 4 times to about 200 times greater than the minimum mean peel strength; or wherein the maximum mean peel strength is from about 5 times to about 175 times greater than the minimum mean peel strength; or wherein the maximum mean peel strength is from about 5 times to about 150 times greater than the minimum mean peel strength; or wherein or wherein the maximum mean peel strength is from about 5 times to about 125 times greater than the minimum mean peel strength; or wherein the maximum mean peel strength is from about 5 times to about 100 times greater than the minimum mean peel strength; or wherein the maximum mean peel strength is from about 10 times to about 95 times greater than the minimum mean peel strength; or wherein the maximum mean mean
- the invention provides an interfacial region comprising at least two zones, wherein the zone with maximum mean peel strength has a mean peel strength that is from about 2 times to about 5 times greater than a mean peel strength of the zone with minimum mean peel strength; or wherein the maximum mean peel strength is from about 5 times to about 10 times greater than the minimum mean peel strength; or wherein the maximum mean peel strength is from about 10 times to about 15 times greater than the minimum mean peel strength; or wherein the maximum mean peel strength is from about 15 times to about 20 times greater than the minimum mean peel strength; or wherein the maximum mean peel strength is from about 20 times to about 25 times greater than the minimum mean peel strength; or wherein the maximum mean peel strength is from about 25 times to about 30 times greater than the minimum mean peel strength; or wherein the maximum mean peel strength is from about 30 times to about 35 times greater than the minimum mean peel strength; or wherein the maximum mean peel strength is from about 35 times to about 40 times greater than the minimum mean peel strength; or wherein the maximum mean peel strength is from about 40 times to about
- the highest peel strength is taken as that measured/ob served just prior to initiation of the tearing through the bulk of the peel arm and/or in any significant separation of layers within the peel arm.
- the invention provides an interfacial region comprising at least two zones, wherein at least one of the zones has a mean peel strength of from about 0.01 to about 4.0 kJ/m 2 ; or wherein at least one of the zones has a mean peel strength of from about 0.25 to about
- the invention provides an interfacial region comprising at least two zones, wherein at least one of the zones has a mean peel strength of from about 0.01 to about 0.5 kJ/m 2 ; or wherein at least one of the zones has a mean peel strength of from about 0.5 to about 1.0 kJ/m 2 ; or wherein at least one of the zones has a mean peel strength of from about 1.0 to about 1.5 kJ/m 2 ; or wherein at least one of the zones has a mean peel strength of from about 1.5 to about 2.0 kJ/m 2 ; or wherein at least one of the zones has a mean peel strength of from about 2.0 to about 2.5 kJ/m 2 ; or wherein at least one of the zones has a mean peel strength of from about 2.5 to about 3.0 kJ/m 2 ; or wherein at least one of the zones has a mean peel strength of from about 3.0 to about 3.5 kJ/m 2 ; or wherein at least one of the zones has a mean peel strength of from about 3.0 to
- the invention provides an interfacial region comprising at least two zones, wherein at least one of the zones has a mean peel strength of from about 8.0 to about 12.0 kJ/m 2 ; or wherein at least one of the zones has a mean peel strength of from about 8.5 to about 11.5 kJ/m 2 ; or wherein at least one of the zones has a mean peel strength of from about 9.0 to about 11.0 kJ/m 2 ; or wherein at least one of the zones has a mean peel strength of from about
- the invention provides an interfacial region comprising at least two zones, wherein at least one of the zones has a mean peel strength of from about 8.0 to about 8.5 kJ/m 2 ; or wherein at least one of the zones has a mean peel strength of from about 8.5 to about 9.0 kJ/m 2 ; or wherein at least one of the zones has a mean peel strength of from about 9.0 to about 9.5 kJ/m 2 ; or wherein at least one of the zones has a mean peel strength of from about 10.0 to about 10.5 kJ/m 2 ; or wherein at least one of the zones has a mean peel strength of from about 10.5 to about 11.0 kJ/m 2 ; or wherein at least one of the zones has a mean peel strength of from about 11.0 to about 11.5 kJ/m 2 ; or wherein at least one of the zones has a mean peel strength of from about 11.5 to about 12.0
- the mean peel strength of the zone with the maximum mean peel strength is in the range of from about 0.3 kJ/m 2 to about 12.0 kJ/m 2 .
- the mean peel strength can be any one of the following numbers in kJ/m 2 :
- such mean peel strength is within the range defined by selecting any two numbers above, including the end-points of such range.
- the invention provides a polymeric interlayer comprising at least two zones, wherein the zones are distributed in an ordered pattern. In an embodiment, the zones are distributed in a grid, in concentric circles or in a dot pattern. In another embodiment, the invention provides a polymeric interlayer comprising at least two zones, wherein the zones are distributed stochastically.
- the invention provides a debonding region comprising at least two zones, wherein at least one of the zones comprises a polyvinyl acetal, an ionomer, a thermoplastic elastomer, a silane, an ethylvinylacetate, or combinations thereof.
- at least one of the zones comprises a polyvinyl acetal.
- at least one of the zones comprises an ionomer.
- at least one of the zones comprises a thermoplastic elastomer.
- at least one of the zones comprises a silane.
- at least one of the zones comprises an ethylvinylacetate.
- the invention provides a debonding region comprising at least two zones, wherein the zones each comprise a polyvinyl acetal, an ionomer, a thermoplastic elastomer, a silane, an ethylvinylacetate, or combinations thereof.
- the zones each comprises a polyvinyl acetal.
- both of the zones comprise an ionomer.
- the zones each comprise a thermoplastic elastomer.
- the zones each comprise a silane.
- the zones each comprise an ethylvinylacetate.
- the zones each comprise a combination of these materials.
- the invention provides a debonding region comprising at least two zones, wherein at least one of the zones comprises the ionomer and the ionomer is a sodium- neutralized ethylene-a,P-unsaturated carboxylic acid copolymer.
- the invention provides a polymeric interlayer comprising at least two zones, wherein the zones each comprise the ionomer and the ionomer is a sodium-neutralized ethylene-a,P-unsaturated carboxylic acid copolymer.
- the invention provides a debonding region comprising at least two zones, wherein at least one of the zones comprises the polyvinyl acetal and the polyvinyl acetal is a polyvinyl butyral.
- the invention provides a fluorinated-ethylene-pro- pylene (FEP) layer comprising at least two zones, wherein the zones each comprise the polyvinyl acetal and the polyvinyl acetal is a polyvinyl butyral.
- FEP fluorinated-ethylene-pro- pylene
- the invention provides a polymeric interlayer comprising at least two zones, wherein at least one of the zones further comprises an adhesion modifying agent.
- the adhesion modifying agent is a silane, an alkali metal salt, an alkaline earth metal salt or a carboxylic group-containing olefinic polymer.
- the adhesion modifying agent is a silane.
- the adhesion modifying agent is an alkali metal salt.
- the adhesion modifying agent is an alkaline earth metal salt.
- the adhesion modifying agent is a carboxylic group-containing olefinic polymer.
- the invention provides a polymeric interlayer comprising at least two zones, wherein at least one of the zones comprises the adhesion modifying agent in a range of from about 5% to about 25% by weight of combined weight in the zone. In another embodiment, the invention provides a polymeric interlayer comprising at least two zones, wherein at least one of the zones comprises the adhesion modifying agent in a range of from about 10% to about 20% by weight of combined weight in the zone.
- the invention provides, wherein at least one of the zones comprises the adhesion modifying agent in a range of from about 5% to about 10% by weight of combined weight in the zone; or wherein at least one of the zones comprises the adhesion modifying agent in a range of from about 10% to about 15% by weight of combined weight in the zone; or wherein at least one of the zones comprises the adhesion modifying agent in a range of from about 15% to about 20% by weight of combined weight in the zone; or wherein at least one of the zones comprises the adhesion modifying agent in a range of from about 20% to about 25% by weight of combined weight in the zone.
- the invention provides a polymeric interlayer comprising at least two zones, wherein at least one of the zones comprises the adhesion modifying agent in a range of from about 50% to about 75% by weight of combined weight in the zone. In another embodiment, the invention provides a polymeric interlayer comprising at least two zones, wherein at least one of the zones comprises the adhesion modifying agent in a range of from about 60% to about 70% by weight of combined weight in the zone.
- the invention provides a polymeric interlayer comprising at least two zones, wherein at least one of the zones comprises the adhesion modifying agent in a range of from about 50% to about 55% by weight of combined weight in the zone; or wherein the adhesion modifying agent is present in a range of from about 55% to about 60% by weight of combined weight in the zone; or wherein the adhesion modifying agent is present in a range of from about 65% to about 70% by weight of combined weight in the zone; or wherein the adhesion modifying agent is present in a range of from about 70% to about 75% by weight of combined weight in the zone.
- the invention provides a polymeric interlayer comprising at least two zones, wherein the interlayer has a thickness of from about 0.1 mm to about 10.0 mm; or wherein the interlayer has a thickness of from about 0.25 mm to about 7.5 mm; or wherein the interlayer has a thickness of from about 0.35 mm to about 5.0 mm; or wherein the interlayer has a thickness of from about 0.5 mm to about 2.5 mm.
- the invention provides a polymeric interlayer comprising at least two zones, wherein the interlayer has a thickness of from about 0.1 mm to about 1.0 mm; or wherein the interlayer has a thickness of from about 1.0 mm to about 2.0 mm; or wherein the interlayer has a thickness of from about 2.0 mm to about 3.0 mm; or wherein the interlayer has a thickness of from about 3.0 mm to about 4.0 mm; or wherein the interlayer has a thickness of from about 4.0 mm to about 5.0 mm; or wherein the interlayer has a thickness of from about 5.0 mm to about 6.0 mm; or wherein the interlayer has a thickness of from about 6.0 mm to about 7.0 mm; or wherein the interlayer has a thickness of from about 7.0 mm to about 8.0 mm; or wherein the interlayer has a thickness of from about 8.0 mm to about 9.0 mm; or wherein the interlayer has a thickness of from about 9.0 mm;
- the invention provides a polymeric interlayer comprising at least two zones, wherein the interlayer is disposed between two panes of glass.
- at least one of the glass panes is float glass.
- both of the glass panes are float glass.
- the interlayer is in contact with the tin side of the float glass.
- the invention provides a debonding region comprising at least two zones, wherein the fluorinated-ethylene-propylene (FEP) layer has a thickness of from about 0.001 mm to about 1.0 mm; or wherein the fluorinated-ethylene-propylene (FEP) layer has a thickness of from about 0.01 mm to about 0.5 mm; or wherein the fluorinated-ethylene-propylene (FEP) layer has a thickness of from about 0.15 mm to about 0.2 mm.
- FEP fluorinated-ethylene-propylene
- the invention provides a debonding region comprising at least two zones, wherein the Debonding region has a thickness of from about 0.001 mm to about 1.0 mm; or wherein the debonding region has a thickness of from about 0.01 mm to about 0.5 mm; or wherein the debonding region has a thickness of from about 0.15 mm to about 0.25 mm.
- the invention provides a debonding region comprising at least two zones, wherein the debonding region is disposed between two panes of glass.
- at least one of the glass panes is float glass.
- both of the glass panes are float glass.
- the debonding region is in contact with the tin side of the float glass.
- the invention provides a debonding region comprising at least three zones; or wherein the debonding region comprises at least four zones; or wherein the interlayer comprises at least five zones; or wherein the debonding region comprises at least six zones; or wherein the debonding region comprises at least seven zones; or wherein the debonding region comprises at least eight zones; or wherein the debonding region comprises at least nine zones; or wherein the debonding region comprises at least ten zones.
- the invention provides a polymeric interlayer comprising at least two zones, wherein at least one of the zones is shaped as a dot, a circle, a square, a rectangle, a pentagon, a hexagon; or is amorphous.
- the invention provides a polymeric interlayer comprising at least two zones, wherein the zones are each shaped as a dot, a circle, an oval, a triangle, a square, a rectangle, a pentagon, a hexagon; or is amorphous.
- at least one of the zones are shaped as a dot.
- at least one of the zones are shaped as a circle.
- At least one of the zones are shaped as an oval. In an embodiment, at least one of the zones are shaped as a triangle. In an embodiment, at least one of the zones are shaped as a square. In an embodiment, at least one of the zones are shaped as a rectangle. In an embodiment, at least one of the zones are shaped as a pentagon. In an embodiment, at least one of the zones are shaped as a hexagon. In an embodiment, at least one of the zones are amorphous.
- the invention provides a polymeric interlayer comprising at least two zones, wherein at least one of the zones is shaped as gridlines, crisscross lines, random lines, concentric circles, eccentric circles, spaghetti patterns and flat strips.
- the invention provides a polymeric interlayer comprising at least two zones, wherein the zones are each shaped as gridlines, crisscross lines, random lines, concentric circles, eccentric circles, spaghetti patterns and flat strips.
- at least one of the zones are shaped as gridlines.
- at least one of the zones are shaped as crisscross lines.
- at least one of the zones are shaped as random lines.
- At least one of the zones are shaped as concentric circles. In an embodiment, at least one of the zones are shaped as eccentric circles. In an embodiment, at least one of the zones are shaped as a spaghetti pattern. In an embodiment, at least one of the zones are shaped as a flat strip.
- the invention provides a polymeric interlayer comprising at least two zones, wherein the zones have a size in a range of from about 0.5 times a thickness of the interlayer to about 10 times the thickness of the interlayer; or wherein the zones have a size in a range of from about 1.5 times the thickness to about 9.0 times the thickness of the interlayer; or wherein the zones have a size in a range of from about 2.0 times the thickness to about 8.0 times the thickness of the interlayer; or wherein the zones have a size in a range of from about 3.0 times the thickness to about 7.0 times the thickness of the interlayer; or wherein the zones have a size in a range of from about 4.0 times the thickness to about 6.0 times the thickness of the interlayer; or wherein the zones have a size in a range of from about 4.5 times the thickness to about 5.5 times the thickness of the interlayer; or wherein the zones have a size that is about 5.0 times the thickness to of the interlayer.
- the invention provides a polymeric interlayer comprising at least two zones, wherein the zones have a size in a range of from about 0.5 times a thickness of the interlayer to about 1.5 times the thickness of the interlayer; or wherein the zones have a size in a range of from about 1.5 times the thickness to about 2.0 times the thickness of the interlayer; or wherein the zones have a size in a range of from about 2.0 times the thickness to about 3.0 times the thickness of the interlayer; or wherein the zones have a size in a range of from about 3.0 times the thickness to about 4.0 times the thickness of the interlayer; or wherein the zones have a size in a range of from about 4.0 times the thickness to about 5.0 times the thickness of the interlayer; or wherein the zones have a size in a range of from about 5.0 times the thickness to about 6.0 times the thickness of the interlayer; or wherein the zones have a size in a range of from about 5.0 times the thickness to about 6.0 times the thickness of the interlayer; or wherein the zones have
- the invention provides a polymeric interlayer comprising at least two zones, wherein the zones are shaped as a dot or circle having a diameter in the range of from about 0.5 times a thickness of the interlayer to about 10 times the thickness of the interlayer; or wherein the zones are shaped as a dot or circle having a diameter in the range of from about 1.5 times the thickness to about 9.0 times the thickness of the interlayer; or wherein the zones are shaped as a dot or circle having a diameter in the range of from about 2.0 times the thickness to about 8.0 times the thickness of the interlayer; or wherein the zones are shaped as a dot or circle having a diameter in the range of from about 3.0 times the thickness to about 7.0 times the thickness of the interlayer; or wherein the zones are shaped as a dot or circle having a diameter in the range of from about 4.0 times the thickness to about 6.0 times the thickness of the interlayer; or wherein the zones are shaped as a dot or circle having a diameter in the range of from about 4.0
- the invention provides a polymeric interlayer comprising at least two zones, wherein the zones are shaped as a dot or circle having a diameter in the range of from about 0.5 times a thickness of the interlayer to about 1.5 times the thickness of the interlayer; or wherein the zones are shaped as a dot or circle having a diameter in the range of from about 1.5 times the thickness to about 2.0 times the thickness of the interlayer; or wherein the zones are shaped as a dot or circle having a diameter in the range of from about 2.0 times the thickness to about 3.0 times the thickness of the interlayer; or wherein the zones are shaped as a dot or circle having a diameter in the range of from about 3.0 times the thickness to about 4.0 times the thickness of the interlayer; or wherein the zones are shaped as a dot or circle having a diameter in the range of from about 4.0 times the thickness to about 5.0 times the thickness of the interlayer; or wherein the zones are shaped as a dot or circle having a
- this invention relates to an adhesive polymeric interlayer (API) as described above, wherein an effective diameter of the discrete zone is in a range of from about 0.1 mm to about 50 mm.
- API adhesive polymeric interlayer
- the invention provides an API wherein an effective diameter of the discrete zone selected from one of the following numbers or is in a range defined by any two numbers including the endpoints of such range, as measured in mm:
- this invention relates to an adhesive polymeric interlayer (API) as described above, wherein the effective diameter of the regular shaped discrete zone, the random shaped discrete zone, or the cluster discrete zone is from about 1 multiple to about 150,000,000-multiples of the thickness of the discrete zone.
- An exemplary set of multiples includes the following numbers, those included within a range formed by any two numbers below:
- the invention provides an interlayer that comprises discrete debonding treated zones that have a surface area on one side that is a percentage number of the area of the substrate or the API surface where the percentage number is one of the following numbers, or is within a range defined by any two of the following numbers, including the endpoints of such range:
- the invention provides polymeric interlayer comprising at least two zones, wherein at least one of the zones covers a surface area of from about 10% to about 100% of one of the glass panes: [0320] 10, 11 ,12 13, 14, 15, 16, 17, 18, 19, 20, 21, 22, 23, 24, 25, 26, 27, 28, 29, 30, 31, 32, 33,
- the invention relates to a polymeric interlayer comprising at least two zones, wherein at least one of the zones covers a surface area of one of the glass panes, which is within a range defined by any two numbers above, in the units of percent surface area covered, including the endpoints of such a range.
- the invention provides a polymeric interlayer comprising at least two zones, wherein one of the zones covers a surface area of from about 10% to about 100% of one of the glass panes; or wherein one of the zones covers a surface area of from about 15% to about 55% of one of the glass panes; or wherein one of the zones covers a surface area of from about 20% to about 50% of one of the glass panes; or wherein one of the zones covers a surface area of from about 25% to about 45% of one of the glass panes; or wherein one of the zones covers a surface area of from about 30% to about 40% of one of the glass panes.
- the invention provides a polymeric interlayer comprising at least two zones, wherein one of the zones covers a surface area of from about 10% to about 15% of one of the glass panes; or wherein one of the zones covers a surface area of from about 15% to about 20% of one of the glass panes; or wherein one of the zones covers a surface area of from about 20% to about 25% of one of the glass panes; or wherein one of the zones covers a surface area of from about 25% to about 30% of one of the glass panes; or wherein one of the zones covers a surface area of from about 30% to about 35% of one of the glass panes; or wherein one of the zones covers a surface area of from about 35% to about 40% of one of the glass panes; or wherein one of the zones covers a surface area of from about 40% to about 45% of one of the glass panes; or wherein one of the zones covers a surface area of from about 45% to about 50% of one of the glass panes; or
- the invention provides a polymeric interlayer comprising at least two zones, wherein one of the zones covers a surface area of from about 1% to about 35% of one of the glass panes; or wherein one of the zones covers a surface area of from about 5% to about 30% of one of the glass panes; or wherein one of the zones covers a surface area of from about 5% to about 25% of one of the glass panes; or wherein one of the zones covers a surface area of from about 10% to about 20% of one of the glass panes.
- the invention provides a polymeric interlayer comprising at least two zones, wherein one of the zones covers a surface area of from about 1% to about 5% of one of the glass panes; or wherein one of the zones covers a surface area of from about 5% to about 10% of one of the glass panes; or wherein one of the zones covers a surface area of from about 10% to about 15% of one of the glass panes; or wherein one of the zones covers a surface area of from about 15% to about 20% of one of the glass panes; or wherein one of the zones covers a surface area of from about 20% to about 25% of one of the glass panes; or wherein one of the zones covers a surface area of from about 25% to about 30% of one of the glass panes; or wherein one of the zones covers a surface area of from about 30% to about 35% of one of the glass panes.
- the invention provides a polymeric interlayer comprising at least two sets of discrete zones, wherein one set of discrete zones, for example, the controlled debonding treatment zones covers a surface area of: from about 1% to about 80% of the surface areas of one of the glass substrate; from about 10% to about 60% of one of the glass panes; from about 20% to about 50% of one of the glass substrate; from about 30% to about 40% of the surface areas of one of the glass substrate; from about 5% to about 25% of the surface areas of one of the glass substrate; from about 1% to about 35% of the surface areas of one of the glass substrate; from about 15% to about 55% of one of the glass panes; from about 25% to about 45% of one of the glass panes; from about 10% to about 15% of one of the glass panes; from about 15% to about 20% of one of the glass panes; from about 20% to about 25% of one of the glass panes; from about 25% to about 30% of one of the glass panes; from about 30% to about
- this invention envisions the same area coverage or a different area coverage between a first glass substrate and the corresponding API surface and a second glass substrate and the corresponding API surface, for example in a glass substrate 1/API/glass substrate 2 laminate.
- this invention also envisions stacks of laminates. So, for example if glass substrate was designated as “A” and the API was designated as “B”, the following laminates are envisioned herein:
- At least one of the API layers in such a stack of the invention comprises the discrete zones as described herein.
- an Ao means the substrate is not present in that arrangement at that spot in a stack.
- this invention envisions another protective layer—abrasion-resistance coated polyester for example. While this invention has been described with a focus on a rigid substrate (e.g. glass), in some cases a coated polyester, polycarbonate, nylon, and other polymeric substrates are also included.
- a rigid substrate e.g. glass
- a coated polyester, polycarbonate, nylon, and other polymeric substrates are also included.
- thinner interlayers are plied together to make a thicker interlayer.
- the invention provides a polymeric interlayer comprising at least three zones; or wherein the interlayer comprises at least four zones; or wherein the interlayer comprises at least five zones; or wherein the interlayer comprises at least six zones; or wherein the interlayer comprises at least seven zones; or wherein the interlayer comprises at least eight zones; or wherein the interlayer comprises at least nine zones; or wherein the interlayer comprises at least ten zones.
- the invention provides a polymeric interlayer comprising the number of zones per cm 2 in the range 0.04 to 10,000 including the endpoints of the range.
- the number of zones per cm 2 include any one of the following numbers and any number within a range defined by any two numbers below, including the endpoints:
- the number of zones described above are measured per cm 2 , per inch 2 , per ft 2 , and per m 2 .
- the invention provides a polymeric interlayer comprising three zones; or wherein the interlayer comprises at least four zones; or wherein the interlayer comprises at least five zones; or wherein the interlayer comprises at least six zones; or wherein the interlayer comprises at least seven zones; or wherein the interlayer comprises at least eight zones; or wherein the interlayer comprises at least nine zones; or wherein the interlayer comprises at least ten zones.
- the invention provides a laminate comprising the polymeric interlayer described herein.
- the laminate comprises wood, plastic, or glass.
- the laminate comprises wood.
- the laminate comprises plastic.
- the laminate comprises glass.
- the glass used in the Examples was soda-lime glass, standard annealed (obtained from Guardian Industries, Inc., Galax VA, USA).
- the adhesion promotion used was gamma-aminopropyltri ethoxy silane (Silquest A-l 100, available from Momentive Performance Materials, Inc., Waterford, NY USA).
- Fluorinated-ethylene-propylene (FEP) films (DuPont Teflon® FEP-50) used was 13 microns in thickness and purchased from American Durafilm Co, Inc., 55 Boynton Rd, Holliston MA 01746.
- laminate breakage behavior and glass-polymer adhesion during breakage have been studied on laminates fabricated from annealed float glass and an ionomer interlayer sold by Kuraray America, Inc. (Wilmington, DE, USA) under the trademark “SENTRYGLAS®.”
- Discrete cohesive debonding zones were created by embedding fluorinated-ethylene-pro- pylene (FEP) films into the ionomer.
- FEP fluorinated-ethylene-pro- pylene
- the FEP film DuPont Teflon® FEP-50 used was 13 microns in thickness and purchased from American Durafilm Co, Inc., 55 Boynton Rd, Holliston MA 01746. Holes of either 2 mm diameter or 5 mm diameter were cut into some FEP films on a 10 mm x 10 mm uniform square grid pattern using a laser-cutter (BOSSLASER, Model LS-1416 608 Trestle Point, Sanford FL 32771). In all examples, the FEP films were positioned to be within the top 10 % of the ionomer interlayer (i.e. close to the glass-ionomer interface).
- the glass used in the Examples was soda-lime glass; standard annealed (obtained from Guardian Industries, Inc., Galax VA, USA).
- Float glass is manufactured by floating the molten soda-lime-silica melt on a bath of molten metallic tin.
- the glass “tin” side is the glass that contacted the molten tin during manufacture and the glass “air” side is the opposite side that did not come into contact with the molten tin.
- Trace tin (Sn) impurities in the glass “tin” surface influence polymer-glass adhesion.
- Float glass is available from Guardian Industries, Inc., Galax VA, USA.
- Adhesion promoter was applied to the glass surface to increase glass-ionomer adhesion.
- the active ingredient in the adhesion promotion treatment is gamma-aminopropyltriethoxysilane (Silquest A-l 100, available from Momentive Performance Materials, Inc., Waterford, NY USA).
- a solution of the following composition (weight %) was used: 2-propanol (92.00 %), water (7.90 %), acetic acid (0.01%), gamma-aminopropyltriethoxysilane (0.09%).
- Laminate Fabrication A pre-press assembly, in which the ionomer films, FEP films and glass were stacked in the desired order at room temperature, was placed into a disposable vacuum bag and held for 60 minutes under a vacuum of 25-30 inches of water to remove any air contained between the layers of the pre-press assembly.
- the pre-press assembly was loaded while still applying a vacuum to the bag into an air autoclave.
- the samples and bags were heated to 135°C under an applied hydrostatic air pressure of 0.7 MPa.
- the vacuum to the bag was removed after reaching 135°C and the laminates were held for 90 minutes in an air autoclave at an applied hydrostatic pressure of 0.7 MPa.
- the samples were then cooled at an approximate rate of 4°C/minute under constant pressure. After approximately 25 minutes of cooling, when the air temperature was less than about 50°C, the excess pressure was vented and the laminate was cooled to room temperature and removed from the autoclave.
- Table 1 shows the layup of the components prior to heating and autoclaving. Wherever the FEP films contained holes, the ionomer flowed during lamination to fill in the holes and create a fully interconnected polymer phases with no remaining voids.
- Laminate Breakage Ball-on-Ring
- a key performance attribute of laminated safety glass is the behavior during and after glass breakage. Specifically, the tear and penetration resistance of a laminate are key to its safety performance. In order to evaluate the laminate breakage properties a ball-on-ring testing protocol was used.
- a typical load-displacement trace is shown in Figure 13.
- the tear energy represents to work done to create a first tear in the polymer interlayer during laminate deformation after first-cracking of each glass ply.
- Adhesion Glass Loss During Ball-on-Ring Testing
- FIG. 8 shows the laminate structure used for establishing the laminate toughness and post-glass breakage durability of laminated glass made with ionomer only. Laminate layup details are given in Table 1 and the sample is designated as CE-1.
- Figure 11 shows the schematic laminate structure used for establishing the laminate toughness and post-glass breakage durability of laminated glass made with SentryGlas® with two embedded continuous, planar FEP layers. Laminate layup details are given in Table 1 and the sample is designated as CC-1.
- Figure 10 shows the schematic laminate structure used for establishing the laminate toughness and post-glass breakage durability of laminated glass made with ionomer with two embedded FEP layers.
- the FEP layers contained circular holes (2 mm diameter) located on a uniform square grid 10 mm x 10 mm.
- Laminate layup details are given in Table 1 and the sample is designated as CD-I.
- Figure 10 shows the schematic laminate structure used for establishing the laminate toughness and post-glass breakage durability of laminated glass made with ionomer with two embedded FEP layers.
- the FEP layers contained circular holes (5 mm diameter) located on a uniform square grid 10 mm x 10 mm. Laminate layup details are given in Table 1 and the sample is designated as CD-2.
- the glass used in the Examples was soda-lime glass, standard annealed (obtained from Guardian Industries, Inc., Galax VA, USA).
- PVA Polyvinyl alcohol, Elvanol® 90-50, CAS Number 9002-89-5, available from Kuraray America, Inc. 2625 Bay Area Blvd. Houston, TX 77058.
- Trosifol® PVB Sheeting available from Kuraray Americas was used as described herein to prepare samples for peel strength testing and impact testing described below.
- Aqueous solutions were prepared for each of the above PVA materials by dissolving into demineralized water under stirring at 80°C and then was allowed to cool to room temperature. Solutions were prepared at either 0.5% or 0.05% from the Elvanol® 90-50 PVA. Solutions containing silane also used Momentive A- 1106 (aqueous solution), this additive was added to make a final 0.5% concentration of silane combined along with the PVA.
- Nominal 0.9-mm ionomer sheeting or 0.76-mm PVB sheeting was then immersed into the respective solutions, held for 5 seconds and then withdrawn and allowed to dry by hanging at ambient temperature and humidity. After one hour, these treated sheets were used to prepare the laminates below, for either impact testing (300-mm squares) or peel test samples as described below.
- Glass laminates were prepared from each of the ionomer sheets and PVA layers by the following method.
- Annealed glass sheets (300x300x3 mm) were washed with a solution of trisodium phosphate (5 g/1) in de-ionized water at 50°C for 5 min, then rinsed thoroughly with de-ionized water and dried.
- Three layers of each respective ionomer sheets (about 0.76 mm thick each) as listed in Table 1 were stacked together and placed between two lites of glass sheet (to yield an interlayer thickness of 2.28 mm).
- the moisture level of the ionomer sheet was kept at or below 0.08% by weight by minimizing contact time to the room environment (about 35% RH).
- the moisture level of the ionomer sheet was measured using a coulometric Karl Fischer method (Metrohm Model 800) with a heating chamber temperature of 150°C for the sample vials.
- the ionomer sheeting was cut into small pieces to fit into the sample vials weighing a total of 0.40 grams.
- the pre-lamination assembly was then taped together with a piece of polyester tape in a couple locations to maintain relative positioning of each layer with the glass lites.
- a nylon fabric strip was placed around the periphery of the assembly to facilitate air removal from within the layers.
- the assembly was placed inside a nylon vacuum bag, sealed and then a connection was made to a vacuum pump.
- a vacuum was applied to allow substantial removal of air from within (air pressure inside the bag was reduced to below 50 millibar absolute).
- the bagged assembly was then heated in a convection air oven to 120°C and held for 30 min.
- a cooling fan was then used to cool the assembly down to near room temperature and the assembly was disconnected from the vacuum source and the bag removed yielding a fully pre-pressed assembly of glass and interlayer.
- the assembly was then placed into an air autoclave and the temperature and pressure were increased from ambient to 135°C at 13.8 bar over 15 min. This temperature and pressure was held for 30 min and then the temperature was decreased to 40°C at a cooling of about 2.5°C/min whereby the pressure was then dropped back to ambient (over 15 min) and the final laminates were removed from the autoclave.
- Float glass is manufactured by floating the molten soda-lime-silica melt on a bath of molten metallic tin.
- the glass “tin” side is the glass that contacted the molten tin during manufacture and the glass “air” side is the opposite side that did not come into contact with the molten tin.
- Trace tin (Sn) impurities in the glass “tin” surface influence polymer-glass adhesion.
- Float glass is available from Guardian Industries, Inc., Galax VA, USA.
- All glass was washed prior to fabrication of the laminates using soapy de-ionized water at 50°C and rinsed thoroughly using de-ionized water. Generally, to produce soapy water, soap or detergent is added to water in an amount to form a lather when mixed.
- Laminate Fabrication a pre-press assembly, in which the PVA layer, rigid substrate polymer interlayer and glass were stacked in the desired order at room temperature, was placed into a disposable vacuum bag and held for 60 minutes under a vacuum of 25-30 inches of water to remove any air contained between the layers of the pre-press assembly.
- the pre-press assembly was loaded while still applying a vacuum to the bag into an air autoclave.
- the samples and bags were heated to 135°C under an applied hydrostatic air pressure of 0.7 MPa.
- the vacuum to the bag was removed after reaching 135°C and the laminates were held for 90 minutes in an air autoclave at an applied hydrostatic pressure of 0.7 MPa.
- the samples were then cooled at an approximate rate of 4°C/minute under constant pressure. After approximately 25 minutes of cooling, when the air temperature was less than about 50°C, the excess pressure was vented and the laminate was cooled to room temperature and removed from the autoclave.
- Adhesion is a key requirement for laminated glass.
- a standard peel test method was used to characterize adhesion in the samples described.
- Laminates were prepared for adhesion tests following the approaches described with two important modifications.
- a 25.4 mm wide strip of a thin polyester release tape (25 mm x 25 mm) was applied to one edge of one piece of glass prior to assembly of the glass and polymer components. This tape only lightly adheres to the glass and enables a strip of polymer to be gripped by the peel -testing fixture.
- a thin release film (Teflon® 13 mm) was placed between the polymer and one of the glass pieces. This allows the removal of one piece of glass so that a strip of polymer can be peeled off one of the glass pieces.
- a 40 mm wide strip of polymer was separated from the adjacent polymer by cutting two channels using a sharp knife. Care was taken to make sure the channels were deep enough to fully cut through the polymer and detach it from adjacent material.
- a peel configuration of 90 degrees was used and run with an extension rate of 0.18 mm/s at 23°C and 50 % RH.
- An MTS Criterion M45 universal testing machine, with a 1 kN load cell operating in displacement control mode was used for the measurements.
- the force-displacement characteristic were recorded at a frequency of 1 Hz.
- Five samples were tested for each adhesion treatment and the peel force was recorded as a function of extension.
- Figure 1 shows a typical peel measurement. With uniform adhesion control methods, a steady-state peel force is attained after an interfacial crack initiates. The peel force demonstrates small fluctuations. The energy to create unit area of interface is defined as the peel strength, /, and for the 90 degree peel geometry is given by:
- P is the peel force and w is the peel arm width. Using units of Newtons and mm, this yields a peel strength in units of kJ/m 2 .
- the mean peel strength has been determined by fitting a horizontal line to the steady-state peel force response.
- a conventional impact test widely used to test the laminates in the safety glazing industry is the five-pound (2.27-kg) steel ball drop test. This test is defined in American National Standard Z26.1-1983 Section 5.26 Penetration Resistance, Test 26. The purpose of this test is to determine whether the glazing material has satisfactory penetration resistance. For automotive windshields, a minimum performance level is set at eight out of ten samples passing a twelve foot (3.66-m) ball drop without the ball penetrating the sample within 5 seconds of the impact. The test method calls for controlling laminate temperature between 77 to 104°F (25 to 40°C).
- the laminates (separated to provide air circulation) were placed in a controlled temperature oven, a minimum of 2 hours prior to impact to equilibrate to 23C +/- 2C. Rather than dropping the five-pound ball (2.27-kg) from 12 feet (3.66-m), a variety of drop heights ranging from 2.44-m to 6.71-m were used to assess the “mean” support height (the height at which it is estimated that 50% of the samples would be penetrated). At each various drop impact height, the length of any tear in the laminate and interlayer was also measured and by testing multiple samples at each drop height (avg. of 3 laminates), the height necessary to create a tear of 2.54-cm and 12.7-cm was also computed.
- Laminates prepared above were then immersed into room temperature demineralized water for 1 hour followed by placing the laminates into a chamber adjusted to -20°C for 16 hours. Laminates were then removed and allowed to warm back to room temperature (23°C +/- 2°C) for 7 hours. The process was repeated for a total of 10 cycles and then the degree of debonding/delamination was observed by visual inspection. Image analysis was performed on the laminates to quantify the extent of the debonding if present. The laminates were thoroughly cleaned using WINDEX glass cleaner (S.C. Johnson & Son, Inc.) and lint-less cloths and were inspected to ensure that they were free of bubbles and other defects which might otherwise interfere with making valid optical measurements.
- WINDEX glass cleaner S.C. Johnson & Son, Inc.
- the laminates were then evaluated by means of a Haze-gard Plus hazemeter (Byk- Gardner) to obtain a measurement of percent haze.
- the measurement of haze followed the practice outlined in American National Standard (ANSI Z26.1-1966) “Safety Code for Safety Glazing Materials for Glazing Motor Vehicles Operating on Land Highways”.
- the Haze-gard Plus hazemeter meets the proper criteria for this standard was used in all forthcoming measurements. Haze standards which are traceable to the National Bureau of Standards (now NIST) were used to ensure that the instrument was well-calibrated and operating properly.
- Annealed glass was scribed, cut into 100 mm x 300 mm rectangular-shaped pieces and then washed per the procedure described earlier.
- Thin polyester tape 25 um thickness x 25 mm width
- silicone adhesive was applied to the glass surface on the ‘side-of-interest’ (air or tin- side) in two parallel strips providing a uniform 25 mm wide bonding area in between. This procedure allows for the creation of a very well-defined bonding area without the need to cut through the polymer layer to create a peel strip as is conventionally performed in standard peel strength methodologies.
- EX1-01 through EX1-30 are all examples utilizing ionomer interlayer (IO-1) and examples EX1-31 through EX1-42 contain plasticized PVB interlayer.
- Examples EX1-01 through EX-05 are control samples with a glass orientation whereby the interlayer is bonded to the air-side of each of the glass lites. This is denoted as a ‘TAAT’ orientation.
- Examples EX1-05 through EX1-08 are similar samples but bonded to the tin-side of each of the glass lites (denoted as ‘ATTA’ glass orientation).
- the adhesion level assigned to each of the laminated glass groupings was based on the data derived from a peel measurement from a surrogate sample possessing the same treatment condition as had been applied to the interlayer contained within the ball-drop laminates and with the interlayer being bonded to the respective side of the glass (air-side or tin-side).
- the ionomer interlayer is known to generally possess higher adhesion to the tin-side of the glass than the air-side (reference available from Kuraray “SentryGlas® Lamination Guide”).
- Example EX1-03 had a tear length of 7.6-cm and EX1-08 had a tear length of 26.5-cm, both impacted from a drop height of 4.88-m.
- Examples EX1-09 through EX1-13 were constructed from an ionomer interlayer which had been dip-coated into a solution of PVA in demineralized water at a concentration of 0.5 wt.%. Notably, none of these samples formed any tears due to the ball impact test, at any of the drop heights tested. Drop height level was increased beyond the previous sample sequences to 6.10-m (EX1-13). Surprisingly, even at this much higher impact energy level, no tear was observed in the impacted laminate. Another performance aspect that was measured for each ball drop sample was the quantity of glass loss that resulted from the impact event. Glass loss beyond a certain level could jeopardize the safety and integrity aspects of the glass laminate.
- EX1-19 through EX1-30 were prepared using a PVA/water solution concentration of 0.05%.
- EX1-19 through EX1-24 were made using ATTA glass orientation and EX1-25 through EX1-30 were made using TAAT glass orientation.
- the adhesion level was found to be higher than the series prepared at 0.5 wt.% PVA concentration. No tears were found in this series, even at the higher impact drop heights, however glass loss was much higher than the PVA/silane sample set.
- the adhesion level found between the airside (0.159-kJ/m A 2) and the tin-side (0.157-kJ/m 2 ) was nominally ‘the same’, and well-within experimental error.
- This behavior is highly advantageous, since the inventive art overcomes the typical factors that create variability that is inherent in conventional glass lamination processes. Many of these factors are well-known, such as, different glass compositions, variety of glass washing techniques, moisture variations in the interlayer, different processing and lamination conditions (e.g. autoclave temperature and cycle time), etc.
- the cohesive treatment has provided a means to supply a composite interlayer whereby the adhesion (as measured by the peel test) is controlled ‘within’ the composite structure and can be designed to be less sensitive or nearly insensitive to the substrate to which it is bonded.
- Examples EX1-31 through EX1-42 were prepared from commercial plasticized PVB sheeting (Trosifol® brand from Kuraray). All laminated glass samples were prepared using TAAT glass orientation. Samples EX1-31 through EX1-34 were controls with drop heights ranging from 1.83-m through 3.66-m. Samples EX1-35 through EX1-38 utilized the same PVB sheeting but were first dipped into a PVA/water solution at 0.5 wt.% PVA concentration. Samples EX1-39 through EX1-42 were prepared by treated by dipping into a PVA/silane/water solution at 0.5 wt.% PVA concentration and 0.2 wt.% of silane.
- Table 3 List of examples with various combinations of continuous treatment.
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Abstract
La présente invention concerne une structure stratifiée comprenant au moins un substrat en verre et une couche intermédiaire polymère adhésive (API) qui comprend des zones de décollement cohésives sensiblement discrètes et/ou sensiblement continues dans leur disposition. Ces zones de décollement sont situées de préférence sur l'épaisseur de 10 % de l'API à partir de l'interface de ladite API et du substrat en verre. Ces zones permettent une combinaison unique de décollement d'API-verre modifié, de ténacité du stratifié et de durabilité du stratifié. Divers motifs spatiaux et densités de décollement sont décrits, ainsi que les propriétés de matériau ainsi obtenues.
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PCT/US2021/060814 WO2022132418A2 (fr) | 2020-12-16 | 2021-11-24 | Structures stratifiées avec couche intermédiaire polymère adhésive composite comprenant des zones de décollement cohésives pour une performance améliorée |
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WO2022132418A2 (fr) | 2022-06-23 |
WO2022132418A3 (fr) | 2022-08-04 |
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