CN105754544B - Touch screen fitting optics transparent resin and attaching process - Google Patents
Touch screen fitting optics transparent resin and attaching process Download PDFInfo
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- CN105754544B CN105754544B CN201410781866.0A CN201410781866A CN105754544B CN 105754544 B CN105754544 B CN 105754544B CN 201410781866 A CN201410781866 A CN 201410781866A CN 105754544 B CN105754544 B CN 105754544B
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Abstract
The invention discloses a kind of touch screen fitting optics transparent resin and attaching process.The touch screen fitting is the double cured organic siliconresins of ketoxime removing type moisture/ultraviolet light with optics transparent resin, by weight percentage, including the silicone terminated dimethyl silicone polymer of 100 parts of vinyl ketone oximidos, 5-100 parts of MQ resins, 0.1-20 parts of sulfydryl silicone oil, 0.1-2 parts of moisture-curable catalyst and 0.1-2 parts of ultraviolet initiators.There is good initial bonding strength in pressure-sensitive state through ultraviolet light irradiation after fitting of the invention optics transparent resin gluing, will not be subjected to displacement after fitting, the moisture-curable of the touch screen posted through the air is finally reached good bonding intensity.The double cured silicone resins of the ketoxime removing type that the present invention selects can save 1 year so that the fitting of inventive touch screen is more preferable with optics transparent resin keeping quality under room temperature；And under equal conditions, moisture-curable speed is faster than selecting dealcoholized type pair cured silicone resin.
Description
Technical field
The invention belongs to optical adhesive/sealant preparation and electronic information technical fields, and in particular to a kind of touch screen
Fitting optics transparent resin and attaching process.
Background technique
Smart phone and plate market, which mostly use, at present directly fits technology (Direct Bonding or full
Lamination) eliminate LCM(liquid crystal module) and touched panel glass or film between gap.Many touch panel factories into
When row glass gluing, habit is using the optical adhesive tape OCA(Optical Clear that production efficiency is higher, thickness is uniform
Adhesive) coating technique, but OCA is similar to a kind of transparent double-sided pressure-sensitive, and adhesive strength is smaller, is unsuitable for adhesive strength
More demanding fitting.It, can not when being easy to produce bubble and increase fraction defective, and being bonded simultaneously using this technology in fitting
It was found that micro-bubble may also expand with the time.Bubble removing problem will affect outside yield, since OCA is not easy to reprocess, the flaw
Defective product can only be scrapped mostly, low so as to cause productivity effect and increase fitting factory's cost pressure.
Compared to OCA, ultraviolet curing optics of liquids transparent resin LOCA(Liquid Optical Clear Adhesive)
It since abutted equipment is simple, can reprocess, be easy deaeration, the cost of material is low, the features such as influence by ink segment difference, by more
Carry out the welcome of more touch panel manufacturers.But simultaneously because touch panel frame portion is printed with lighttight ink,
Ultraviolet light cannot be irradiated to these places through ink, so that uncured region is generated, even if these regions are additionally carried out sidelight
Source irradiation can not ensure completion of cure, and this considerably increases equipment costs, reduce production efficiency.
Patent application CN 103992650 discloses a kind of double cured silicone resin combinations of ultraviolet light/moisture, light transmission
Part can be avoided common UV resin dash area and not solidified with ultraviolet curing, dash area with moisture-curable
The problem of.But ultraviolet light irradiation after pressure-sensitive character can not be presented, once by ultraviolet light irradiation solidify at once, at this time due to
Resin surface, which has been cured, does not have viscosity, cannot carry out the fitting of cover-plate glass or film again.And an urgent demand in the market
It is capable of providing after a kind of irradiation of ultraviolet light and pressure-sensitive state is presented, there is good initial bonding strength, will not be displaced after fitting, place
A period of time reaches the resin material of very high adhesive strength.
Summary of the invention
The object of the present invention is to provide a kind of optically transparent touch screen fitting optical lens with moisture-curable function
Ming tree rouge and attaching process.
Fitting of the invention after gluing, is bonded it in cover-plate glass or film vacuum on LCM with optics transparent resin
Preceding progress ultraviolet light irradiation, because being not in common there is no the shading of cover-plate glass or film upper edge sub-ink
The problem of dash area of ultraviolet curing optics of liquids transparent resin does not solidify.
Pressure-sensitive state, which is presented, through ultraviolet light irradiation after gluing on LCM in fitting optics transparent resin of the invention has
Good initial bonding strength will not be subjected to displacement after fitting, and the moisture-curable of the touch screen posted through the air is finally reached
Good bonding intensity.
Realizing the technical solution of the object of the invention is: touch screen fitting optics transparent resin, with weight percent
Meter, including the silicone terminated dimethyl silicone polymer of 100 parts of vinyl ketone oximidos, 5-100 parts of MQ resins, 0.1-20 parts of sulfydryl silicone oil,
0.1-2 parts of moisture-curable catalyst and 0.1-2 parts of ultraviolet initiators.
The present invention uses the organosilicon UV resin (ultraviolet curable resin) with moisture-curable function, the gluing on LCM
After irradiated through ultraviolet light, then carry out the vacuum abutted of cover-plate glass or film, the touch screen posted is through the air
Moisture-curable is finally reached good bonding intensity.
Wherein, the MQ silicone resin is by tetra functional siloxane polycondensation chain link (Q) and single functionality siloxane unit
(M) organic siliconresin constituted, molal weight 1000-8000, M/Q ratio are 0.6-1.0.MQ resin can be liquid
It can be solid.The MQ resin is preferably methyl MQ resin or vinyl MQ resin.
The silicone terminated dimethyl silicone polymer of vinyl ketone oximido has the following structure:
X1, X2, X3 and X4 represent methyl, ethyl, any one group in butanone oximido, and n is the integer of 100-10000.
X1, X2, X3, X4 can be the same or different, and preferably be all butanone oximido.
The sulfydryl silicone oil has the following structure:
R1, R2, R3 represent methyl, ethyl, propyl, vinyl, phenyl, any base in the saturation of long-chain or unsaturated alkyl
Group.R1, R2, R3 may be the same or different.The preferred methyl of R1, R3, the preferred propyl of R2, m and n are the integer of 4-1000.
By weight percentage, sulfhydryl content is 0.1-30wt% in the sulfydryl silicone oil, and sulfhydryl content is preferably 0.1-
20wt%。
The ultraviolet initiator is selected from 2- hydroxy-2-methyl -1- phenyl -1- acetone (1173), 2,4,6- front three
The mixture of base benzoyl-diphenyl phosphine oxide (TPO), 2,4,6- tri-methyl benzophenone and 4- methyl benzophenone
(Esacure TZT), benzoin dimethylether (651), benzophenone, 1- hydroxy-cyciohexyl Benzophenone (184), α, α '-ethyoxyl
One or more of mixing in acetophenone (DEAP) or α-amine alkyl phenones.It is preferred that 2- hydroxy-2-methyl -1- phenyl -1- acetone
(1173) or 1- hydroxy-cyciohexyl Benzophenone (184).
The moisture-curable catalyst is organo-tin compound, titanate ester compound, α silane coupling agent, lewis acid
Class or Louis's alkaloid compound.It is preferred that organo-tin compound or titanate ester compound.
Compared with prior art, the invention has the advantages that
1. attaching process of the invention is to carry out ultraviolet photo-curing before fitting, cover-plate glass or film side are avoided
The problem of edge ink dash area does not solidify.
2. pressure-sensitive state can be presented after ultraviolet photo-curing, will not be subjected to displacement after fitting and current OCA performance
It is similar, it can be bonded using existing OCA abutted equipment and technique, without increasing new abutted equipment.
3. optical clear resin of the invention can also further be consolidated moisture after cover-plate glass or film vacuum fitting
Change, substantially increases the adhesive strength between LCM and cover-plate glass or film.
4. the MQ resin that the present invention selects, through experiments, it was found that, the initial bonding strength after ultraviolet light irradiation can not only be improved,
The transparency of resin can be greatly improved, this has practical significance in touch screen fitting.
5. the double cured silicone resins of the ketoxime removing type that the present invention selects, so that optical clear is used in the fitting of inventive touch screen
Resin keeping quality is more preferable, can save under room temperature 1 year；And under equal conditions, the present invention selects the double solidifications of ketoxime removing type to have
The moisture-curable speed of machine silicone resin is faster than selecting dealcoholized type pair cured silicone resin.
Specific embodiment
The present invention is described further below in conjunction with embodiment and comparative example.
The present invention provides a kind of optically transparent, UV resin (ultraviolet curable resin) with moisture-curable function and new
Type attaching process.
The organosilicon UV resin with moisture-curable function is made of five kinds of ingredients, and vinyl ketone oximido is silicone terminated
Dimethyl silicone polymer, MQ resin, sulfydryl silicone oil crosslinking agent, moisture-curable catalyst and ultraviolet initiator.But it is of the invention
Constituent is not limited to this five kinds of ingredients, can add transparent inorganic filler, response type or non-reactive plasticizer, dilute as needed
Release agent, heat stabilizer, levelling agent, defoaming agent, thixotropic agent, preservative, light stabilizer etc..
Wherein, the silicone terminated dimethyl silicone polymer of vinyl ketone oximido in the present invention has the following structure:
X1, X2, X3 and X4 represent methyl, ethyl, any one group in butanone oximido, and n is the integer of 100-10000.
X1, X2, X3, X4 can be the same or different, and preferably be all butanone oximido.
The silicone terminated dimethyl silicone polymer of vinyl ketone oximido in the present invention can use terminal hydroxy group polydimethylsiloxanes
Alkane and vinyl ketone oximino silane coupling agent react in the presence of catalyst to prepare, and can also purchase the poly dimethyl blocked
Raw material of the siloxanes as constituent.
When preparation, the vinyl ketone oximino silane coupling agent for sealing end can be the coupling of three ketoximinosilanes of vinyl
Agent is also possible to two ketoximinosilanes coupling agent of vinyl.
MQ resin of the invention is by tetra functional siloxane polycondensation chain link (Q) and single functionality siloxane unit (M) structure
At organic siliconresin, molal weight 1000-8000, M/Q ratio be 0.6~1.0.MQ resin can be liquid can also be with
It is solid.Different according to the functional group on silicon atom, MQ resin can be divided into methyl MQ resin, phenyl MQ resin, aminomethyl phenyl
MQ resin, vinyl MQ resin, hydrogeneous MQ resin.The preferred methyl MQ resin of the present invention and vinyl MQ resin.
The MQ resin that the present invention selects finds that it can not only improve the initial bonding strength after ultraviolet light irradiation, can also mention significantly
The transparency of high resin.
Sulfydryl silicone oil structure in the present invention is as follows:
R1, R3 are methyl, and R2 is propyl, the integer that m and n are 4-1000.Wherein, by weight percentage, sulfydryl silicone oil
Middle sulfhydryl content is 0.1-30wt%, preferably 0.1-20wt%.
Ultraviolet initiator in the present invention is selected from 2- hydroxy-2-methyl -1- phenyl -1- acetone (1173), 2,4,6-
The mixture of trimethylbenzoy-dipheny phosphine oxide (TPO), 2,4,6- tri-methyl benzophenone and 4- methyl benzophenone
(Esacure TZT), benzoin dimethylether (651), benzophenone, 1- hydroxy-cyciohexyl Benzophenone (184), α, α '-ethyoxyl
One or more of mixing in acetophenone (DEAP) or α-amine alkyl phenones.It is preferred that 2- hydroxy-2-methyl -1- phenyl -1- acetone
(1173), DEAP or 1- hydroxy-cyciohexyl Benzophenone (184).
The moisture-curable catalyst that the present invention uses has five major class, and organo-tin compound, titanate ester compound, α-silane are even
Join agent, Louis's acids and Louis's alkaloid compound.
Common organic tin moisture-curable catalyst includes: dibutyl tin dilaurate, dibutyltin diacetate, diethyl
Caproic acid dibutyl tin, two sad dibutyl tins, dimethyl maleic acid dibutyl tin, dibutyitin maleate, oxalic acid dioctyl
Tin, distearyl acid dioctyl tin, tin dilaurate dioctyl tin, dimethyl dibutyl tin, two phenoxy group dibutyl tins, two diacetylmonoximes
Base silicon dibutyl tin, dibutyl tin diacetyl acetonate, ethyl diacetoacetate dibutyl tin, double triethoxy silicic acid dibutyl
The reaction product of tin, double triethoxy silicic acid dioctyl tins and diketone oximido tin oxide and silicate compound etc. tetravalent tin
Class compound；The divalent tin compounds such as tin octoate, aphthenic acids tin, stearic acid tin；Three sad Monobutyltins, three isopropoxies but
One of or several mixing of butyl tin etc. but butyl tin or single octyl tin compound or above-mentioned organotin.
Common titanate ester compound includes: tetra isopropyl titanate, tetra-n-butyl titanate esters, (two is pungent for isopropyl three
Base pyrophosphoric acid acyloxy) titanate esters, isopropyl three (dioctyl phosphoric acid acyloxy) titanate esters, two oleic acid acyloxy (two of isopropyl
Octylphosphonic acid acyloxy) titanate esters, single ketones oximido unsaturated fatty acid titanate esters, bis- (two octyloxy pyrophosphoric acid ester groups) ethylene titaniums
The chelate of acid esters and triethanolamine, Di(dioctylpyrophosphato) ethylene titanate, pyrophosphoric acid type single ketones oximido class titanium
Acid esters, two (octyl phenol polyoxyethylene ether) phosphides, tetra isopropyl two (dioctyl phosphito acyloxy) titanate esters or above-mentioned
One or more of mixing of compound etc..
Common α silane coupling agent includes: chloromethyl triethoxysilane, dichloromethyl triethoxysilane, diethylamino
Ylmethyl triethoxysilane, Diethylaminomethyl methyldiethoxysilane, second bis aminomethyl triethoxysilane, positive fourth
Amino methyl triethoxysilane, n-butylaminomethyl methyldiethoxysilane, two n-butylaminomethyl triethoxysilanes,
Own bis aminomethyl methyldiethoxysilane, hexamethylene diamine ylmethyl triethoxysilane, aminopropyltriethoxysilane triethoxysilane,
Aminopropyltriethoxysilane trimethoxy silane, aminopropyltriethoxysilane methyldiethoxysilane, acetoxyl group amino methyl triethoxysilicane
One or more of mixing of alkane, iso-cyanatomethyl triethoxysilane or above-mentioned coupling agent.
Common lewis acid compound includes: long chain fatty acids, alkyl benzene sulphonate, acid phosphatase esters compound, three
It is fluorinated diethyl etherate, boron trifluoride acetic acid complex compound, boron trifluoride tetrahydrofuran complex compound, boron trifluoride methanol complexing
Object, Boron Trifluoride Ethylamine complex compound, boron trifluoride acetonitrile complex compound, boron trifluoride-phenol complex, boron trifluoride are to methyl
Phenol complexes, boron trifluoride benzylamine complex compound, boron trifluoride methyl ether complex compound, boron trifluoride ether complex, boron trifluoride
One or more of carbonic acid dimethyl ester complex or corresponding Boron tribromide, triiodide boron complex or above compound
Mixing.Particularly preferred boron trifluoride etherate, Boron Trifluoride Ethylamine complex compound, boron trifluoride acetonitrile complex compound, trifluoro
Change the mixing of boron carbonic acid dimethyl ester complex one or more.
Common lewis base compound includes: propylamine, butylamine, amylamine, hexylamine, octylame, 2 ethyl hexylamine, nonyl amine, the last of the ten Heavenly stems
The primary amino-compounds such as amine, dodecyl amine, cetylamine, octadecylamine, cyclohexylamine；Diethylamine, di-n-propylamine, dibutyl amine, diamylamine,
The alkyl such as didecylamine, two (dodecyl amines), two (cetylamines), two (octadecylamines) replace secondary-amine compound；Triethylamine, three
The aliphatic tertiary amines class compound such as hexylamine, trioctylamine；The aromatic nitrile bases such as dodecyl polyaniline, octadecyl aniline, triphenylamine
Class compound；Ethanol amine, diethanol amine, triethanolamine, diethyl triamine, trientine, cyclohexylamine, benzyl amine, six methylenes
Base diamines, guanidine compound, Ma beautiful jade class compound, glyoxaline compound, 1,8- diazabicyclo (5,4,0) endecatylene -7
(DBU) etc. other cyclic annular or one or more of the aminated compounds with substituted functional group or above compound mixing.
The preferred organo-tin compound of moisture-curable catalyst of the invention or titanate ester compound.
Coating technique of the invention can be used blade coating, roller coating, slot coated (SLOT DIE), dropping curtain coating, bar coating,
The various modes such as silk-screen printing and automatically dropping glue, as long as can be uniformly coated on LCM.It can also be with gluing in cover-plate glass
It goes up then and LCM is vacuum abutted.
The test of light transmittance uses GB/T 2410-2008, is converted into 100 μm of light transmittances.
It is illustrated below with reference to specific example.
The present invention has moisture-curable, optically transparent organosilicon UV resin, and specific formula is as follows:
[example -1] polydimethylsiloxanes resin that viscosity is silicone terminated for the two butanone oximido of vinyl of 20000mPa.s
100 parts are added in planetary mixer, and 50 parts of methyl MQ resins are added, and 80 degree dissolve by heating 1.0 parts of sulfydryl silicone oil of addition later
(sulfhydryl content is 20wt% in sulfydryl silicone oil) stirs evenly.It is finally cooled to room temperature and 1.0 parts of ultraviolets initiations is added
Irgacure184,0.5 part of tetra-tert titanate esters, stirs 30min under vacuum conditions, is filled in 330mL silica gel bucket, so
Touch screen fitting experiment is carried out afterwards.
[attaching process] uniformly coats the optical clear resin of example -1 using slot coated mode on 20 inches of LCM,
For rubberised layer with a thickness of 200 μm, high voltage mercury lamp radiation energy is 1000mJ/cm2, irradiation finishes carries out cover-plate glass vacuum patch at once
It closes, this optical transparency resin adhesive layer shows pressure-sensitive character, and vacuum abutted cover-plate glass later will not generate displacement, Ke Yijin
Enter next processing procedure heating pressurization deaeration.The touch screen process -20 posted spends (30min), 60 degree of (30min) cooling thermal impacts
100 times, the high temperature and humidity of 60 degree of 95% relative humidity 240h is tested, and the removing with homemade jig detection four angles of touch screen is strong
Degree, the results are shown in Table -1.
The same example -1 of [example 2-5] preparation method, formula and physical property are shown in Table -1.
[comparative example 1] polydimethylsiloxanes resin that viscosity is silicone terminated for the two butanone oximido of vinyl of 20000mPa.s
100 parts are added in planetary mixer, and 30 parts of vinyl MQ resins are added, and 80 degree dissolve by heating 1.0 parts of sulfydryl silicon of addition later
Oil (sulfhydryl content is 20wt% in sulfydryl silicone oil) stirs evenly.It is finally cooled to room temperature and 1.0 parts of ultraviolets initiations is added
Irgacure184 does not add moisture-curable catalyst tetra-tert titanate esters, stirs 30min under vacuum conditions, be filled to
In 330mL silica gel bucket, touch screen fitting experiment is then carried out.
The same comparative example -1 of [comparative example 2-4] preparation method, formula and physical property are shown in Table -2.
Table -1
Table -2
Embodiment 1 uses viscosity for the silicone terminated dimethyl silicone polymer of two butanone oximido of vinyl, the MQ of 20000mPa.s
Resin, sulfydryl silicone oil, ultraviolet initiator Irgacure184 and tetra-tert titanate esters composition, apply on the touchscreen
Pressure-sensitive character is presented after glue UV irradiation, the peel strength average value at vacuum abutted rear four angles is 4.2N, although early strength
It is smaller, but after cooling thermal impact and high temperature and humidity experiment, moisture-curable is completed, therefore peel strength increases substantially,
Considerably beyond the peel strength specification value 15N of client.Although not listed in table -1, the touch screen that posts even without
Cooling thermal impact and high temperature and humidity experiment, it has been more than customer specifications that only room temperature 7 days, peel strength, which can also reach 30N,
The standard of value 15N.
Embodiment 2-5 using the silicone terminated dimethyl silicone polymers of vinyl butanone oximido of different viscosities, difference MQ resin,
Different sulfhydryl content silicone oil and different catalyst respectively obtain the organosilicon UV resin combination with moisture-curable.Using same
The vacuum abutted technique of sample, peel strength have been more than the specification value 15N of client.
As a comparison, comparative example 1-4 does not add moisture-curable catalyst, although the peel strength at initial stage is differed with embodiment
Less, but after cooling thermal impact and high temperature and humidity experiment, because not having moisture-curable characteristic, peel strength is not obtained
It is significantly promoted, does not reach minimum specification value 15N as defined in client.Simultaneously it has also been found that comparative example 2 and 4 does not add MQ
Resin, light transmittance reduce 3% or more than be accordingly added to MQ resin.
Claims (7)
1. touch screen fitting optics transparent resin, it is characterised in that: based on parts by weight, including 100 parts of vinyl ketone oximidos
Silicone terminated dimethyl silicone polymer, 5-100 parts of MQ resins, 0.1-20 parts of sulfydryl silicone oil, 0.1-2 parts of moisture-curable catalyst and 0.1-
2 parts of ultraviolet initiators；
Wherein, the MQ resin is made of tetra functional siloxane polycondensation chain link (Q) and single functionality siloxane unit (M)
Organic siliconresin, molal weight 1000-8000, M/Q ratio be 0.6-1.0, the MQ resin is methyl MQ resin
Or vinyl MQ resin.
2. touch screen fitting optics transparent resin according to claim 1, it is characterised in that: the vinyl ketoxime
The silicone terminated dimethyl silicone polymer of base has the following structure:
,
X1、X2、X3And X4Methyl, ethyl, any one group in butanone oximido are represented, n is the integer of 100-10000.
3. touch screen fitting optics transparent resin according to claim 2, it is characterised in that: X1、X2、X3、X4It is all fourth
Ketoxime base.
4. touch screen fitting optics transparent resin according to claim 1, it is characterised in that: by weight percentage,
Sulfhydryl content is 0.1-30wt% in the sulfydryl silicone oil.
5. touch screen fitting optics transparent resin according to claim 1, it is characterised in that: the ultraviolet draws
It sends out agent and is selected from 2- hydroxy-2-methyl -1- phenyl -1- acetone, 2,4,6- trimethylbenzoy-dipheny phosphine oxide, 2,4,6-
The mixture of tri-methyl benzophenone and 4- methyl benzophenone, benzoin dimethylether, benzophenone, 1- hydroxy-cyciohexyl benzene
One or more of mixing in ketone, α, α '-acetophenone or α-amine alkyl phenones.
6. touch screen fitting optics transparent resin according to claim 1, it is characterised in that: the moisture-curable touching
Matchmaker is to appoint in organo-tin compound, titanate ester compound, α-silane coupling agent, Louis's acids or Louis's alkaloid compound
Meaning is one or more of.
7. a kind of touch screen attaching process, it is characterised in that: use optical clear using touch screen as described in claim 1 fitting
Resin carries out gluing on the substrate for be coated with conductive film, then carries out ultraviolet light irradiation, and pressure-sensitive state is presented in optical clear resin,
Vacuum abutted cover-plate glass or film, fitting place in air after completing and carry out moisture-curable.
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| DE102017202624A1 (en) * | 2017-02-17 | 2018-08-23 | Tesa Se | Vibration-damping silicone pressure-sensitive adhesive |
| KR102606392B1 (en) * | 2017-06-30 | 2023-11-29 | 다우 실리콘즈 코포레이션 | Dual cure organopolysiloxane composition |
| CN108519833B (en) * | 2018-04-03 | 2024-03-15 | 京东方科技集团股份有限公司 | Touch display panel forming method and touch display motherboard |
| CN109517574B (en) * | 2018-10-24 | 2021-04-23 | 东莞市贝特利新材料有限公司 | Ultraviolet curing organic silicon liquid optical cement composition, preparation method and application thereof |
| TW202130738A (en) * | 2020-02-04 | 2021-08-16 | 美商陶氏有機矽公司 | High frequency silicone dampening gel |
| CN117402587B (en) * | 2023-12-15 | 2024-02-23 | 有行鲨鱼（上海）科技股份有限公司 | Photo-thermal dual-curing organic silicon liquid optical cement and preparation method thereof |
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