CN107384282A - A kind of flexible electronic substrate adhesive and its preparation method and application - Google Patents
A kind of flexible electronic substrate adhesive and its preparation method and application Download PDFInfo
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- CN107384282A CN107384282A CN201710652649.5A CN201710652649A CN107384282A CN 107384282 A CN107384282 A CN 107384282A CN 201710652649 A CN201710652649 A CN 201710652649A CN 107384282 A CN107384282 A CN 107384282A
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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
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
- C09J163/10—Epoxy resins modified by unsaturated compounds
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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
- C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
- C09J175/04—Polyurethanes
- C09J175/14—Polyurethanes having carbon-to-carbon unsaturated bonds
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/67—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere
- H01L21/683—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere for supporting or gripping
- H01L21/6835—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere for supporting or gripping using temporarily an auxiliary support
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- 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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2221/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof covered by H01L21/00
- H01L2221/67—Apparatus for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components; Apparatus not specifically provided for elsewhere
- H01L2221/683—Apparatus for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components; Apparatus not specifically provided for elsewhere for supporting or gripping
- H01L2221/68304—Apparatus for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components; Apparatus not specifically provided for elsewhere for supporting or gripping using temporarily an auxiliary support
- H01L2221/68381—Details of chemical or physical process used for separating the auxiliary support from a device or wafer
- H01L2221/68386—Separation by peeling
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Abstract
The invention discloses a kind of flexible electronic substrate adhesive and preparation method thereof, each component is mixed by following weight parts：100 parts of modified acrylic ester resin, 10 100 parts of epoxy resin, 1 10 parts of light trigger, 8 15 parts of reactive diluent, 1 15 parts of thermal curing agents.The invention also discloses application of the above-mentioned adhesive in flexible electronic substrate processing procedure.The advantages of BDB adhesive produced by the present invention combines epoxy resin and acrylate, solve the problems, such as common adhesives it is not peelable or peel off after a large amount of culls, have the characteristics that to be firmly combined with glass and flexiplast electronic substrate, be easily peeled off, residual silkgum content is few, safety and environmental protection, easy for construction, alternative traditional not peelable type adhesive, in the preparation for the electronic equipment flexible display screen such as tablet personal computer, mobile phone, kindle.
Description
Technical field
The present invention relates to technical field of polymer materials, and in particular to a kind of flexible electronic substrate adhesive and its preparation
Method, and the application in flexible electronic substrate process.
Background technology
With global energy crisis and the fast development of science and technology, various ultra-thins, low power consuming, meet human engineering and environmental protection
The numerous and confused rudiment of intelligent electronic information products of concept and listing.The flexible electronic substrate of such product mix is according to traditional
LCD assembles equipment and technique, can deform because heated, if exploitation new equipment and technology in addition, cost increase, thus using by
Flexible base board is temporarily fixed at the method on hard substrate (carrier), the flexural deformation of flexible base board during reducing the techniques such as TFT.
Flexible electronic substrate is temporarily fixed in the prior art, and the company such as TCL, Samsung, Asus is inhaled using vacuum/electrostatic more
Affixed conjunction separating technology, the technique are high to equipment, environmental requirement, and the base material scope of application is small, absorption or may be right when removing substrate
Substrate causes to damage；Another method is to use interim fixed class adhesive products, such as faces flexible base board with common adhesives
When be fixed on hard substrate, after TFT working processes, heating adhesive soften, between flexible base board and hard substrate
Insert wire and carry out manual stripping, because of manual operations, it is easy to which flexible base board is caused to damage.In order to avoid stripping causes by hand
Damage, made again between carrier substrates and flexible base board later metal level, oxide skin(coating), dielectric film etc. as sacrifice layer or
DBL layers (De-Bonding Layer, release layer), it is extra to make release layer increase although protecting by viscous flexible base board
The complexity of technique, and the process conditions more difficult control peeled off, it is unfavorable for making the flexible display of high quality.Also one
Kind avoids peeling off the technology for causing damage by hand, is to be scanned in hard carrier substrate back using High energy laser beam, makes gluing
Agent aging, adhesive strength decline, so that flexible base board can strip down from carrier, but this method needs superlaser
Scanning, production efficiency are relatively low, it is also possible to which the device of preparation is affected.Therefore, it is necessary to which a kind of swash without high energy
Light aging is strippable BDB adhesive products.
" memo " of Minnesota Mining and Manufacturing Company belongs to BDB adhesive, remote using more than 10 μm of microballoon of diameter, microsphere diameter
More than emulsion adhesive, form point with adherend surface and contact, contacted compared to emulsion adhesive with the face of adherend, contact area
Greatly reduce, make adhesive become to be easily peeled off, while not inharmonious connection function again.But the problem of existing is, low peel strength
Realize premised on sacrificing adhesive strength, can be only applied to the occasion that adhesive strength requires low.
Patent CN103540269A uses the acrylate containing phenoxy group and vinyl, and for monomer, coumarin derivative is light
Reversible cross-linking agent, prepare a kind of reversible adhesive of ultraviolet lighting.Wherein, coumarin derivative issues in 315-400nm illumination
Third contact of a total solar or lunar eclipse dimerization reaction forms dimer, and and can photocleavage is reactant under 190-280nm illumination.But the adhesive prepares work
Skill is complicated, severe reaction conditions, to equipment requirement height, it is difficult to large-scale production.
The mobility of temperature influence crystalline polymer, Japan Patent Hei 9-249858 disclose a kind of adhesive,
Its molecular side chain contains crystallizable polymers, and crystallizable, glue-line volume contraction after crystallization during less than 15 DEG C, peel strength reduces,
Therefore reducing temperature can make the adhesive become prone to peel off.LG Chemical Ltd. then by triphenyl phosphoric acid (81 DEG C of fusing point),
3- hydroxy phenyl phosphoroso- propionic acid (HPP；C9H11O4P；158 DEG C of fusing point), 9,10- dihydroxy -9- oxa- -10- phospho hetero phenanthrenes -10-
Oxide (DOPO；C12H9O2P；119 DEG C of fusing point) etc. have 50-200 DEG C of fusing point crystalline material be added to acrylate
In be prepared for a kind of low-temperature adhesion, high temperature peel off adhesive.When temperature is less than crystalline material fusing point, crystalline material is in crystallization
State, adhesive strength is big, and when temperature is higher than the fusing point of crystalline material, crystalline material is in molten condition, and mobility improves, made
Obtain adhesive to be easily peeled off, but cull is serious after the stripping of such adhesive.
The content of the invention
The invention provides a kind of flexible electronic substrate adhesive and preparation method thereof and in flexible electronic substrate processing procedure
In application.The advantages of comprehensive epoxy resin of the present invention and acrylate, the two is compounded, prepare flexible electronic substrate use
Adhesive.The adhesive strength of the adhesive is very high, when needing to peel off, peel strength need to can only be dropped rapidly after ultraviolet light
It is low, it is a kind of bonding and removes bonding (Bonding and Debonding, BDB) adhesive, base material is not damaged in stripping process,
Heat-resist and cull is few, preparation technology is simple, easy to use.In addition, the adhesive, without using organic solvent, environmental protection is without dirt
Dye.
The technical solution adopted by the present invention is as follows：
A kind of flexible electronic substrate adhesive, including component A and component B, each component are mixed by following weight parts：
Component A：
Component B：
Thermal curing agents 1-15 parts.
There is epoxyn raw material to be easy to get, and adhesive strength is high, heat-resist, good dimension stability, safety and environmental protection
The advantages that, but toughness is bad；Acrylate can prepare ultraviolet photo-curing cementing agent, and photocuring is simple to operate, curing rate
It hurry up, glued membrane good toughness, shrinkage factor is big, adhesive can be caused to be easily peeled off due to shrinking.Acrylate can be additionally used in toughness reinforcing
Epoxy resin and modified acrylic ester resin compounding are prepared flexible electronic substrate adhesive, make two by epoxy resin, the present invention
Kind polymer has complementary advantages.
In the present invention, epoxy resin is bonded component as heat cure, and dosage is bigger, and the adhesive strength of gained adhesive is got over
It is high；Modified acrylic ester resin peels off component as photocuring, and dosage is bigger, and the peel strength of gained adhesive is lower, gluing
Agent is more easily peeled off, and residual silkgum content can also reduce；In the case where the present invention matches, the adhesive strength of gained adhesive is moderate, and adhesive is easy
It is relatively low in stripping, residual silkgum content.
Thermal curing agents dosage is bigger, and the active hydrogen for participating in reacting is more, and curing rate is faster, but heat release is serious, after solidification
Glue-line fragility is bigger；Thermal curing agents dosage is fewer, then curing rate is slower, and solidification is insufficient, and the adhesive effect of adhesive is poor.
It is different in view of the hardening time needed under different occasions, the dosage of thermal curing agents in the present invention is obtained after optimization.
Light trigger dosage is too low, and photocuring reaction is incomplete, adhesive after ultraviolet light peel strength still compared with
Height, flexible base board are difficult to peel off；Light trigger dosage is too high, then causes waste of resource, draws by preferably obtaining light in the present invention
Send out the dosage of agent.
Preferably, described modified acrylic ester resin is changed from epoxy modification acrylate resin and/or polyurethane
Property acrylate, viscosity is 2000-8000mPas (60 DEG C).Epoxy modification acrylate resin has epoxy resin and propylene concurrently
It is the advantages of acid ester resin, good with epoxy resin compatibility；And polyurethane-modified polyacrylate resin has polyurethane and acrylic acid concurrently
The advantages of ester resin.
Wherein, shown in described polyurethane-modified polyacrylate resin structure such as formula (I)：
In formula (I),
R is selected from
R ' isN is 1~10 integer.
Preferably, described epoxy modification acrylate resin from bisphenol type epoxy modified acrylic ester resin and/
Or phenolic epoxy modified acrylic ester resin, bisphenol type epoxy modified acrylic ester resin are epoxy modification acrylate trees
Most wide one kind of use range in fat；Phenolic epoxy modified acrylic ester resin is applicable to the field of rapid ultraviolet photocuring
Close, because containing 2 functional groups in each bisphenol type epoxy modified acrylic ester resin molecule, each phenolic epoxy is modified
Acrylate molecule averagely contains 3.6 functional groups, so phenol aldehyde type reactivity is high, curing rate is fast, but phenol aldehyde type
The cost of epoxy modification acrylate resin is higher, and application is extensive not as bisphenol type epoxy modified acrylic ester resin.
Further preferably, the structure such as formula (II) of described epoxy modification acrylate resin or (III) are shown
In formula (II) and (III), R is defined as described above, and n is 1~3 integer.
Preferably, described epoxy resin is from bisphenol A type epoxy resin, bisphenol f type epoxy resin, hydrogenated bisphenol A
One in type epoxy resin, methylol bisphenol A type epoxy resin, o-cresol formaldehyde type epoxy resin, resorcinol type epoxy resin
Kind is a variety of.Above-mentioned epoxy resin is in a liquid state at room temperature, and viscosity is 7000-18000mPas (25 DEG C), good fluidity,
It is easy to be coated with.
Preferably, described light trigger is radical polymerization mould assembly light trigger, including benzoin and its derivatives, benzene
The one or more of ethyl ketone photoinitiator and acylphosphine oxide.Wherein, benzoin and its derivatives such as styrax bis ether；Benzene
Ethyl ketone photoinitiator such as 2,2- diethoxies phenyl ethyl ketone, 1- hydroxy-cyciohexyl phenyl ketones；Fragrant ketone-type photoinitiators are such as
Benzophenone, 2,4,6- trimethylbenzophenones；Acylphosphine oxide such as 2,4,6- trimethylbenzoyls diphenyl phosphine oxide
(TPO)。
Preferably, described reactive diluent is from GMA, hexamethylene -1,2- dicarboxylic acids two
Ethylene oxidic ester, 4,5- 7-oxa-bicyclo[4.1.0-1,2- diformazans acid glycidyl ester, ethoxylated bisphenol a diacrylate, dimethoxy
One or more in base tetraacrylate and dipentaerythritol acrylate.These reactive diluent modest viscosities,
Can effectively reduce system viscosity, wherein, GMA, hexamethylene -1,2- dicarboxylic acids 2-glycidyl ester,
4,5- 7-oxa-bicyclo[4.1.0-1,2- diformazan acid glycidyl esters contain 1,2,3 epoxy radicals respectively, can participate in heat cure reaction
In, effectively improve adhesive strength, GMA, ethoxylated bisphenol a diacrylate, dimethoxy propane
Tetraacrylate, dipentaerythritol acrylate contain 1,2,4,6 acrylate group respectively, and it is anti-to participate in photocuring
Ying Zhong, effectively reduce peel strength.
Preferably, described thermal curing agents are aliphatic amine curing agent, alicyclic amines curing agent or aromatic amine
Class curing agent.Wherein, aliphatic amine curing agent includes diethylenetriamine, triethylene tetramine, TEPA and isophthalic diformazan
One or more in amine；Alicyclic amines curing agent includes 1,3- double (aminomethyl) hexamethylene, N- aminoethyl piperazines and loop coils
One or more in diamines；Aromatic amine curing agent includes m-phenylene diamine (MPD), 4,4 '-diaminodiphenylsulfone and 4,4 '-diamino
One or more in base diphenyl-methane.
Preferably, described flexible electronic substrate adhesive, including component A and component B, each component press following weight
Part mixing：
Component A：
Component B：
Thermal curing agents 1-15 parts.
Above-mentioned flexible electronic substrate is moderate with adhesive adhesive strength, and adhesive is easily peeled off, and residual silkgum content is relatively low.
Present invention also offers a kind of preparation method of above-mentioned flexible electronic substrate adhesive, including：By epoxy resin
It is well mixed with modified acrylic ester resin, adds reactive diluent and light trigger, be well mixed under the conditions of lucifuge, obtain group
Divide A, using thermal curing agents as component B, produce the flexible electronic substrate adhesive of two-component.When in use by component B addition groups
Divide in A and be uniformly mixed, be placed in removing bubble in vacuum drying oven, you can gluing.
Present invention also offers a kind of application of above-mentioned flexible electronic substrate adhesive in flexible electronic substrate processing procedure,
Specifically include：
(1) cleaning hard glass baseplate surface；
(2) described flexible electronic substrate is spread evenly across on hard glass substrate with adhesive with spreader；
(3) flexible electronic substrate for being intended to be bonded, which is covered on the hard glass substrate for be coated with adhesive, to be carried out at solidification
Reason, makes flexible electronic substrate be temporarily fixed on hard glass substrate；
(4) it is processed on flexible electronic substrate；
(5) 6000-10000mW/cm is used2High-pressure sodium lamp, ultraviolet light irradiation 40-100s, makes the modification in adhesive
Acrylate is photocured cross-linked, because gluing oxidant layer cross-linking shrinkage makes adhesive lose viscosity, so as to remove hard glass
Substrate and the adhesive for losing viscosity, obtain the flexible electronic substrate after working process.
Preferably, the coating thickness of adhesive is 0.05~0.2mm.
Described flexible electronic substrate can be thin for polyimides (PI) film, polyethylene terephthalate (PET)
Film etc..
In step (3), different solidification processing methods is selected according to different thermal curing agents, when thermal curing agents in adhesive
During from aliphatic amine or alicyclic amines curing agent, through cold curing 20-50min, rapid curing bonding is applicable to
And not heatable occasion, if hardening time is less than 20min, solidification is incomplete, and adhesive strength is relatively low, and hardening time exceedes
50min, have been cured completely, without continuing to extend hardening time；When thermal curing agents select aromatic amine heat cure in adhesive
During agent, through 90-150 DEG C of solidification 30-60min, if solidification temperature is less than 90 DEG C, solidification is incomplete, and adhesive strength is relatively low, if
Solidification temperature is higher than 150 DEG C, and the adhesive film fragility after solidification is big；If hardening time is less than 30min, solidification is incomplete, bonding
Low intensity, hardening time more than 60min, have been cured completely, without continuing to extend hardening time.
Adhesive epoxy resin heat cure bonding mechanism is：Under thermal curing agents effect, epoxide group is opened, epoxy
Resin crosslinks reaction, is solidified into adhesive dry film, flexible base board is bonded on hard substrate, reaches temporarily fixed mesh
's.
By taking diethylenetriamine thermal curing agents as an example, the reaction is as follows：
In step (4), described working process includes carrying out TFT (Thin Film Transistor, thin film transistor (TFT))
Processing.
The uv cure machine reason of modified acrylic ester resin includes in adhesive：
After ultraviolet light adhesive, under light trigger effect, the acrylate group of modified acrylic ester resin
Between crosslink reaction.Before ultraviolet lighting, the epoxy radicals heat cure in adhesive is crosslinked, after ultraviolet lighting, third
Enoate group further crosslinks reaction, and excessively crosslinking shrinks adhesive dry film, causes adhesive strength to decline, flexible base
Plate is easy to peel off from hard substrate.
In step (5), if intensity of illumination is less than 6000mW/cm2, peel strength is higher；More than 10000mW/cm2Although stripping
From low intensity, but cause energy waste.Gel content can reflect the photocured cross-linked degree of adhesive film, and gel content is got over
Greatly, photocuring degree is higher, and the gel content of the glued membrane of different ultraviolet lighting times can be measured using extraction process.It is photocured cross-linked
Degree increase with the extension of light application time, peel strength reduce.In 6000-10000mW/cm2Under intensity of illumination, during illumination
Between be less than 40s, gel content is low, and photocuring degree is low, and peel strength is high；After light application time is more than 80s, gel content is close to most
Greatly, and continue to extend light application time, gel content change is little, and peel strength no longer substantially reduces, from the saving energy and time
From the point of view of cost, preferably 60~80s irradiates splitting time as ultraviolet light.
Compared with the existing technology, the present invention has following significant technological progress：
(1) the invention provides a kind of excellent performance, preparation technology be simple and convenient to operate, solvent-free environment-friendly type it is flexible
Electric substrate adhesive.
(2) the advantages of adhesive of the invention combines epoxy resin and acrylate, utilizes epoxy resin thermosetting
Change and produce high adhesive strength, flexible electronic substrate is temporarily fixed on hard glass substrate, make third by ultraviolet light
Olefin(e) acid ester resin crosslinks, because adhesive film is excessively crosslinked, peel strength substantially reduces, be easily peeled off so as to prepare one kind,
Lossless base material and the few BDB adhesive of cull.
(3) adhesive using pure acrylate resin as bonding component is compared, adhesive of the invention uses asphalt mixtures modified by epoxy resin
Fat has more preferable heat resistance as bonding component.
Brief description of the drawings
Fig. 1 is slide surface cull condition diagram after stripping adhesive film；
Fig. 2 is the thermogravimetric curve of adhesive prepared by embodiment 1.
Embodiment
The method of testing used in the embodiment of the present invention is as follows：
1st, adhesive adhesive strength and peel strength test
300 × 25mm glass substrates are fully cleaned using absolute ethyl alcohol, the adhesive even spread that will be prepared with spreader
In on the hard glass substrate after cleaning, precuring is stood, then covers 350 × 25mm Kaptons (PI films), then
Glass-PI film test bars are placed in the metal trough of control bondline thickness, metal trough upper cap upper glass plates, 5kg weights are placed on plate
Code, room temperature or it is heating and curing at this pressure, obtains the test bars that bondline thickness is about 100 μm.Partial test batten reference
Standard GB/T/T 2790-1995《Adhesive 180 degree peeling strength test method-flexible material is to rigid material》Directly survey
Its fixed 180 ° of peel strengths, are as a result the adhesive strength of this adhesive, and another part test bars are placed in high-pressure sodium lamp
(6000-10000mW/cm2) under ultraviolet light certain time (40-100s), determine its 180 ° of peel strengths, as a result be this
The peel strength of adhesive.
2nd, adhesive cull situation characterizes
Slide is fully cleaned using absolute ethyl alcohol, the adhesive prepared is spread evenly across on slide with spreader,
Precuring is stood, then covers 4 × 2cm Kaptons (PI films), heating or cold curing and the thickness for controlling gluing oxidant layer
About 0.1mm is spent, is subsequently placed in high-pressure sodium lamp (6000-10000mW/cm2) under ultraviolet lighting certain time (40-100s), peel off
Observation slide surface cull under petrographic microscope (Japanese NIKON companies, ECLIPSE E600W POL) is placed in after adhesive film
Situation, for photo as shown in figure 1, wherein, (a) is adhesive prepared by the embodiment of the present invention 1, (b) is common commercially available adhesive (section
Good new material Co., Ltd, KJ-998).As a result show compared with common adhesives, after adhesive prepared by this method is peeled off
Residual silkgum content is few.
3rd, adhesive thermogravimetric curve
2mg or so adhesive is taken, under nitrogen atmosphere, with 20 DEG C/min heating rate, in 50 DEG C of -700 DEG C of temperature
In the range of to adhesive carry out thermogravimetic analysis (TGA) (PE companies of the U.S., Pyris 1TGA thermal analyzers).With the maximum weightless speed of curve
The intersection point of tangent line and extrapolated baseline at rate is designated as T as initial decomposition temperatureonset, the result of adhesive prepared by embodiment 1
As shown in Fig. 2 T in Fig. 2onset=325 DEG C.
4th, the gel content of extraction process measure glued membrane
0.2g adhesive films are taken, and are cut into 1.5 × 1 × 1mm small pieces, weighs and is designated as m0, using dimethylbenzene as extraction
Agent, 24h is extracted using apparatus,Soxhlet's, sample is flushed three times after taking out with pure dimethylbenzene, is then placed into 80 DEG C of vacuum and is dried
24h is dried in case, then is placed in drier, weighs and is designated as m1, gel content Gc is calculated as follows：
Embodiment 1
By 100 parts of bisphenol type epoxy modified acrylic ester resins (Wenzhou Heng Li printing materials Co., Ltd, HL-160) with
20 parts of epoxy resin (blue star Xingchen Synthetic Matrials Co., Ltd., Nantong, WSR618) are well mixed, add 18 parts of methacrylic acids
Ethylene oxidic ester and 3.6 parts of 1- hydroxycyclohexyl phenyl ketones (Zhejiang Yangfan New Materials Co., Ltd., PI008), lucifuge
Under the conditions of be well mixed with mechanical agitation, obtain component A, using 2 parts of diethylenetriamines as component B, produce two-component BDB flexible electricals
Submounts adhesive.
Component B is added in component A and stirred, is placed in vacuum drying oven and removes bubble, with spreader by adhesive
It is spread evenly across (the thickness 0.1mm of gluing oxidant layer) on the hard glass substrate after cleaning.Kapton (is closed in Shanghai again
Resin research institute, H films) it is fitted on the hard glass substrate for being coated with adhesive, solidify 30min at room temperature, survey adhesive
Adhesive strength；In 8000mW/cm2Ultraviolet light 80s under intensity of illumination, survey the peel strength of adhesive.
The adhesive strength of this group of sample reaches 2.8N/25mm, and peel strength 0.18N/25mm, residual silkgum content is few, starting
Decomposition temperature is 325 DEG C.
Embodiment 2~4
Two-component BDB flexible electronic substrate adhesive is prepared using the method for embodiment 1, differs only in change diethyl
The dosage of alkene triamine, its adhesive strength, peel strength and TonsetValue is shown in Table 1.
Table 1
Embodiment 5~7
Two-component BDB flexible electronic substrate adhesive is prepared using the method for embodiment 1, differs only in change room temperature
Hardening time, adhesive strength, peel strength and the T of this group of sampleonsetValue is shown in Table 2.
Table 2
Embodiment 8~10
Two-component BDB flexible electronic substrate adhesive is prepared using the method for embodiment 1, it is ultraviolet to differ only in change
Light application time, adhesive strength, peel strength and the T of this group of sampleonsetValue is shown in Table 3.
Table 3
Embodiment 11~17
Two-component BDB flexible electronic substrate adhesive is prepared using the method for embodiment 1, the difference is that changing heat cure
Species, dosage and the condition of cure of agent, adhesive strength, peel strength and the T of this group of sampleonsetValue is shown in Table 4.
Table 4
Embodiment 18~20
Two-component BDB flexible electronic substrate adhesive is prepared using the method for embodiment 1, the difference is that changing bisphenol-A
The proportioning of type ring oxygen modified acrylic ester resin and epoxy resin, adhesive strength, peel strength and the T of this group of sampleonsetValue is shown in
Table 5.
Table 5
Embodiment 21~23
Two-component BDB flexible electronic substrate adhesive is prepared using the method for embodiment 1, the difference is that changing ultraviolet light
According to intensity, adhesive strength, peel strength and the T of this group of sampleonsetValue is shown in Table 6.
Table 6
Embodiment 24
100 parts of bisphenol type epoxy modified acrylic ester resins are well mixed with 18 parts of epoxy resin, add 10 parts of hexamethylenes
Alkane -1,2- dicarboxylic acids 2-glycidyl ester and 3.8 parts of 1- hydroxy-cyciohexyl phenyl ketones, mixed with mechanical agitation under the conditions of lucifuge
Close uniformly, obtain component A, using 2 parts of thermal curing agents diethylenetriamines as component B, produce two-component BDB flexible electronic substrate glue
Stick.
Component B is added into component A, and is uniformly mixed, is placed in vacuum drying oven and removes bubble, gluing.Operating procedure
With embodiment 1, the adhesive strength of this group of sample is 5.3N/25mm, and peel strength 0.89N/25mm, residual silkgum content is few, starting
Decomposition temperature TonsetFor 326 DEG C.
Embodiment 25
100 parts of bisphenol type epoxy modified acrylic ester resins are well mixed with 19 parts of epoxy resin, add 9 part of two season
The acrylate of penta tetrol six and 3 parts of 1- hydroxy-cyciohexyl phenyl ketones, it is well mixed under the conditions of lucifuge, is obtained with mechanical agitation
Component A, using 2.2 parts of thermal curing agents diethylenetriamines as component B, produce two-component BDB flexible electronic substrate adhesive.
It is uniformly mixed after component B is added into component A, is placed in removing bubble in vacuum drying oven, you can gluing.Operation
Technique is with embodiment 1, and the adhesive strength of this group of sample is 1.9N/25mm, and peel strength 0.20N/25mm, residual silkgum content is few,
Initial decomposition temperature TonsetFor 325 DEG C.
Embodiment 26
100 parts of epoxy novolac modified acrylic ester resins are well mixed with 20 parts of epoxy resin, add 12 parts of methyl-props
Olefin(e) acid ethylene oxidic ester and 4 parts of 1- hydroxy-cyciohexyl phenyl ketones, it is well mixed with mechanical agitation under the conditions of lucifuge, obtains group
Divide A, using 2 parts of thermal curing agents diethylenetriamines as component B, produce two-component BDB flexible electronic substrate adhesive.
It is uniformly mixed after component B is added into component A, is placed in removing bubble in vacuum drying oven, you can gluing.Operation
Technique is with embodiment 1, and the adhesive strength of this group of sample is 3.5N/25mm, and peel strength 0.50N/25mm, residual silkgum content is few,
Initial decomposition temperature TonsetFor 327 DEG C.
Embodiment 27
100 parts of polyurethane-modified polyacrylate resins are well mixed with 21 parts of epoxy resin, add 10 parts of metering systems
Acid glycidyl ester and 3.8 parts of 1- hydroxycyclohexyl phenyl ketones, it is well mixed with mechanical agitation under the conditions of lucifuge, obtains component
A, using 2 parts of thermal curing agents diethylenetriamines as component B, produce two-component BDB flexible electronic substrate adhesive.
It is uniformly mixed after component B is added into component A, is placed in removing bubble in vacuum drying oven, you can gluing.Operation
Technique is with embodiment 1, and the adhesive strength of this group of sample is 1.2N/25mm, and it is 0.20N/25mm to peel off strong, and residual silkgum content is few, is risen
Beginning decomposition temperature TonsetFor 321 DEG C.
Claims (10)
1. a kind of flexible electronic substrate adhesive, it is characterised in that including component A and component B, each component presses following weight parts
Mixing：
Component A：
Component B：
Thermal curing agents 1-15 parts.
2. flexible electronic substrate adhesive according to claim 1, it is characterised in that described modification acrylate tree
Fat selects epoxy modification acrylate resin and/or polyurethane-modified polyacrylate.
3. flexible electronic substrate adhesive according to claim 2, it is characterised in that described epoxy-modified acrylic acid
Ester resin selects bisphenol type epoxy modified acrylic ester resin and/or phenolic epoxy modified acrylic ester resin.
4. flexible electronic substrate adhesive according to claim 1, it is characterised in that described epoxy resin is from double
Phenol A types epoxy resin, bisphenol f type epoxy resin, bisphenol-A epoxy resin, methylol bisphenol A type epoxy resin, adjacent first
One or more in phenol aldehyde type epoxy resin and resorcinol type epoxy resin.
5. flexible electronic substrate adhesive according to claim 1, it is characterised in that described light trigger is freely
Base polymeric photoinitiator, including benzoin and its derivatives, acetophenones light trigger and acylphosphine oxide one kind or
It is a variety of.
6. flexible electronic substrate adhesive according to claim 1, it is characterised in that described reactive diluent is selected
GMA, hexamethylene-1,2- dicarboxylic acids 2-glycidyl ester, 4,5- 7-oxa-bicyclo[4.1.0-1,2- dioctyl phthalate
Ethylene oxidic ester, ethoxylated bisphenol a diacrylate, dimethoxy propane tetraacrylate and the acrylic acid of dipentaerythritol six
One or more in ester.
7. flexible electronic substrate adhesive according to claim 1, it is characterised in that described thermal curing agents are fat
Race's amine curing agent, alicyclic amines curing agent or aromatic amine curing agent.
A kind of 8. preparation method of the flexible electronic substrate adhesive described in any one of claim 1~7, it is characterised in that
Including：Epoxy resin is well mixed with modified acrylic ester resin, addition reactive diluent and light trigger, under the conditions of lucifuge
It is well mixed, component A is obtained, using thermal curing agents as component B, produces the flexible electronic substrate adhesive of two-component.
9. the flexible electronic substrate adhesive described in a kind of any one of claim 1~7 is in flexible electronic substrate processing procedure
Using.
10. application of the flexible electronic substrate adhesive according to claim 9 in flexible electronic substrate processing procedure, it is special
Sign is, including：
(1) cleaning hard glass baseplate surface；
(2) described flexible electronic substrate is spread evenly across on hard glass substrate with adhesive with spreader；
(3) flexible electronic substrate for being intended to be bonded, which is covered on the hard glass substrate for be coated with adhesive, carries out curing process,
Flexible electronic substrate is set to be temporarily fixed on hard glass substrate；
(4) it is processed on flexible electronic substrate；
(5) 6000-10000mW/cm is used2High-pressure sodium lamp, ultraviolet light irradiation 40-100s, makes the modified acroleic acid in adhesive
Ester resin is photocured cross-linked, because gluing oxidant layer cross-linking shrinkage makes adhesive lose viscosity, so as to remove hard glass substrate and
The adhesive of viscosity is lost, obtains the flexible electronic substrate after working process.
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