CN103044248A - Low-polymer cross-linking agent, preparation method thereof, insulation protection photoresist for manufacturing process of touch screen device and application thereof - Google Patents
Low-polymer cross-linking agent, preparation method thereof, insulation protection photoresist for manufacturing process of touch screen device and application thereof Download PDFInfo
- Publication number
- CN103044248A CN103044248A CN2012105279765A CN201210527976A CN103044248A CN 103044248 A CN103044248 A CN 103044248A CN 2012105279765 A CN2012105279765 A CN 2012105279765A CN 201210527976 A CN201210527976 A CN 201210527976A CN 103044248 A CN103044248 A CN 103044248A
- Authority
- CN
- China
- Prior art keywords
- linking agent
- touch screen
- photoresist
- insulation protection
- screen device
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 0 C*=*[N+]([O-])SC Chemical compound C*=*[N+]([O-])SC 0.000 description 2
Images
Landscapes
- Materials For Photolithography (AREA)
Abstract
The invention discloses a low-polymer cross-linking agent, a preparation method thereof, an insulation protection photoresist for the manufacturing process of a touch screen device and application thereof. The low-polymer cross-linking agent is prepared by condensation and condensation between pentaerythritol triacrylate or dipentaerythritol pentaacrylate and one of cyclic hydrocarbon group carboxylic acid, cyclic hydrocarbon group anhydride and cyclic hydrocarbon group carboxylate of C5-C30 saturated C atoms, or one of aryl carboxylic acid, aryl anhydride and aryl carboxylate of C7-C20, or one of terminal group siloxane-containing carboxylic acid, terminal group acyl chloride, terminal group acylamino and terminal group nitrile. The insulation protection photoresist obtained by adding the low-polymer cross-linking agent to an insulation protection photoresist formula has the advantages of good flowability, high transmittance and easiness in coating, the heat-resisting light transmittance of a pixel or protective layer is higher than 94%, the heat-resisting temperature is higher than 260 DEG C and the resistance valve of surface resistivity is within a range of 5.0 E+15-16 ohms and good electrical insulation property is achieved.
Description
Technical field
The present invention relates to photoresist and relative linking agent Material Field, be specifically related to a kind of oligopolymer linking agent and preparation method thereof and touch screen device processing procedure insulation protection photoresist and application.The insulation protection photoresist that namely will contain the oligopolymer linking agent by the gold-tinted processing procedure is applied on the touch screen device.
Background technology
The mainstream technology in touch-screen market just is transitioned into condenser type from resistance-type at present, and replacement velocity is more and more faster.Show (2012) according to the DisplaySearch statistic data, capacitive touch screen will occupy 52% of whole market, resistive touch screen with under slide into about 44%.Compare with touch screens, capacitance plate is in the advantage that possesses skills aspect response speed and the accuracy, faster response speed and better accuracy are arranged, the what is more important capacitance plate can be realized multi-point touch, realize more operation, promote client's operating experience, capacitive touch screen is replaced resistive touch screen has become trend.
Capacitive touch screen can be divided into surface-type and projection type.The surface-type capacitance touch screen is the five-line electric resistance touch screen of mutation, and performance is without obvious lifting, and projection-type capacitive touch screen has then effectively overcome short, the shortcoming such as transmittance is low, energy consumption is high in resistive touch screen work-ing life, and performance boost is remarkable.Therefore the projection-type capacitive touch screen technology becomes the main flow in the capacitive touch screen technology, and has accelerated the replacement of capacitive touch screen to resistive touch screen.
Projecting type capacitor panel plate generally places the transparency carrier below, and protection is good, can touch operation by finger or special pen, even also can operate the projecting type capacitor screen with gloves.The projecting type capacitor screen can bear more than one hundred million times click, is longer than touch screens work-ing life.In addition, the projecting type capacitor screen does not have the clearance, by simple optical design, transmittance can be brought up to 90%.Compare with the surface-type capacitance plate, the projecting type capacitor screen is simple in structure, need not manual synchronizing, also can not produce drift phenomenon.The projecting type capacitor screen adopts matrix structure, and tolerance range is high, can realize multiple point touching.
Projecting type capacitor screen is divided into Flim structure and Glass structure two large classes according to the Sensor material, compare with the Flim structure Glass structure capacitive shield have long service life, transmittance advantages of higher and being paid attention to by most manufacturer.Glass structure capacitive screen can be further divided into two plane type (DITO) and one plane type (SITO) two large classes according to the distributing position of electrode.Two plane type capacitance plate X, Y electrode lay respectively at glass substrate both sides face.
That one plane type or two plane type structure all must be used a kind of be coated with and photoetching development becomes the transparent photoresist of figure-OC negative light resistance agent in the middle of the gold-tinted making technology, realize that wherein but the exposure imaging major ingredient except alkali soluble resins, is exactly linking agent.Known linking agent is to use Viscoat 295, pentaerythritol triacrylate, tetramethylol methane tetraacrylate, tetramethylolmethane five acrylate or tetramethylolmethane six acrylate or their mixture.In fact because can't separate, what mostly use is mixture.Up to the present, aforesaid method is being obtained more effective result aspect linking agent.
But, in order to pursue small figure adherence and heat-resistant stability, many times the lithographic accuracy of this negative light resistance agent goes wrong owing to crosslinked adherence is not enough, when final result is reflected in the spectral filter of making, glue appears falling in the place that resin residue is arranged around the pixel graphics or should not fall glue, and then causes electrical insulating property to descend.Major cause is that existing linking agent resistance toheat is not good, in the high-temperature process of back segment, the time oxidation Yellowing is arranged, cause transmitance to quickly fall to below 90% from 96%, affect the backlight efficient of device or even whole screen.
In order to address these problems, there is method to propose to regulate the hardness of the central alkali soluble resins of prescription, namely improve molecular weight of polymers.But, if excessively increase molecular weight (M.w), the polarities match degree can not be unified between the component, following point will occur: the positive negative value of the edge section of the pixel cell that forms on the substrate (CD Loss) engrail, surface irregularity or angle section poor (Slope) is higher.
The thinking that another kind addresses the above problem is to control technique so that make temperature reduction or high temperature as far as possible
Operating time shortens.But this control has its limit, can not really solve the problem of the crosslinked adherence deficiency of lithographic accuracy of negative light resistance agent.
Summary of the invention
In order to overcome the deficiencies in the prior art, the object of the present invention is to provide a kind of oligopolymer linking agent, so that the terminal hydroxy group esterification of linking agent function monomer becomes other groups to carry out " end socket ", improve its resistance toheat.
Another object of the present invention is to provide a kind of preparation method of oligopolymer linking agent, for the preparation of oligopolymer linking agent of the present invention.
Another purpose of the present invention is to provide a kind of touch screen device processing procedure insulation protection photoresist that contains oligopolymer linking agent of the present invention, so that photoresist has good dispersiveness and mobile, satisfy simultaneously to put down being coated with large-size device requirement in (Slit) making, and the controlled touch screen device of pattern of the pixel of making; Realize high permeability, be fit to multiple coating process construction, have the characteristics such as pixel cell precision raising of satisfactory stability and making.
The 4th purpose of the present invention is to provide a kind of and utilizes insulation protection photoresist of the present invention to prepare the method for insulative bridge, to obtain a kind of good insulating, transmittance height and the high insulative bridge of heat-resisting transmittance.
The 5th purpose of the present invention is to provide a kind of insulative bridge with good insulation properties, high transmission rate and heat-resisting transmittance.
The 6th purpose of the present invention is to provide a kind of protective layer with good insulation properties, high transmission rate and heat-resisting transmittance and preparation method thereof.
For addressing the above problem, the technical solution adopted in the present invention is as follows:
A kind of oligopolymer linking agent is characterized in that it is to be formed by raw material A and R polycondensation, A pentaerythritol triacrylate wherein, and structural formula is (1); Perhaps double pentaerythritol C5 methacrylate, structural formula is (2);
Wherein, R is a kind of in the saturated C atom cyclic hydrocarbon radical carboxylic acid, acid anhydrides, carboxylate salt of C5～C30; Or a kind of in the aryl carboxylic acid of C7～C20, aryl acid anhydrides, aryl carboxylic acid salt; Perhaps a kind of in the carboxylic acid of terminal group silicone-containing, acyl chlorides, amide group, the nitrile; Raw material A is (1:4)～(1:10) with the ratio of the amount of substance of R, and the viscosity of described linking agent is 50-60cp.
R selects to contain the compound of siloxy, aryl, amino groups among the present invention, because siloxy, aryl, amino etc. and central other composition highly compatibles of prescription, so that the dispersiveness of photoresist and mobile having concurrently good the time, satisfy to put down being coated with large-size device requirement in (Slit) making, and the pattern of the pixel of making is controlled.Wherein, R of the present invention specifically can be selected from a kind of in the following compounds:
A kind of preparation method of oligopolymer linking agent may further comprise the steps:
1) High Temperature Pre reaction: under the gold-tinted environment, the compound of the compound of described structural formula (1) or structural formula (2) and compound, catalyzer, dehydration agent, hot stopper and the solvent that R represents are added in the reactor, be communicated with nitrogen, under nitrogen atmosphere, react, wherein catalyzer divides and joins in the reactor for three times, react in the water-bath of high temperature under stirring, afterwards underpressure distillation is except by product;
2) low-temp reaction: reduce bath temperature, with the product of High Temperature Pre reaction in the continuous reaction of low temperature water-bath relaying, after reaction finishes, the underpressure distillation product, to product washing, neutralization, drying, after the pure water washing again fractionation obtain product.
Among the above-mentioned preparation method, described catalyzer is one or more mixing among sulfuric acid, hydrochloric acid, phosphoric acid, phosphorous acid, F3CCOOH, tosic acid, iron trichloride, aluminum chloride, sal enixum, tetrabutyl titanate, aluminum oxide, silicon-dioxide, dicyclohexylcarbodiimide, Si Lv Aluminum ether complexes, acidic cation-exchange resin and pyridine, xylidine, the DMAP etc., ethylene linkage in raw material reacts, and preferred described catalyzer adopts a kind of in the organic basess such as pyridine, xylidine or DMAP; Described solvent is one or more mixing of ethyl acetate, propylene glycol monomethyl ether, propylene glycol methyl ether acetate, pimelinketone, n-Butyl lactate, dipropylene glycol methyl ether and 3-ethoxyl ethyl propionate etc., the dehydration agent that the present invention adopts is the DCC(dicyclohexylcarbodiimide) or the DBU(diazabicylo), hot stopper is Resorcinol.
The temperature of high temperature bath is 80-100 ℃ in the step 1), and stirring velocity is 70-90rpm, and the reaction times is 2.5-3.5 hour, underpressure distillation 0.4-0.6 hour.
Step 2) temperature of low temperature water-bath is 50-60 ℃ in, and the time of continuing reaction is 6-10 hour, adopts 5% NaCl washing, the dilute hydrochloric acid neutralization.
A kind of touch screen device processing procedure insulation protection photoresist, it is prepared from by the following component in weight part:
The viscosity of described photoresist is 2-10cp.
The structural formula of above-mentioned organosiloxane polymer is as follows:
In the described general formula (1), X represents the Ar base, and Y represents the Ar base; R
1Expression straight chain or graft copolymer; R
2The expression alkylene, contain the N alkyl, contain a kind of in O alkyl or the halogen atom alkyl; R
3Expression hydrogen or methyl; R
4Expression methyl or ethyl; The n value is 5～300.Specifically can be selected from application number and be in 201210070934.3 the patent application a kind of in the resulting organosiloxane polymer of embodiment 1-6.
The structural formula of above-mentioned cyclohexyl copolymerized macromolecule resin is as follows:
Its weight-average molecular weight is 8000-20000, and wherein Y is Si or C atom; Z is the cyclohexyl formate base; R
1Be saturated C atom straight chain hydrocarbon or carboxyl; R
2Be unsaturated aromatic hydrocarbon base or carboxyl; R
3With R
4, R
5Be identical group or different group, all be selected from a kind of in hydrogen atom or the alkoxyl group.Specifically can be selected from application number and be in 201210174131.32 the patent application a kind of in the resulting cyclohexyl copolymerized macromolecule of the embodiment 1-6 resin.
Described initiator is 2,4-trichloromethyl (4 '-p-methoxy-phenyl)-6-triazine, 2,4-trichloromethyl-(4 '-methoxyl-styrene)-6-triazine, 2,2 '-two (2-chloro-phenyl-s) 4,4', 5, the 2 – hydroxy-2-methyl in 5 '-tetraphenyl bisglyoxaline, the second phthalein benzene compound-1-phenyl-propane-l-ketone (Irgacure-369), 2-methyl-(4-methylbenzene sulfenyl)-2-beautiful jade-l-propane-1-ketone (Irgacure-907) and 2-phenmethyl-2-dimethylamino-1-(4-beautiful jade phenyl)-a kind of in butane-l-ketone etc.
Above-mentioned solvent is a kind of in methylethylketone, ethyl cellosolve, glycol dimethyl ether, ethylene glycol diethyl ether, Propylene Glycol Dimethyl Ether, diethylene glycol dimethyl ether, 2-oxyethyl group propyl alcohol, 2-methoxypropanol, 3-methoxybutanol, pimelinketone, cyclopentanone, propylene glycol methyl ether acetate, propylene-glycol ethyl ether acetic ester, the butylacetate etc.
Utilize insulation protection photoresist of the present invention to prepare the insulative bridge method, it may further comprise the steps in turn:
1) coating: at substrate coating insulation protection photoresist of the present invention, form the figure of 1-3 μ m on the surface of substrate;
2) front baking: under the substrate after the coating and 60-140 ℃ the temperature, baking 100-140s;
3) exposure: exposure energy 40-200mj/cm
2, the Gap value is 50-200um;
4) develop: under the undisguise template, shadow liquid consumption is 0.25-0.5Kg/cm
2, development 30-90S;
5) baking after: 210-260 degree centigrade, baking 25-60min.
Above-mentioned steps 1) adopts this area coating process commonly used in, specifically can adopt spin, slit, a kind of in the coating processes such as slit+spin.
A kind of insulative bridge comprises substrate and forms the pixel of 1-3 μ m at substrate coating photoresist claimed in claim 6; Described pixel profile is changed between 20 °-40 °; The resistance value of the electrical insulating property of pixel is in 5.0E+15 ~ 16 ohm, and transmittance is more than 97%, and heat-resisting transmittance is more than 94%.
Above-mentioned substrate adopts glass substrate, organic transparent substrates such as PC, PET, a kind of in flexible substrate or the ITO electrode layer.
A kind of protective layer is used for the touch screen device outermost layer, is coated with the protective layer of the 1-3um that photoresist of the present invention forms at the touch screen device outermost layer, and the transmittance of described protective layer is more than 98%.
A kind of making method of protective layer, it may further comprise the steps in turn:
1) coating: at touch screen device coating insulation protection photoresist claimed in claim 5, form the protective layer of 1-3 μ m on the surface of touch screen device;
2) front baking: the touch screen device after the coating dries by the fire 100-140s under 60-140 ℃ temperature;
3) exposure: exposure energy 40-200mj/cm
2, the Gap value is 50-200um;
4) baking after: 210-260 degree centigrade, baking 25-60min.
Compared to existing technology; beneficial effect of the present invention is: oligopolymer linking agent of the present invention joins in the insulation protection photoresist; the photoresist that obtains has good flowability and high permeability; be easy to coating; the heat-resisting transmittance of protective layer can reach more than 94% after the coating; heat resisting temperature can reach more than 260 ℃, and the resistance of protective layer resistivity demonstrates good electrical insulating property in 5.0E+15 ~ 16 ohm scope.In addition, the adherence (reservation of 20um width Marker lines) that the pixel lines after the photoengraving that the application of the invention is made develops can be good, the Profile of pixel can be controlled between 20 °-40 ° simultaneously.And photoresist layer dig a hole and the anti-Performance Detection such as ultrasonic under pattern still keep good.
Below in conjunction with the drawings and specific embodiments the present invention is described in further detail.
Description of drawings
Fig. 1 represents to adopt the situation of pixel adherence zero in the middle of the insulation protection of embodiment 7-12 insulation photoresist, and Masker design line thickness is 4um, because the cause of gap and exposure energy, developed width shows among the figure and all adheres in the 20um scope;
Fig. 2 digs a hole under exposure imaging technique the situation of precision and adherence zero in the middle of representing to adopt the insulation protection of embodiment 7-12 insulation photoresist;
The insulating protective layer that Fig. 3 represents to adopt Comparative Examples 1 insulation photoresist is anti-when ultrasonic ● situation;
The insulating protective layer that Fig. 4 and Fig. 5 represent to adopt embodiment 7-12 insulation photoresist is in anti-zero situation when ultrasonic;
Fig. 6 is the electromicroscopic photograph of the insulation protection Profile of employing embodiment 7-12 insulation photoresist;
Fig. 7 for plating ITO on the insulating protective layer that adopts Comparative Examples 1 insulation photoresist after the pattern of insulative bridge during the situation of line resistance △;
Fig. 8 for plating ITO on the insulation layer of the insulation photoresist that adopts embodiment 7-12 after the pattern of insulative bridge during the situation of line resistance zero;
Fig. 9 represents to adopt the transmittance curve situation of all examples in the middle of the insulation protection of embodiment 7-12 insulation photoresist: more than 97%;
Figure 10 represents the heat-resisting transmittance curve of Comparative Examples 1, and some is reduced on 88%.
Embodiment
Below be specific embodiment of the present invention, wherein " part " represents weight part.
Embodiment 1
Under the gold-tinted environment, get 2.34 parts of substrate pentaerythritol triacrylates, and 7.25 parts of the compounds of said structure formula (1-8) expression, 3 parts of pyridines, 0.00005 part of Resorcinol, DCC0.001 part, 20 parts of 3-ethoxyl ethyl propionates; The above-mentioned raw materials adding is equipped with in the there-necked flask of water trap, and pyridine divides three interpolations, and is each a, puts into magneton and thermometer; Be communicated with nitrogen, reaction is 3 hours in the 80rpm stirring velocity access 80 degree water-baths, and underpressure distillation removed by product in 0.5 hour; Water-bath is cooled to 60 degree, continues reaction 8 hours, finishes reaction, and the underpressure distillation product uses the 5%NaCl washing, in the dilute hydrochloric acid and after use again salt of wormwood dry, after the pure water washing again fractionation obtain product, be numbered 1.
Embodiment 2
Under the gold-tinted environment, get 2.34 parts of substrate pentaerythritol triacrylates, and 6.82 parts of the compounds of said structure formula (1-6) expression, 0.9 a part DMAP(divides three addings, adds 0.3 part at every turn), 0.00005 part of Resorcinol, DCC0.001 part, 20 parts of 3-ethoxyl ethyl propionates; Add and be equipped with in the there-necked flask of water trap, put into magneton, thermometer; Be communicated with nitrogen, reaction is 3 hours in the 80rpm stirring velocity access 70 degree water-baths, and underpressure distillation removed by product in 0.5 hour; Water-bath is cooled to 60 degree, continues reaction 8 hours, finishes reaction; The underpressure distillation product uses the 5%NaCl washing, in the dilute hydrochloric acid and after use again salt of wormwood dry, after the pure water washing again fractionation obtain product, be numbered 2.
Embodiment 3
Under the gold-tinted environment, get 2.34 parts of substrate pentaerythritol triacrylates, and 8.48 parts of the compounds of said structure formula (1-7) expression, 1.5 a part DMAP(divides three addings, each 0.5 part), 0.00005 part of Resorcinol, DCC0.001 part, 20 parts of 3-ethoxyl ethyl propionates; Add and be equipped with in the there-necked flask of water trap, put into magneton, thermometer; Be communicated with nitrogen, reaction is 3 hours in the 80rpm stirring velocity access 100 degree oil baths, and underpressure distillation removed by product in 0.5 hour; Water-bath is cooled to 60 degree, continues reaction 8 hours, finishes reaction.The underpressure distillation product uses the 5%NaCl washing, in the dilute hydrochloric acid and after use again salt of wormwood dry, pure water washs again that fractionation obtains product, is numbered 3.
Embodiment 4
Under the gold-tinted environment, get 2.68 parts of substrate double pentaerythritol C5 methacrylates, and 7.25 parts of the compounds of said structure formula (1-8) expression, 3 parts of pyridines, 0.00005 part of Resorcinol, DBU0.001 part, 20 parts of 3-ethoxyl ethyl propionates; Add and be equipped with in the there-necked flask of water trap.Put into magneton, thermometer; Be communicated with nitrogen.Reaction is 3 hours in the 80rpm stirring velocity access 80 degree water-baths, and underpressure distillation removed by product in 0.5 hour.Be cooled to 60 degree, continue reaction 8 hours, finish reaction.The underpressure distillation product uses the 5%NaCl washing, in the dilute hydrochloric acid and after use again salt of wormwood dry, after the pure water washing again fractionation obtain product, be numbered 4.
Embodiment 5
Under the gold-tinted environment, get 2.68 parts of substrate double pentaerythritol C5 methacrylates, and 6.25 parts of the compounds of said structure formula (1-23) expression, 1.5 a part DMAP(divides three addings, each 0.5 part), 0.00005 part of Resorcinol, DCC0.001 part, 20 parts of 3-ethoxyl ethyl propionates; Add and be equipped with in the there-necked flask of water trap, put into magneton, thermometer; Be communicated with nitrogen.Reaction is 3 hours in the 80rpm stirring velocity access 90 degree water-baths, and underpressure distillation removed by product in 0.5 hour; Water-bath is cooled to 60 degree, continues reaction 8 hours, finishes reaction, and the underpressure distillation product uses the 5%NaCl washing, in the dilute hydrochloric acid and after use again salt of wormwood dry, after the pure water washing again fractionation obtain product, numbering 5.
Embodiment 6
Under the gold-tinted environment, get 2.68 parts of substrate double pentaerythritol C5 methacrylates, and 7.25 parts of the compounds that represent of said structure formula 1-7,1.5 parts of DMAP(divide three addings), 0.00005 part of Resorcinol, DCC0.001 part, 20 parts of 3-ethoxyl ethyl propionates; Add and be equipped with in the there-necked flask of water trap.Put into magneton, thermometer; Be communicated with nitrogen.Reaction is 3 hours in the 80rpm stirring velocity access 90 degree water-baths, and underpressure distillation removed by product in 0.5 hour; Water-bath is cooled to 60 degree, continues reaction 8 hours, finishes reaction, and the underpressure distillation product uses the 5%NaCl washing, in the dilute hydrochloric acid and after use again salt of wormwood dry, after the pure water washing again fractionation obtain product, be numbered 6.
Embodiment 7-12
A kind of touch screen device processing procedure insulation protection photoresist, it is prepared from by the following component in weight part:
The viscosity of described photoresist is 2-10cp.
Wherein the oligopolymer linking agent is the product that is numbered 1-6 in above-described embodiment, it is the organosiloxane polymer among the embodiment 2 in 201210070934.3 patent applications that organosiloxane polymer is selected application number, and cyclohexyl copolymerized macromolecule resin is selected the cyclohexyl copolymerized macromolecule resin of embodiment 4 in 201210174131.32 the patent application.In addition, adopt the DPHA(double pentaerythritol methacrylate) join in the above-mentioned prescription as a comparison case 1 as linking agent.Component and consumption concrete in embodiment 7-12 and the Comparative Examples 1 see Table 1.
Table 1: embodiment 7-12
Utilize respectively the insulation protection photoresist in above-described embodiment 7-12 and the Comparative Examples 1 to prepare the insulative bridge method, it may further comprise the steps in turn:
1) coating: at substrate coating insulation protection photoresist of the present invention, form the figure of 1-3 μ m on the surface of substrate;
2) front baking: under the substrate after the coating and 60-140 ℃ the temperature, baking 100-140s;
3) exposure: exposure energy 40-200mj/cm
2, the Gap value is 50-200um;
4) develop: under the undisguise template, shadow liquid consumption is 0.25-0.5Kg/cm
2, development 30-90S;
5) baking after: 210-260 degree centigrade, baking 25-60min.
Wherein, adherence is used under the Nikon microscope x20 condition and is observed; Electrical insulating property is the surface resistivity under 100K HZ test condition; Heat-resisting transmittance is the 400nm place transmittance under the test condition that 300 ℃/15min does not vacuumize; Anti-excusing from death is in 40 ℃/30mins ultrasonic frequency: the adherence under the test condition of 40KHZ/ power: 360W; The test of Profile is that the tangent value calculating according to thickness and gradient projection gets under Nikon microscope x50 dark-field; The results are shown in following table 2.
Table 2:
| Embodiment | Linking agent | Adherence | Electrical insulating property | Heat-resisting transmitance | Anti-ultrasonic | Profile |
| 7 | 1 | △ | △ | 91% | △ | ○ |
| 8 | 2 | ○ | ○ | 90% | △ | ○ |
| 9 | 3 | △ | ○ | 94% | ○ | ○ |
| 10 | 4 | ○ | ○ | 93% | ○ | ○ |
| 11 | 5 | ○ | ○ | 94% | ○ | ○ |
| 12 | 6 | ○ | ○ | 93% | ○ | ○ |
| Comparative Examples 1 | DPHA | ● | △ | 88% | ● | ○ |
Annotate:
Adherence: ● expression 30um width (actual measurement) pixel lines have and come off; △ represents that 30um width (actual measurement) pixel lines do not come off, but line edge has damage; Zero expression 30um width (actual measurement) pixel and line edge all do not damage;
Electrical insulating property: △ represents wired resistance drift; Zero expression resistance value is in 5.0E+15 ~ 16 ohm;
Anti-ultrasonic: ● represent that hundred lattice cutter cut place big area come off; △ represents that hundred lattice cutter cut places come off once in a while; Zero expression, hundred lattice cutter cut places do not come off;
Profile: the zero expression gradient is in 20 ~ 40 degree angular regions.
Above-mentioned embodiment only is preferred implementation of the present invention; can not limit the scope of protection of the invention with this, the variation of any unsubstantiality that those skilled in the art does on basis of the present invention and replacement all belong to the present invention's scope required for protection.
Claims (10)
1. an oligopolymer linking agent is characterized in that it is to be formed by raw material A and R polycondensation, and wherein A is pentaerythritol triacrylate, and structural formula is (1); Perhaps double pentaerythritol C5 methacrylate, structural formula is (2);
Wherein, R is a kind of in the saturated C atom cyclic hydrocarbon radical carboxylic acid, acid anhydrides, carboxylate salt of C5～C30; Perhaps a kind of in C7～C20 aryl carboxylic acid, aryl acid anhydrides, the aryl carboxylic acid salt; Perhaps a kind of in the carboxylic acid of terminal group silicone-containing, acyl chlorides, amide group, the nitrile; The molar ratio of raw material A and R is (1:4)～(1:10), and the viscosity of described linking agent is 50-60cp.
2. the preparation method of an oligopolymer linking agent is characterized in that may further comprise the steps:
1) High Temperature Pre reaction: under the gold-tinted environment, the compound of the compound of structural formula claimed in claim 1 (1) or structural formula (2) and compound, catalyzer, dehydration agent, hot stopper and the solvent that R represents are added in the reactor, be communicated with nitrogen, under nitrogen atmosphere, react, wherein catalyzer divides and joins in the reactor for three times, react in the water-bath of high temperature under stirring, afterwards underpressure distillation is except by product
2) low-temp reaction: reduce bath temperature, with the product of High Temperature Pre reaction in the continuous reaction of low temperature water-bath relaying, after reaction finishes, the underpressure distillation product, to product washing, neutralization, drying, after the pure water washing again fractionation obtain product.
3. the preparation method of oligopolymer linking agent according to claim 2, it is characterized in that: the temperature of high temperature bath is 80-100 ℃ in the step 1), and stirring velocity is 70-90rpm, and the reaction times is 2.5-3.5 hour, underpressure distillation 0.4-0.6 hour.
4. the preparation method of oligopolymer linking agent according to claim 2 is characterized in that: step 2) in the temperature of low temperature water-bath be 50-60 ℃, the time of continuing reaction is 6-10 hour, adopts 5% NaCl washing, the dilute hydrochloric acid neutralization.
5. touch screen device processing procedure insulation protection photoresist, it is characterized in that: it is prepared from by the following component in weight part:
6. touch screen device processing procedure insulation protection photoresist according to claim 5, it is characterized in that: the viscosity of described photoresist is 2-10cp.
7. utilize insulation protection photoresist claimed in claim 5 to prepare the insulative bridge method, it is characterized in that it may further comprise the steps in turn:
1) coating: at substrate coating insulation protection photoresist claimed in claim 5, form the figure of 1-3 μ m on the surface of substrate;
2) front baking: the substrate after the coating dries by the fire 100-140s under 60-140 ℃ temperature;
3) exposure: exposure energy 40-200mj/cm
2, the Gap value is 50-200um;
4) develop: shadow liquid consumption is 0.25-0.5Kg/cm
2, development 30-90S;
5) baking after: 210-260 degree centigrade, baking 25-60min.
8. insulative bridge is characterized in that: the pixel that it comprises substrate and forms 1-3 μ m at substrate coating photoresist claimed in claim 6, and described pixel profile is changed between 20 °-40 °; The resistance value of the electrical insulating property of pixel is in 5.0E+15 ~ 16 ohm, and transmittance is more than 97%, and heat-resisting transmittance is more than 94%.
9. protective layer is characterized in that: be coated with the protective layer of the 1-3um that photoresist claimed in claim 6 forms at the touch screen device outermost layer, the transmittance of described protective layer is more than 98%.
10. the making method of a protective layer is characterized in that it may further comprise the steps in turn:
1) coating: at touch screen device coating insulation protection photoresist claimed in claim 5, form the protective layer of 1-3 μ m on the surface of touch screen device;
2) front baking: the touch screen device after the coating dries by the fire 100-140s under 60-140 ℃ temperature;
3) exposure: exposure energy 40-200mj/cm
2, the Gap value is 50-200um;
4) baking after: 210-260 degree centigrade, baking 25-60min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012105279765A CN103044248A (en) | 2012-12-10 | 2012-12-10 | Low-polymer cross-linking agent, preparation method thereof, insulation protection photoresist for manufacturing process of touch screen device and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012105279765A CN103044248A (en) | 2012-12-10 | 2012-12-10 | Low-polymer cross-linking agent, preparation method thereof, insulation protection photoresist for manufacturing process of touch screen device and application thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103044248A true CN103044248A (en) | 2013-04-17 |
Family
ID=48057136
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2012105279765A Pending CN103044248A (en) | 2012-12-10 | 2012-12-10 | Low-polymer cross-linking agent, preparation method thereof, insulation protection photoresist for manufacturing process of touch screen device and application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103044248A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103760751A (en) * | 2013-12-20 | 2014-04-30 | 深圳市查科本显示材料有限公司 | High-temperature yellowing resistant and high-temperature high-humidity resistant OC negative photoresist and process method thereof in manufacturing of touch screen device |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1892573A1 (en) * | 2006-08-22 | 2008-02-27 | FUJIFILM Corporation | Photopolymerizable composition comprising fine particles of organic pigment |
| CN102702431A (en) * | 2012-05-30 | 2012-10-03 | 深圳市惠乐光电有限公司 | Cyclohexyl copolymer resin and preparation method thereof as well as color photoresist and preparation method thereof |
| CN103149799A (en) * | 2011-12-07 | 2013-06-12 | 三菱化学株式会社 | Colored resin composition, color filter, liquid crystal display and organic el display device |
-
2012
- 2012-12-10 CN CN2012105279765A patent/CN103044248A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1892573A1 (en) * | 2006-08-22 | 2008-02-27 | FUJIFILM Corporation | Photopolymerizable composition comprising fine particles of organic pigment |
| CN103149799A (en) * | 2011-12-07 | 2013-06-12 | 三菱化学株式会社 | Colored resin composition, color filter, liquid crystal display and organic el display device |
| CN102702431A (en) * | 2012-05-30 | 2012-10-03 | 深圳市惠乐光电有限公司 | Cyclohexyl copolymer resin and preparation method thereof as well as color photoresist and preparation method thereof |
Non-Patent Citations (3)
| Title |
|---|
| CAS: "107481-55-0", 《STN-REGISTRY》 * |
| CAS: "139218-59-0", 《STN-REGISTRY》 * |
| CAS: "67326-46-9", 《STN-REGISTRY》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103760751A (en) * | 2013-12-20 | 2014-04-30 | 深圳市查科本显示材料有限公司 | High-temperature yellowing resistant and high-temperature high-humidity resistant OC negative photoresist and process method thereof in manufacturing of touch screen device |
| CN103760751B (en) * | 2013-12-20 | 2018-05-25 | 深圳市查科本显示材料有限公司 | High-temperature yellowing resistant and high-temperature high-humidity resistant OC negative photoresist and process method thereof in manufacturing of touch screen device |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103443750B (en) | Coating composition for touch panels, coating film, and touch panel | |
| TWI696888B (en) | Photosensitive resin composition for touch panel, cured film using the same, and touch panel including such cured film as a component | |
| CN102736764B (en) | Contact panel and manufacture method thereof | |
| CN103988154B (en) | The forming method of resin solidification film figure, photosensitive polymer combination, photosensitive element, the manufacture method of touch panel and resin cured film | |
| CN103612456B (en) | A kind of antistatic scratching-resistingprotective protective film and preparation method thereof | |
| CN101465173B (en) | Touch screen transparent conductive film and preparation method thereof | |
| CN104699309A (en) | Touch screen, manufacturing method thereof and display device | |
| CN104795131B (en) | Transparent conductor and touch panel | |
| KR101475780B1 (en) | Organic-inorganic complex resin composition which is useful as a protecting layer | |
| TWI401272B (en) | A resin composition, a method for forming a protective film of a color filter, and a color filter protective film | |
| CN104054042B (en) | The diaphragm and touch panel of touch panel electrode | |
| CN104040644A (en) | Transparent electroconductive film | |
| KR20140009193A (en) | Touch panel | |
| TWI590001B (en) | Touch panel, radiation-sensitive resin composition and cured film | |
| CN107705883A (en) | Transparency electrode including its touch sensor and image display | |
| CN104199580A (en) | Touch screen, manufacturing method of touch screen and touch display device | |
| CN102053493A (en) | Radiation-sensitive composition, protective film and inter layer insulating film, and method for forming the same | |
| CN108351722A (en) | Film touch sensing | |
| JPWO2007135909A1 (en) | Thermosetting resin composition and cured product thereof | |
| CN103044248A (en) | Low-polymer cross-linking agent, preparation method thereof, insulation protection photoresist for manufacturing process of touch screen device and application thereof | |
| CN103760751A (en) | High-temperature yellowing resistant and high-temperature high-humidity resistant OC negative photoresist and process method thereof in manufacturing of touch screen device | |
| CN106066731A (en) | A kind of touch-control display panel and preparation method thereof, touch control display apparatus | |
| CN104182067B (en) | A kind of contact panel and its manufacture method | |
| CN104820324A (en) | Liquid crystal display component and radiation-sensitive resin composition | |
| CN104850266A (en) | Touch display panel, method for manufacturing same and display device |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C12 | Rejection of a patent application after its publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20130417 |