CN111234772B - A kind of silicone liquid optical glue and using method thereof - Google Patents
A kind of silicone liquid optical glue and using method thereof Download PDFInfo
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- CN111234772B CN111234772B CN202010046888.8A CN202010046888A CN111234772B CN 111234772 B CN111234772 B CN 111234772B CN 202010046888 A CN202010046888 A CN 202010046888A CN 111234772 B CN111234772 B CN 111234772B
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- 239000003292 glue Substances 0.000 title claims abstract description 141
- 239000007788 liquid Substances 0.000 title claims abstract description 55
- 230000003287 optical effect Effects 0.000 title claims abstract description 55
- 229920001296 polysiloxane Polymers 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 title claims abstract description 15
- 239000000853 adhesive Substances 0.000 claims abstract description 33
- 230000001070 adhesive effect Effects 0.000 claims abstract description 33
- 239000000565 sealant Substances 0.000 claims abstract description 28
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 20
- 239000010703 silicon Substances 0.000 claims abstract description 20
- 238000012360 testing method Methods 0.000 claims abstract description 11
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 7
- 239000000126 substance Substances 0.000 claims abstract description 7
- 238000007429 general method Methods 0.000 claims abstract description 4
- 229920002545 silicone oil Polymers 0.000 claims description 60
- 239000001257 hydrogen Substances 0.000 claims description 54
- 229910052739 hydrogen Inorganic materials 0.000 claims description 54
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 49
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 49
- 229920002554 vinyl polymer Polymers 0.000 claims description 43
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 41
- 239000004568 cement Substances 0.000 claims description 35
- 239000003054 catalyst Substances 0.000 claims description 30
- 229920002050 silicone resin Polymers 0.000 claims description 24
- 229910052697 platinum Inorganic materials 0.000 claims description 20
- 239000003112 inhibitor Substances 0.000 claims description 13
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 13
- 238000001723 curing Methods 0.000 claims description 10
- 239000013008 thixotropic agent Substances 0.000 claims description 9
- 239000004034 viscosity adjusting agent Substances 0.000 claims description 6
- 125000004178 (C1-C4) alkyl group Chemical group 0.000 claims description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 4
- 125000006656 (C2-C4) alkenyl group Chemical group 0.000 claims description 2
- KLFRPGNCEJNEKU-FDGPNNRMSA-L (z)-4-oxopent-2-en-2-olate;platinum(2+) Chemical compound [Pt+2].C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O KLFRPGNCEJNEKU-FDGPNNRMSA-L 0.000 claims description 2
- FBSNEJXXSJHKHX-UHFFFAOYSA-N CC1=C(C(C=C1)([Pt]C)C)C Chemical compound CC1=C(C(C=C1)([Pt]C)C)C FBSNEJXXSJHKHX-UHFFFAOYSA-N 0.000 claims description 2
- 229910020388 SiO1/2 Inorganic materials 0.000 claims description 2
- 229910020447 SiO2/2 Inorganic materials 0.000 claims description 2
- 229910020487 SiO3/2 Inorganic materials 0.000 claims description 2
- FKRMGVVORAROKX-UHFFFAOYSA-N [Pt].[Pt].ClC1=C(CCCC1)Cl Chemical compound [Pt].[Pt].ClC1=C(CCCC1)Cl FKRMGVVORAROKX-UHFFFAOYSA-N 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims description 2
- 125000000217 alkyl group Chemical group 0.000 claims description 2
- CCQPAEQGAVNNIA-UHFFFAOYSA-N cyclobutane-1,1-dicarboxylic acid Chemical compound OC(=O)C1(C(O)=O)CCC1 CCQPAEQGAVNNIA-UHFFFAOYSA-N 0.000 claims description 2
- 229910021485 fumed silica Inorganic materials 0.000 claims description 2
- 238000013007 heat curing Methods 0.000 claims description 2
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 2
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 claims description 2
- CLSUSRZJUQMOHH-UHFFFAOYSA-L platinum dichloride Chemical compound Cl[Pt]Cl CLSUSRZJUQMOHH-UHFFFAOYSA-L 0.000 claims description 2
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims description 2
- 238000004383 yellowing Methods 0.000 abstract description 20
- 230000003712 anti-aging effect Effects 0.000 abstract 1
- 230000032683 aging Effects 0.000 description 33
- 230000000694 effects Effects 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 12
- 238000004132 cross linking Methods 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 5
- 238000000576 coating method Methods 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 238000010030 laminating Methods 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 229920005989 resin Polymers 0.000 description 5
- 239000011347 resin Substances 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 230000005856 abnormality Effects 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 3
- 238000003475 lamination Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- -1 methyl cyclohexyl vinyl Chemical group 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 229920001187 thermosetting polymer Polymers 0.000 description 3
- 230000004075 alteration Effects 0.000 description 2
- 229940120638 avastin Drugs 0.000 description 2
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- CREMABGTGYGIQB-UHFFFAOYSA-N carbon carbon Chemical compound C.C CREMABGTGYGIQB-UHFFFAOYSA-N 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000007822 coupling agent Substances 0.000 description 2
- 125000000753 cycloalkyl group Chemical group 0.000 description 2
- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 description 2
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 2
- 125000001624 naphthyl group Chemical group 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 230000002265 prevention Effects 0.000 description 2
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 2
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 229910002027 silica gel Inorganic materials 0.000 description 2
- 239000000741 silica gel Substances 0.000 description 2
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 2
- 238000001029 thermal curing Methods 0.000 description 2
- 239000004970 Chain extender Substances 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 230000003139 buffering effect Effects 0.000 description 1
- DLDJFQGPPSQZKI-UHFFFAOYSA-N but-2-yne-1,4-diol Chemical compound OCC#CCO DLDJFQGPPSQZKI-UHFFFAOYSA-N 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 125000000113 cyclohexyl group Chemical group [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C([H])([H])C1([H])[H] 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 description 1
- 230000004313 glare Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- NCWQJOGVLLNWEO-UHFFFAOYSA-N methylsilicon Chemical compound [Si]C NCWQJOGVLLNWEO-UHFFFAOYSA-N 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Classifications
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- 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
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
-
- 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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
-
- 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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
本发明提供了一种有机硅液态光学胶及其使用方法，包括框胶和面胶；其中，根据标准GB/T 614‑2006化学试剂折射率测定通用方法进行测试，所述框胶和面胶的折射率差值≤0.005。本发明提供的有机硅液态光学胶中的框胶和面胶的折射率差值极小，化学兼容性强，可以确保贴合后的框胶和面胶的界面没有痕迹；并且，本发明的框胶和面胶具有优异的耐老化抗黄变性能。The invention provides an organic silicon liquid optical adhesive and a method for using the same, including a frame glue and a surface glue; wherein, the test is carried out according to the standard GB/T 614-2006 general method for measuring the refractive index of chemical reagents, and the frame glue and the surface glue are tested. The refractive index difference ≤ 0.005. The difference in refractive index between the frame glue and the surface glue in the silicone liquid optical glue provided by the present invention is extremely small, and the chemical compatibility is strong, which can ensure that the interface between the glued frame glue and the surface glue has no traces; The sealant and top adhesive have excellent anti-aging and anti-yellowing properties.
Description
Technical Field
The invention belongs to the technical field of adhesives, and relates to an organic silicon liquid optical adhesive and a using method thereof.
Background
The full-lamination means that liquid optical cement is used for seamlessly laminating the display module with the touch panel/cover plate, so that the light loss and glare are reduced, the contrast is increased, the display effect is improved, and meanwhile, the technology has multiple effects of dust prevention, water prevention, stress buffering and the like. At present, the fully-laminated liquid optical adhesive in the market adopts a frame adhesive and a surface adhesive form, and the common use of the frame adhesive and the surface adhesive brings a new interface problem. The frame glue and the surface glue have poor compatibility, so that an interface is obvious and the display effect of the lamination is influenced; meanwhile, due to the difference of the refractive indexes between the frame glue and the surface glue, an obvious boundary line appears at the interface of the frame glue and the surface glue on the cured screen, and poor display is caused after the module is lightened. Further, after long-term use, interface traces become more and more obvious, resulting in a very large negative visual effect.
CN107286901A discloses a touch screen full-lamination frame glue and a preparation method thereof, which comprises the following components, by mass, 20-40% of vinyl silicone oil, 1-15% of hydrogen-containing silicone oil, 1-3% of a coupling agent, 30-50% of 110 raw glue, 5-10% of a thixotropic agent, 1-3% of a hardness regulator, 1-3% of a construction aid, 0.001-0.05% of a catalyst and 0.001-0.05% of an inhibitor. The frame glue provided by the invention has good compatibility with the organic silicon liquid glue, and can prevent the problem of bubble nucleus impurities in the organic silicon liquid optical glue after curing and attaching, but the frame glue is in a thermal curing form, and can reduce the production efficiency when being matched with ultraviolet cured surface glue.
However, the currently used optical adhesives have the defects of poor aging resistance, easy yellowing and the like, wherein the yellowing refers to the phenomena of color spots, yellowing of colors and even falling off after long-time use; the reason of yellowing generally includes the use of a catalyst, and when the addition amount of the catalyst is large, the platinum in the catalyst is easy to generate yellowing due to the fact that the platinum in the catalyst becomes dark platinum black after contacting air; meanwhile, in order to ensure that the optical adhesive has certain mechanical properties, a large number of phenyl or naphthyl aromatic groups and aromatic groups are basically introduced into the structure, so that the high-temperature aging yellowing of the system is easy to be serious. CN106047278A discloses a high-refractive-index yellowing-resistant LED packaging silica gel, which comprises a component A and a component B, wherein the weight ratio of the component A to the component B is 4: 1; the component A comprises the following raw materials in parts by weight: 80-90 parts of methyl cyclohexyl vinyl silicone resin, 8-18 parts of modified organic silicon with a cycloheyl and cyclohydrocarbyl structure-contained main chain, 0.1-0.3 part of platinum catalyst and 1-5 parts of adhesive; the component B comprises the following raw materials in parts by weight: 30-50 parts of modified organic silicon with a cyclohexyl and cycloalkyl structure in a main chain of a cyclic olefin end capping, 50-70 parts of modified organic silicon with a cycloalkyl structure in a main chain of a chain extender silicon hydrogen end capping and 0.1-0.3 part of inhibitor. Although the optical adhesive with higher yellowing resistance is obtained by abandoning the benzene ring structure in the structure, most of the mechanical properties are lost; meanwhile, the silica gel has a high refractive index.
Therefore, it is desired to develop and apply an optical adhesive which can realize seamless adhesion and has excellent aging resistance.
Disclosure of Invention
The invention aims to provide an organic silicon liquid optical cement and a using method thereof. The refractive index difference between the frame glue and the surface glue in the organic silicon liquid optical cement provided by the invention is extremely small, so that no trace is left on the interface between the frame glue and the surface glue after the frame glue and the surface glue are attached; in addition, the frame glue and the surface glue have excellent aging resistance and yellowing resistance.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the invention provides an organic silicon liquid optical cement, which comprises a frame cement and a surface cement;
wherein, the test is carried out according to the general method for measuring the refractive index of the chemical reagent GB/T614-2006, and the refractive index difference between the frame glue and the surface glue is less than or equal to 0.005, such as 0.004, 0.003, 0.002, 0.001 and the like.
The refractive index of the invention is a measurement result of the final form of the liquid optical cement after being cured.
The refractive index difference of the frame glue and the surface glue provided by the invention is extremely small and is less than 0.005, so that the technical effect of traceless bonding can be realized in application.
After the liquid optical adhesive provided by the invention is aged for 1000h at 90 ℃, the refractive index difference between the frame adhesive and the surface adhesive is still below 0.005, the frame adhesive and the surface adhesive are not separated, and the joint interface still has no trace, so that the liquid optical adhesive provided by the invention has good aging resistance and yellowing resistance.
In the present invention, the refractive indices of the frame glue and the face glue are each independently selected from 1.405-1.425, such as 1.408, 1.410, 1.412, 1.415, 1.418, 1.420, 1.422, and the like.
In the invention, the face glue comprises 60-80 parts of vinyl silicone oil, 5-40 parts of hydrogen-containing silicone oil and 5-25 parts of hydrogen-containing silicone resin by taking the total mass of the face glue as 100 parts, and further comprises a platinum catalyst and an inhibitor, wherein the platinum catalyst is used in an amount of 1-20ppm and the inhibitor is used in an amount of 5-200ppm by taking the total mass of the hydrogen-containing silicone oil and the hydrogen-containing silicone resin in the face glue as 100%.
The frame glue comprises, by 100 parts by total mass of the frame glue, 50-80 parts of vinyl silicone oil, 5-15 parts of hydrogen-containing silicone oil, 5-20 parts of hydrogen-containing silicone resin and 10-25 parts of a viscosity regulator, and further comprises a platinum catalyst, wherein the platinum catalyst is used in an amount of 0.5-2.5ppm, such as 0.8ppm, 1.0ppm, 1.2ppm, 1.5ppm, 1.7ppm, 1.9ppm, 2.0ppm, 2.2ppm, 2.4ppm and the like, by total mass of the hydrogen-containing silicone oil and the hydrogen-containing silicone resin in the frame glue being 100%.
Besides the viscosity regulator, the surface glue and the frame glue are applied by selecting the same type of components, so that the differences in the aspects of refractive index, chromatic aberration, haze and the like of the surface glue and the frame glue can be ensured to be small, the compatibility of the surface glue and the frame glue is extremely high, and the traceless laminating effect can be achieved.
It should be noted that in the components of the frame gum and the face gum in the present invention, although the names and types of the components are the same, the same materials are not necessarily selected, for example, the frame gum and the face gum both contain vinyl silicone oil, but since the vinyl silicone oil has different vinyl contents, molecular weights, etc., the specific selection of the vinyl silicone oil in the frame gum and the face gum may be the same or different, as long as the specific materials selected are all vinyl silicone oil. This explanation is made for other components such as hydrogen-containing silicone oil, hydrogen-containing silicone resin, and the like.
In the face glue of the invention, the vinyl silicone oil is 60-80 parts, such as 62 parts, 65 parts, 68 parts, 70 parts, 72 parts, 75 parts, 78 parts and the like.
In the face glue of the invention, the hydrogen-containing silicone oil is 5-40 parts, such as 15 parts, 20 parts, 25 parts, 30 parts, 35 parts and the like.
In the face glue of the invention, the hydrogen-containing silicone resin is 5-25 parts, such as 6 parts, 8 parts, 10 parts, 15 parts, 18 parts, 20 parts, 22 parts and the like.
In the face glue of the invention, the platinum catalyst is 1-20ppm, such as 2ppm, 5ppm, 10ppm, 12ppm, 15ppm, 18ppm and the like.
In the face gum of the present invention, the inhibitor is 5 to 200ppm, for example, 10ppm, 20ppm, 50ppm, 80ppm, 100ppm, 120ppm, 150ppm, 180ppm, etc.
In the sealant of the present invention, the vinyl silicone oil is 50 to 80 parts, for example, 55 parts, 60 parts, 65 parts, 70 parts, 75 parts, and the like.
In the sealant of the present invention, the hydrogen-containing silicone oil is 5 to 40 parts, for example, 15 parts, 20 parts, 25 parts, 30 parts, 35 parts, and the like.
In the sealant of the present invention, the hydrogen-containing silicone resin is 5 to 25 parts, for example, 6 parts, 8 parts, 10 parts, 15 parts, 18 parts, 20 parts, 22 parts, etc.
In the sealant of the present invention, the viscosity modifier is 5 to 25 parts, for example, 10 parts, 12 parts, 15 parts, 17 parts, 20 parts, 22 parts, etc.
In the sealant of the present invention, the platinum catalyst is 1 to 50ppm, for example, 2ppm, 5ppm, 10ppm, 12ppm, 15ppm, 18ppm, 20ppm, 30ppm, 40ppm, etc.
In the sealant of the present invention, the inhibitor is 200ppm or more, for example, 210ppm, 220ppm, 250ppm, 280ppm, 300ppm, 320ppm, 350ppm, 380ppm, etc.
In the present invention, the vinyl silicone oil in the sealant and the vinyl silicone oil in the surface sealant are the same or different, and the molecular weight is independently selected from 9000-.
Preferably, the vinyl content in the vinyl silicone oil in the frame glue and the vinyl content in the vinyl silicone oil in the surface glue are each independently selected from 0.01-0.3mmol/g, such as 0.02mmol/g, 0.03mmol/g, 0.04mmol/g, 0.06mmol/g, 0.08mmol/g, 0.1mmol/g, 0.15mmol/g, 0.18mmol/g, 0.20mmol/g, 0.25mmol/g, 0.28mmol/g, and the like.
Preferably, the side group of the vinyl silicone oil in the frame glue and the side group of the vinyl silicone oil in the face glue are respectively and independently selected from linear chain or branched chain alkyl of C1-C4.
The C1-C4 can be C1, C2, C3, C4 and the like, namely methyl, ethyl, propyl, isopropyl, butyl, isobutyl, tert-butyl and the like.
In the invention, the hydrogen-containing silicon resin in the frame glue and the hydrogen-containing silicon resin in the surface glue are the same or different and are liquid MQ type methyl silicon resin.
In the invention, the hydrogen-containing silicone oil in the frame glue and the hydrogen-containing silicone oil in the surface glue are the same or different and have the following structures:
wherein R is1、R2Each independently selected from C1-C4 alkyl groups such as methyl, ethyl, propyl, isopropyl, butyl, isobutyl, tert-butyl and the like, preferably methyl.
R3Is H or methyl.
m is an integer from 10 to 500, such as 8, 10, 15, 20, 25, 30, 35, 40, 45, 50, 80, 100, 120, 150, 180, etc., and n is an integer from 0 to 50, such as 3, 4, 5, 6, 7, 8, 9, 10, 20, 30, 40, etc.
According to the invention, the vinyl silicone oil with large molecular weight and low vinyl content is specifically selected to react with the polyfunctional group hydrogen-containing silicone oil with high reaction activity, so that carbon-carbon single bonds in a cross-linked network are reduced, and the high temperature resistance and aging resistance of the composition can be improved; meanwhile, the hydrogen-containing silicone oil selected by the invention has high reaction activity, so that the use amount of the catalyst can be reduced, and the high catalytic reaction rate can be ensured; and due to the reduction of the dosage of the catalyst, the aging resistance and yellowing resistance of the liquid optical cement can be further improved; in addition, the vinyl silicone oil, the hydrogen-containing silicone oil and the hydrogen-containing silicone resin do not contain easy-yellowing groups such as phenyl, naphthyl or amino, can further increase the aging resistance and yellowing resistance of the liquid optical adhesive, and are more beneficial to the application of the liquid optical adhesive in a harsher environment.
Preferably, in the sealant, the molar ratio of the silicon-hydrogen bond to the vinyl group is 1 (0.95-1.15), such as 1:0.98, 1:1.0, 1:1.05, 1:1.1, 1:1.12, and the like.
Preferably, in the surface glue, the molar ratio of the silicon-hydrogen bond to the vinyl group is 1 (0.95-1.15), such as 1:0.98, 1:1.0, 1:1.05, 1:1.1, 1:1.12 and the like.
Preferably, the hydrogen-containing silicone resin in the frame glue and the hydrogen-containing silicone resin in the surface glue are the same or different and are both liquid MQ type methyl silicone resin.
In the present invention, the viscosity modifier has the following structure:
(R1R2R3SiO1/2)x(R1R2SiO2/2)y(R1SiO3/2)z；
wherein R is1、R3Each independently selected from C1-C4 alkyl or C2-C4 alkenyl, the C1-C4 can be C1, C2, C3, C4 and the like, the C2-C4 can be C2, C3, C4 and the like.
R2One selected from methyl, ethyl, hydroxyl, vinyl or hydrogen atoms.
x, y, z is (0.5-5): (0.25-0.5):1, the 0.5-5 can be 1, 1.5, 2, 2.5, 3, 3.5, 4, 4.5, etc., the 0.25-0.5 can be 0.3, 0.35, 0.4, 0.45, etc.
Preferably, the viscosity of the viscosity modifier is 100000-2500000 mPas, such as 200000 mPas, 500000 mPas, 800000 mPas, 1000000 mPas, 1200000 mPas, 1500000 mPas, 1800000 mPas, 2000000 mPas, 2300000 mPas, and the like.
The viscosity regulator selected by the invention is the silicone resin with higher viscosity, can be reactive or non-reactive, and the constituent groups of the viscosity regulator are the same as the main components of the frame glue and the surface glue, so that the viscosity regulator has small differences in refractive index, chromatic aberration, haze and the like and has good compatibility with other components.
Preferably, the catalyst in the frame glue and the catalyst in the surface glue are independently selected from any one of or a combination of at least two of chloroplatinic acid isopropanol solution, karstedt platinum catalyst, Willing platinum catalyst, (trimethyl) methyl cyclopentadienyl platinum, platinum acetylacetonate, bis (mu-chloro) dichloro (cyclohexene) diplatin, (1,5 cyclo zinc diene) platinum chloride, and 1, 1-cyclobutane dicarboxylic acid diammine platinum.
Preferably, the sealant further includes a thixotropic agent.
Preferably, the thixotropic agent is added in an amount of no more than 0.15 parts, such as 0.01 parts, 0.02 parts, 0.05 parts, 0.08 parts, 0.1 parts, 0.11 parts, 0.13 parts, 0.14 parts, and the like.
Preferably, the thixotropic agent is selected from fumed silica and/or organobentonite.
The invention adjusts the viscosity by adding silicone resin, the addition of thixotropic agent is not more than 0.15 part to adjust the coating manufacturability of the frame glue, and avoids influencing the transparency and refractive index of the frame glue by adding too much thixotropic agent.
Preferably, the inhibitor in the frame glue and the inhibitor in the surface glue are respectively and independently selected from any one or a combination of at least two of alkynol substances, vinyl ring substances or maleate substances.
Preferably, the sealant has a viscosity of 30000-100000 mPas, such as 40000 mPas, 50000 mPas, 60000 mPas, 70000 mPas, 80000 mPas, 90000 mPas, etc., and the topcoat has a viscosity of 1000-6500 mPas, such as 2000 mPas, 3000 mPas, 4000 mPas, 5000 mPas, 6000 mPas, etc.
The surface glue and the frame glue in the range can ensure the operability of coating, sizing, leveling or bubble removal in the subsequent process.
Preferably, the frame glue has a touch value of 1.5-4, such as 2, 2.5, 3, 3.5, etc.
In a second aspect, the invention provides a method for using the thermosetting silicone liquid optical adhesive according to the first aspect, and the method comprises the steps of sealant joint filling, sealant dam enclosing, sealant pre-curing, surface sealant applying, laminating, and heating and curing in sequence.
In the invention, the step of filling the seam by using the frame glue is to coat a circle of the frame glue of the liquid optical glue at the junction of the metal frame and the display surface of the display module to form a seam filling ring, so that the surface glue is prevented from flowing into the backlight module through a gap between the metal frame and the display panel to cause pollution.
The frame glue dam is formed by coating a circle of frame glue of the liquid optical glue on the peripheries of four frames of a metal frame of the display module to prevent a large amount of surface glue from overflowing during fitting, the thickness of the surface glue during fitting is limited, and the uniform thickness of a fitting surface is ensured.
The frame glue pre-curing refers to performing thermal curing on the seam filling ring and the dam enclosing ring, and heating for 10-60min (for example, 20min, 30min, 40min, 50min and the like) in an environment of 45-90 ℃ (for example, 50 ℃, 60 ℃, 70 ℃, 80 ℃ and the like) to complete curing.
The surface glue applying means that the surface glue of the liquid optical glue is coated on the display surface of the display module according to a certain pattern.
The attaching means that the touch module or the protective cover plate is attached to the display module coated with the surface glue of the liquid optical cement in a vertically downward state to form an attaching assembly.
The heating and curing refers to heating the attaching assembly in an environment of 50-90 ℃ (e.g. 60 ℃, 70 ℃, 80 ℃ and the like) for 10-60min (e.g. 20min, 30min, 40min, 50min and the like) to completely cure the surface glue of the liquid optical glue.
In the present invention, the width of the sealant coating is 200-2000 μm, such as 200 μm, 500 μm, 1000 μm, 2000 μm, etc., and the height is 100-600 μm, such as 200 μm, 300 μm, 400 μm, 500 μm, etc., during the dam enclosing.
In the present invention, the coating thickness of the surface glue is 200-2000 μm, such as 200 μm, 500 μm, 1000 μm, 1500 μm, 2000 μm, etc.
The liquid optical cement provided by the invention has the advantages of complete heating and rapid curing, can omit the investment of light curing equipment in a heat curing mode directly, and reduces the cost.
Compared with the prior art, the invention has the following beneficial effects:
(1) the refractive index difference of the frame glue and the surface glue provided by the invention is extremely small and is below 0.005, so that the technical effect of traceless bonding can be realized during application;
(2) according to the invention, the vinyl silicone oil with large molecular weight and low vinyl content is specifically selected to react with the polyfunctional group hydrogen-containing silicone oil with high reaction activity, so that carbon-carbon single bonds in a cross-linked network are reduced, and the high temperature resistance and aging resistance of the composition can be improved; meanwhile, the hydrogen-containing silicone oil selected by the invention has high reaction activity, so that the use amount of the catalyst can be reduced, and the high catalytic reaction rate can be ensured; and due to the reduction of the dosage of the catalyst, the aging resistance and yellowing resistance of the liquid optical cement can be further improved; in addition, the vinyl silicone oil, the hydrogen-containing silicone oil and the hydrogen-containing silicone resin do not contain easy-yellowing groups such as phenyl, naphthyl or amino, can further increase the aging resistance and yellowing resistance of the liquid optical adhesive, and are more beneficial to the application of the liquid optical adhesive in a harsher environment.
(3) The frame glue and the surface glue contained in the organic silicon liquid optical glue provided by the invention have extremely small refractive index difference value below 0.005, excellent aging resistance, good effect after bonding, high stability and no limit state before and after aging.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
The following examples and comparative examples relate to the following materials and the following trade mark information:
(A) vinyl silicone oil
(B) Hydrogen-containing silicone oil
(C) Hydrogen-containing silicon resin
(D) Viscosity modifier
| (Code) | Manufacturer(s) | Number plate | Name (R) | Viscosity (mPa. s) |
| D-1 | New four seas of Hubei province | SH-9502 | Methyl silicone resin | 200000 |
| D-2 | Hangzhou silicon base material | Y-19468 | MDT type methyl silicone resin | 1500000 |
(E) Platinum catalyst
Karstedt catalyst, avastin reagent, product number: K131673.
(F) inhibitors
1, 4-butynediol, an alatin reagent, product number: B103673.
(G) other auxiliaries
Coupling agent: vinyltriethoxysilane, avastin reagent, product number: t103647.
Examples 1 to 6
The silicone liquid optical cement was prepared according to the composition shown in table 1.
TABLE 1
Comparative examples 1 to 4
Thermosetting liquid optical adhesive compositions were prepared according to the components shown in Table 2.
TABLE 2
Performance testing
The thermosetting liquid optical cement compositions provided in examples 1 to 4 and comparative examples 1 to 4 were subjected to the following performance tests:
(1) refractive index: testing according to a general method for measuring the refractive index of a chemical reagent GB/T614-2006, and respectively testing the refractive indexes of the frame glue and the surface glue;
(2) hardness: the shore hardness of the cured samples was tested according to ASTM D2240 (OO shore durometer);
(3) heat aging resistance; preparing a sample sheet to be tested with the thickness of 1mm between two transparent cover plates, aging for 2000h at 90 ℃, and then testing the yellowing b value after aging according to GB/T7921-;
(4) light aging resistance: preparing a sample piece to be tested with the thickness of 1mm between two transparent cover plates, carrying out xenon lamp aging for 1000h under the conditions of 65 ℃ of temperature and 65% of relative humidity according to ISO4892-2-2013, and then testing the yellowing b value after aging according to GB/T7921-2008;
(5) the laminating effect: attaching the display module and the touch panel by using a sample (frame glue and surface glue), wherein the attaching number n is 3, testing and inspecting corresponding items after curing, observing whether the attaching surface has abnormalities such as glue failure, bubbles, yellow spots, fogging and the like, marking the attaching surface as 'PASS' if the attaching surface does not have the abnormalities, and marking the attaching surface as 'NG + abnormal description' if the attaching surface has the abnormalities; and simultaneously observing whether a boundary line appears between the glued and aged frame glue and the surface glue, if not, marking OK, and if so, marking NG, wherein the test conditions are as follows:
a state (initial state after solidification)
High temperature and high humidity: 60 ℃/90% RH multiplied by 1000 h;
high temperature: multiplying the temperature at 90 ℃ for 2000 h;
low temperature: -40 ℃ x 2000 h;
cold and hot impact: 30min at-40 ℃ and 30min at 85 ℃ for 30min, and 1000 cycles.
The test results are shown in tables 3 and 4:
TABLE 3
TABLE 4
According to the embodiment and the performance test, the liquid optical cement prepared by the invention comprises frame glue and surface glue, has excellent light and heat aging resistance, good laminating effect and high stability, and is in a boundless state before and after aging.
In the surface glue, as can be seen from the comparison between the example 1 and the comparative example 1, if the vinyl silicone oil content in the surface glue is too high, the viscosity is too low, the glue flows seriously in the bonding process, the bonding thickness is not uniform, and bubbles (back bubbles) are easily generated during the reliability aging; as can be seen from comparison between example 2 and comparative example 3 and between example 3 and comparative example 2, in the surface adhesive, too high or too low content of the hydrogen-containing resin easily causes transition or insufficiency of crosslinking, thereby causing too high hardness, too large hardness, aging and adhesive failure, and simultaneously generating a boundary line, or insufficient crosslinking degree, poor aging resistance and easy yellowing after aging; as can be seen from the comparison between example 3 and comparative example 4, when the hydrogen-containing silicone oil with low number of silicon-hydrogen bond functions is used in the surface glue, the crosslinking density is low, the light and heat aging resistance is weak, and bond breakage is easy to occur under light and heat aging, so that the glue is yellowed, and the b value is obviously increased after aging.
In the frame glue, as can be seen from comparison between the example 2 and the comparative example 1, if the content of the vinyl silicone oil in the frame glue or the surface glue is too high, the viscosity is too low, the glue flows seriously in the bonding process, the bonding thickness is not uniform, and bubbles (back bubbles) are easily generated during reliability aging; as can be seen from the comparison between the example 3 and the comparative examples 2-3, when the vinyl silicone oil is insufficient (the frame sealant comparative example 2) or the hydrogen-containing silicone oil with low silicon-hydrogen bond functional number (the frame sealant comparative example 3) is used, the crosslinking density is low, the crosslinking degree is not high, and the bond breaking is easy to occur under the aging of light and heat, so that the glue is yellow, and the b value is obviously increased after the aging; comparing example 3 with comparative example 4, it can be seen that if raw materials with high vinyl content are used, more carbon-carbon bonds are produced by crosslinking, and bond breakage is easy to occur under light and heat aging, so that the glue is yellow, and the b value is obviously increased after aging.
The applicant states that the present invention is illustrated by the above examples to show the silicone liquid optical cement and the method of using the same, but the present invention is not limited to the above detailed method, i.e. it does not mean that the present invention must be implemented by relying on the above detailed method. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
Claims (18)
1. An organic silicon liquid optical cement is characterized by comprising frame cement and surface cement;
wherein, the test is carried out according to the general method for measuring the refractive index of the chemical reagent GB/T614-2006, and the refractive index difference between the frame glue and the surface glue is less than or equal to 0.005;
the face glue comprises 60-80 parts of vinyl silicone oil, 5-40 parts of hydrogen-containing silicone oil and 5-25 parts of hydrogen-containing silicone resin by taking the total mass of the face glue as 100 parts, and further comprises a platinum catalyst and an inhibitor, wherein the platinum catalyst is used in an amount of 1-20ppm and the inhibitor is used in an amount of 5-200ppm by taking the total mass of the hydrogen-containing silicone oil and the hydrogen-containing silicone resin in the face glue as 100%;
the frame glue comprises 50-80 parts of vinyl silicone oil, 5-15 parts of hydrogen-containing silicone oil, 5-20 parts of hydrogen-containing silicone resin and 10-25 parts of viscosity regulator by taking the total mass of the frame glue as 100 parts, and further comprises a platinum catalyst, wherein the platinum catalyst is 0.5-2.5ppm by taking the total mass of the hydrogen-containing silicone oil and the hydrogen-containing silicone resin in the frame glue as 100%;
the vinyl silicone oil in the frame glue and the vinyl silicone oil in the surface glue are the same or different, and the molecular weights are respectively and independently selected from 9000-200000;
the vinyl content in the vinyl silicone oil in the frame glue and the vinyl content in the vinyl silicone oil in the surface glue are respectively and independently selected from 0.01 to 0.3 mmol/g;
the hydrogen-containing silicone oil in the frame glue and the hydrogen-containing silicone oil in the surface glue are the same or different and have the following structures:
wherein R is1、R2Each independently selected from C1-C4 alkyl;
R3is H or methyl;
m is an integer of 10 to 500, and n is an integer of 3 to 50.
2. The silicone liquid optical cement of claim 1, wherein the refractive indices of the frame and face glues are each independently selected from 1.405-1.425.
3. The silicone liquid optical adhesive as claimed in claim 1, wherein the vinyl silicone oil in the sealant and the vinyl silicone oil in the surface adhesive are the same or different, and the molecular weights are respectively and independently selected from 10000-200000.
4. The silicone liquid optical glue of claim 1, wherein the pendant vinyl silicone oil groups in the frame glue and the pendant vinyl silicone oil groups in the face glue are each independently selected from linear or branched alkyl groups of C1-C4.
5. The silicone liquid optical cement according to claim 1, wherein the hydrogen-containing silicone resin in the frame glue and the hydrogen-containing silicone resin in the surface glue are the same or different and are liquid MQ type methyl silicone resins.
6. The silicone liquid optical cement according to claim 1, wherein the hydrogen-containing silicone oil in the sealant and the hydrogen-containing silicone oil in the surface cement are the same or different and have the following structures:
wherein R is1、R2Are both methyl;
R3is H or methyl;
m is an integer of 10 to 500, and n is an integer of 3 to 50.
7. The silicone liquid optical cement as claimed in claim 1, wherein the molar ratio of the Si-H bond to the vinyl group in the sealant is 1 (0.95-1.15).
8. The organic silicon liquid optical cement as claimed in claim 1, wherein the molar ratio of the silicon hydrogen bond to the vinyl group in the surface cement is 1 (0.95-1.15).
9. The silicone liquid optical cement according to any one of claims 3-6, wherein the viscosity modifier has the following structure:
(R1R2R3SiO1/2)x(R1R2SiO2/2)y(R1SiO3/2)z；
wherein R is1、R3Each independently selected from C1-C4 alkyl or C2-C4 alkenyl;
R2one selected from methyl, ethyl, hydroxyl, vinyl or hydrogen atom;
x:y:z＝(0.5-5):(0.25-0.5):1。
10. the silicone liquid optical cement as claimed in claim 1, wherein the viscosity of the viscosity modifier is 100000-2500000 mPa-s.
11. The silicone liquid optical cement of claim 1, wherein the sealant further comprises a thixotropic agent.
12. The silicone liquid optical cement of claim 11, wherein the thixotropic agent is added in an amount of no more than 0.15 parts.
13. The silicone liquid optical cement of claim 11, wherein the thixotropic agent is selected from fumed silica and/or organobentonite.
14. The silicone liquid optical adhesive according to claim 1, wherein the inhibitor in the frame glue and the inhibitor in the surface glue are each independently selected from one or a combination of at least two of alkynol substances, vinyl ring substances or maleate substances.
15. The silicone liquid optical adhesive as claimed in claim 1, wherein the viscosity of the sealant is 30000-100000 mPa-s, and the viscosity of the surface adhesive is 1200-6500 mPa-s.
16. The silicone liquid optical cement according to claim 1, wherein the frame cement has a touch value of 1-4.
17. The silicone liquid optical cement as claimed in claim 1, wherein the catalyst in the frame glue and the catalyst in the surface glue are each independently selected from any one of or a combination of at least two of chloroplatinic acid isopropanol solution, karstedt platinum catalyst, Willing platinum catalyst, (trimethyl) methylcyclopentadienyl platinum, platinum acetylacetonate, bis (μ -chloro) dichloro (cyclohexene) diplatinum, (1, 5-Cyclozincdiene) platinum chloride, and 1, 1-cyclobutane dicarboxylic acid diammine platinum.
18. The use method of the silicone liquid optical cement as claimed in any one of claims 1 to 17, wherein the use method comprises sequentially performing sealant caulking, sealant dam enclosing, sealant pre-curing, surface sealant applying, attaching and heat curing.
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