CN107384282B - 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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- CN107384282B CN107384282B CN201710652649.5A CN201710652649A CN107384282B CN 107384282 B CN107384282 B CN 107384282B CN 201710652649 A CN201710652649 A CN 201710652649A CN 107384282 B CN107384282 B CN 107384282B
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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
-
- 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
-
- 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
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 photoinitiator, 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 removing after a large amount of residue glues, have the characteristics that 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 equipments flexible display screen such as tablet 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 technique
With the fast development of global energy crisis and 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 and listing of concept.The flexible electronic substrate of such product mix is according to traditional
LCD assembles equipment and technique, and meeting be deformed because heated, if in addition exploitation new equipment and technology, cost increase, therefore using will
Flexible base board is temporarily fixed at the method on hard substrate (carrier), the bending deformation of flexible base board when reducing the techniques such as TFT.
Flexible electronic substrate is fixed temporarily in the prior art, and the companies such as TCL, Samsung, Asus mostly use vacuum/electrostatic to inhale
Affixed conjunction separating technology, the technique are high to equipment, environmental requirement, and the substrate scope of application is small, may be right when adsorbing or removing substrate
Substrate causes to damage；Another method is such as to face flexible base board with common adhesives using class adhesive products are fixed temporarily
When be fixed on hard substrate, after TFT working process, heating adhesive soften, between flexible base board and hard substrate
It is inserted into conducting wire and carries out manual removing, because of manual operations, it is easy to be damaged to flexible base board.In order to avoid removing causes by hand
Damage, made between carrier substrates and flexible base board again later metal layer, oxide skin(coating), insulating film etc. as sacrificial layer or
DBL layers (De-Bonding Layer, release layer), although protecting the flexible base board glued, the additional release layer that makes increases
The complexity of technique, and the process conditions removed are more difficult to control, are unfavorable for making the flexible display of high quality.There are also one
Kind avoids removing 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, to enable flexible base board to strip down from carrier, but this method needs superlaser
Scanning, production efficiency are lower, it is also possible to affect to the device of preparation.Therefore, it is necessary to one kind to swash without high energy
Light aging, that is, strippable BDB adhesive products.
" memo " of Minnesota Mining and Manufacturing Company belongs to BDB adhesive, and using 10 μm of diameter or more of microballoon, microsphere diameter is remote
Greater than emulsion adhesive, point contact is formed with adherend surface, compared to the face contact of emulsion adhesive and adherend, contact area
It greatly reduces, adhesive is made to become easy removing, while not inharmonious connection function again.But the problem is that low peel strength
It realizes premised on sacrificing adhesive strength, can be only applied to adhesive strength and require low occasion.
Patent CN103540269A uses the acrylate containing phenoxy group and vinyl for monomer, and coumarin derivative is light
Reversible cross-linking agent prepares a kind of reversible adhesive of ultraviolet lighting.Wherein, coumarin derivative is issued in 315-400nm illumination
Third contact of a total solar or lunar eclipse dimerization reaction forms dimer, and energy photocleavage is reactant again under 190-280nm illumination.But the adhesive prepares work
Skill is complicated, severe reaction conditions, the high requirements on the equipment, it is difficult to large-scale production.
The mobility of temperature influence crystalline polymer, Japan Patent Hei 9-249858 discloses a kind of adhesive,
Its molecular side chain contains crystallizable polymers, and crystallizable, glue-line volume contraction after crystallization when being lower than 15 DEG C, peel strength reduces,
Therefore reducing temperature can make the adhesive become prone to remove.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 phenanthrene -10-
Oxide (DOPO；C12H9O2P；119 DEG C of fusing point) etc. be added to acrylate with the crystalline material of 50-200 DEG C of fusing point
In be prepared for a kind of low-temperature adhesion, high temperature removing adhesive.When temperature is lower 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 a molten state, and mobility improves, and makes
It obtains adhesive to be easily peeled off, but residue glue is serious after the removing of such adhesive.
Summary of the invention
The present 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, prepares flexible electronic substrate use
Adhesive.The adhesive strength of the adhesive is very high, when needing to remove, peel strength can need to only drop rapidly after ultraviolet light
It is low, it is a kind of bonding and removes bonding (Bonding and Debonding, BDB) adhesive, does not damage substrate in stripping process,
And residue glue is few, heat-resist, preparation process is simple, easy to use.In addition, the adhesive does not use organic solvent, environmental protection is without dirt
Dye.
The technical solution adopted by the 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:
1-15 parts of thermal curing agents.
Epoxyn is easy to get with raw material, 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 easy to operate, curing rate
Fastly, glue film good toughness, shrinking percentage is big, is easily peeled off since contraction can lead to adhesive.Acrylate can also be used in toughening
Epoxy resin is compounded with modified acrylic ester resin and prepares flexible electronic substrate adhesive by epoxy resin, the present invention, makes two
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 removes 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；Under present invention proportion, the adhesive strength of gained adhesive is moderate, and adhesive is easy
In removing, residual silkgum content is relatively low.
Thermal curing agents dosage is bigger, and the active hydrogen for participating in reaction is more, and curing rate is faster, but heat release is serious, after solidification
Glue-line brittleness 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.
In view of the curing time needed under different occasions is different, the dosage of thermal curing agents in the present invention is obtained after optimization.
Photoinitiator 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 remove；Photoinitiator dosage is excessively high, then causes waste of resource, draws by preferably obtaining light in the present invention
Send out the dosage of agent.
Preferably, the modified acrylic ester resin selects epoxy modification acrylate resin and/or polyurethane to change
Property acrylate, viscosity be 2000-8000mPas (60 DEG C).Epoxy modification acrylate resin has both epoxy resin and propylene
It is the advantages of acid ester resin, good with epoxy resin compatibility；And polyurethane-modified polyacrylate resin has both polyurethane and acrylic acid
The advantages of ester resin.
Wherein, shown in the polyurethane-modified polyacrylate resin structure such as formula (I):
In formula (I),
R is selected from
R ' isThe integer that n is 1~10.
Preferably, the epoxy modification acrylate resin select 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 scope in rouge；Phenolic epoxy modified acrylic ester resin is applicable to the field of rapid ultraviolet photocuring
It closes, 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 higher cost of epoxy modification acrylate resin, application range are extensive not as good as bisphenol type epoxy modified acrylic ester resin.
Further preferably, the structure such as formula (II) of the epoxy modification acrylate resin or (III) are shown
In formula (II) and (III), R is defined as described above, the integer that n is 1~3.
Preferably, the epoxy resin selects bisphenol A type epoxy resin, bisphenol f type epoxy resin, hydrogenated bisphenol A
Type epoxy resin, methylol bisphenol A type epoxy resin, o-cresol formaldehyde type epoxy resin, one in resorcinol type epoxy resin
Kind is a variety of.Above-mentioned epoxy resin is in a liquid state at room temperature, viscosity be 7000-18000mPas (25 DEG C), good fluidity,
It is easy to be coated with.
Preferably, the photoinitiator is radical polymerization mould assembly photoinitiator, including benzoin and its derivatives, benzene
Ethyl ketone photoinitiator and acylphosphine oxide it is one or more.Wherein, benzoin and its derivatives such as styrax bis ether；Benzene
Ethyl ketone photoinitiator such as 2,2- diethoxy phenyl ethyl ketone, 1- hydroxy-cyciohexyl phenyl ketone；Fragrant ketone-type photoinitiators are such as
Benzophenone, 2,4,6- trimethylbenzophenone；Acylphosphine oxide such as 2,4,6- trimethylbenzoyl diphenyl phosphine oxide
(TPO)。
Preferably, the reactive diluent selects glycidyl methacrylate, hexamethylene -1,2- dicarboxylic acids two
Ethylene oxidic ester, 4,5- 7-oxa-bicyclo[4.1.0-1,2- diformazan acid glycidyl ester, ethoxylated bisphenol a diacrylate, dimethoxy
One of base tetraacrylate and dipentaerythritol hexaacrylate are a variety of.These reactive diluent modest viscosities,
System viscosity can be effectively reduced, wherein glycidyl methacrylate, 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 group respectively, can participate in heat cure reaction
In, effectively improve adhesive strength, glycidyl methacrylate, ethoxylated bisphenol a diacrylate, dimethoxy propane
Tetraacrylate, dipentaerythritol hexaacrylate contain 1,2,4,6 acrylate group respectively, and it is anti-to participate in photocuring
Peel strength is effectively reduced in Ying Zhong.
Preferably, the 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, tetraethylenepentamine and isophthalic diformazan
One of amine is a variety of；Alicyclic amines curing agent includes bis- (aminomethyl) hexamethylenes of 1,3-, N- aminoethyl piperazine and loop coil
One of diamines is a variety of；Aromatic amine curing agent includes m-phenylene diamine (MPD), 4,4 '-diaminodiphenylsulfones and 4,4 '-diaminos
One of base diphenyl-methane is a variety of.
Preferably, the flexible electronic substrate adhesive, including component A and component B, each component press following weight
Part mixing:
Component A:
Component B:
1-15 parts of thermal curing agents.
Above-mentioned flexible electronic substrate is moderate with adhesive adhesive strength, and adhesive is easily peeled off, and residual silkgum content is relatively low.
The present invention also provides a kind of preparation methods of above-mentioned flexible electronic substrate adhesive, comprising: by epoxy resin
It is uniformly mixed with modified acrylic ester resin, reactive diluent and photoinitiator is added, be uniformly mixed under the conditions of being protected from light, obtain group
Divide A, is component B to get the flexible electronic substrate adhesive of two-component using thermal curing agents.When in use by component B addition group
Divide in A and be uniformly mixed, is placed in vacuum drying oven and removes bubble, it can gluing.
The present invention also provides a kind of application of above-mentioned flexible electronic substrate adhesive in flexible electronic substrate processing procedure,
It specifically includes:
(1) cleaning hard glass baseplate surface；
(2) flexible electronic substrate is spread evenly across on hard glass substrate with adhesive with spreader；
(3) flexible electronic substrate for being intended to fitting, which is covered on the hard glass substrate for be coated with adhesive, to carry out at solidification
Reason, is temporarily fixed on flexible electronic substrate on hard glass substrate；
(4) it is processed on flexible electronic substrate；
(5) 6000-10000mW/cm is used2High-pressure sodium lamp, ultraviolet light irradiate 40-100s, make the modification in adhesive
Acrylate is photocured cross-linked, since gluing oxidant layer cross-linking shrinkage makes adhesive lose viscosity, to remove hard glass
Substrate and the adhesive for losing viscosity, the flexible electronic substrate after obtaining working process.
Preferably, the coating thickness of adhesive is 0.05~0.2mm.
The 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
When selecting aliphatic amine or alicyclic amines curing agent, through room temperature curing 20-50min, it is applicable to rapid curing bonding
And not heatable occasion, if curing time, less than 20min, not exclusively, adhesive strength is lower for solidification, curing time is more than
50min, has been cured completely, extends curing time without continuing；When thermal curing agents select aromatic amine heat cure in adhesive
When agent, through 90-150 DEG C of solidification 30-60min, if solidification temperature is lower than 90 DEG C, not exclusively, adhesive strength is lower for solidification, if
Solidification temperature is higher than 150 DEG C, and the adhesive film brittleness after solidification is big；If curing time is less than 30min, solidification not exclusively, is bonded
Intensity is low, and curing time is more than 60min, has been cured completely, extends curing time without continuing.
Epoxy resin thermosetting bonding mechanism in adhesive are as follows: under thermal curing agents effect, epoxy group is opened, epoxy
Resin crosslinks reaction, is solidified into adhesive dry film, flexible base board is bonded on hard substrate, reaches the mesh being fixed temporarily
's.
By taking diethylenetriamine thermal curing agents as an example, the reaction is as follows:
In step (4), the 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 photoinitiator effect, the acrylate group of modified acrylic ester resin
Between crosslink reaction.Before ultraviolet lighting, the epoxy group heat cure in adhesive is crosslinked, after ultraviolet lighting, third
Enoate group further occurrence cross-linking reaction, excessively crosslinking shrink adhesive dry film, cause adhesive strength to decline, flexible base
Plate is easy to remove from hard substrate.
In step (5), if intensity of illumination is lower than 6000mW/cm2, peel strength is higher；More than 10000mW/cm2Although stripping
It is low from intensity, but cause energy waste.Gel content is able to 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 glue film 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, when illumination
Between be lower 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, less, peel strength is no longer substantially reduced, from the energy saving and time for gel content variation
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 present invention provides one kind to have excellent performance, preparation process is simple and convenient to operate, solvent-free environment-friendly type is flexible
Electric substrate adhesive.
(2) adhesive of the invention combines the advantages of epoxy resin and acrylate, utilizes epoxy resin thermosetting
Change and generate high adhesive strength, is temporarily fixed at flexible electronic substrate on hard glass substrate, makes third by ultraviolet light
Alkene acid ester resin crosslinking, since adhesive film is excessively crosslinked, peel strength is substantially reduced, thus prepare one kind be easily peeled off,
Lossless substrate and the few BDB adhesive of residue glue.
(3) compared to the adhesive using pure acrylate resin as bonding component, adhesive of the invention uses asphalt mixtures modified by epoxy resin
Rouge has better heat resistance as bonding component.
Detailed description of the invention
Fig. 1 is slide surface residue glue condition diagram after removing adhesive film；
Fig. 2 is the thermogravimetric curve of adhesive prepared by embodiment 1.
Specific embodiment
The test method used in the embodiment of the present invention is as follows:
1, adhesive adhesive strength and peel strength test
300 × 25mm glass substrate is sufficiently cleaned using dehydrated alcohol, the adhesive even spread that will be prepared with spreader
On hard glass substrate after cleaning, precuring is stood, then covers 350 × 25mm Kapton (PI film), then
Glass-PI film test bars are placed in the metal trough of control bondline thickness, metal trough upper cap upper glass plates, 5kg weight is placed on plate
Code room temperature or 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 " is directly surveyed
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), measure its 180 ° of peel strengths, as a result be this
The peel strength of adhesive.
2, adhesive residue glue situation characterizes
Glass slide is sufficiently cleaned using dehydrated alcohol, the adhesive prepared is spread evenly across on glass slide with spreader,
Standing precuring, then covering 4 × 2cm Kapton (PI film), heating or room temperature curing and the thickness for controlling gluing oxidant layer
About 0.1mm is spent, high-pressure sodium lamp (6000-10000mW/cm is subsequently placed in2) under ultraviolet lighting certain time (40-100s), removing
Adhesive film is placed on observation slide surface residue glue under petrographic microscope (Japanese NIKON company, ECLIPSE E600W POL)
Situation, photo are as shown in Figure 1, wherein (a) is adhesive prepared by the embodiment of the present invention 1, is (b) common commercially available adhesive (section
Good new material Co., Ltd, KJ-998).As the result is shown compared with common adhesives, after the adhesive removing of this method preparation
Residual silkgum content is few.
3, adhesive thermogravimetric curve
The adhesive of 2mg or so is taken, under nitrogen atmosphere, with the heating rate of 20 DEG C/min, in 50 DEG C of -700 DEG C of temperature
Thermogravimetic analysis (TGA) (PE company, the U.S., Pyris 1TGA thermal analyzer) is carried out to adhesive in range.With the maximum weightless speed of curve
The intersection point of tangent line and extrapolated baseline at rate is denoted 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.
4, the gel content of extraction process measurement glue film
0.2g adhesive film is taken, and is cut into the small pieces of 1.5 × 1 × 1mm, weighing is denoted as m0, it is extraction with dimethylbenzene
Agent, for 24 hours using Soxhlet extractor extraction, sample is flushed three times after taking out with pure dimethylbenzene, is then placed into 80 DEG C of vacuum and is dried
It dries for 24 hours, then is placed in drier in case, weighing is denoted 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 material Co., Ltd, HL-160) with
20 parts of epoxy resin (blue star Xingchen Synthetic Matrials Co., Ltd., Nantong, WSR618) are uniformly mixed, and 18 parts of methacrylic acids are added
Ethylene oxidic ester and 3.6 parts of 1- hydroxycyclohexyl phenyl ketones (Zhejiang Yangfan New Materials Co., Ltd., PI008), are protected from light
Under the conditions of with mechanical stirring be uniformly mixed, obtain component A, be component B to get two-component BDB flexible electrical using 2 parts of diethylenetriamines
Submount adhesive.
Component B is added in component A and is stirred evenly, removing bubble is placed in vacuum drying oven, with spreader by adhesive
On hard glass substrate after being spread evenly across cleaning (the thickness 0.1mm of gluing oxidant layer).Kapton (is closed in Shanghai again
At resin research institute, H film) it is fitted on the hard glass substrate for being coated with adhesive, solidify 30min at room temperature, surveys adhesive
Adhesive strength；In 8000mW/cm2Ultraviolet light 80s under intensity of illumination surveys 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, difference is only that change diethyl
The dosage of alkene triamine, 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, difference is only that change room temperature
Curing 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, difference is only that change is ultraviolet
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
Type, 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 proportion 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 uniformly mixed with 18 parts of epoxy resin, 10 parts of hexamethylenes are added
Alkane -1,2- dicarboxylic acids 2-glycidyl ester and 3.8 parts of 1- hydroxy-cyciohexyl phenyl ketones, it is mixed with mechanical stirring under the conditions of being protected from light
It closes uniformly, obtains component A, be component B to get two-component BDB flexible electronic substrate glue using 2 parts of thermal curing agents diethylenetriamines
Stick.
Component A is added in component B, and is uniformly mixed, removing bubble, gluing are placed in vacuum drying oven.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 TonsetIt is 326 DEG C.
Embodiment 25
100 parts of bisphenol type epoxy modified acrylic ester resins are uniformly mixed with 19 parts of epoxy resin, 9 part of two season is added
Penta tetrol, six acrylate and 3 parts of 1- hydroxy-cyciohexyl phenyl ketones are uniformly mixed with mechanical stirring under the conditions of being protected from light, are obtained
Component A is component B to get two-component BDB flexible electronic substrate adhesive using 2.2 parts of thermal curing agents diethylenetriamines.
It is uniformly mixed after component A is added in component B, is placed in vacuum drying oven and removes bubble, it 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 TonsetIt is 325 DEG C.
Embodiment 26
100 parts of epoxy novolac modified acrylic ester resins are uniformly mixed with 20 parts of epoxy resin, 12 parts of methyl-props are added
Olefin(e) acid ethylene oxidic ester and 4 parts of 1- hydroxy-cyciohexyl phenyl ketones are uniformly mixed with mechanical stirring under the conditions of being protected from light, obtain group
Divide A, is component B to get two-component BDB flexible electronic substrate adhesive using 2 parts of thermal curing agents diethylenetriamines.
It is uniformly mixed after component A is added in component B, is placed in vacuum drying oven and removes bubble, it 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 TonsetIt is 327 DEG C.
Embodiment 27
100 parts of polyurethane-modified polyacrylate resins are uniformly mixed with 21 parts of epoxy resin, 10 parts of metering systems are added
Acid glycidyl ester and 3.8 parts of 1- hydroxycyclohexyl phenyl ketones are uniformly mixed with mechanical stirring under the conditions of being protected from light, obtain component
A is component B to get two-component BDB flexible electronic substrate adhesive using 2 parts of thermal curing agents diethylenetriamines.
It is uniformly mixed after component A is added in component B, is placed in vacuum drying oven and removes bubble, it can gluing.Operation
For technique with embodiment 1, the adhesive strength of this group of sample is 1.2N/25mm, and removing is by force 0.20N/25mm, and residual silkgum content is few, rises
Beginning decomposition temperature TonsetIt is 321 DEG C.
Claims (8)
1. a kind of application of flexible electronic substrate adhesive in flexible electronic substrate processing procedure, which is characterized in that the flexibility
Electric substrate is made of with adhesive component A and component B, and each component is mixed by following weight parts:
Component A:
Component B:
1-15 parts of thermal curing agents；
Concrete application step includes:
(1) cleaning hard glass baseplate surface；
(2) flexible electronic substrate is spread evenly across on hard glass substrate with adhesive with spreader；
(3) flexible electronic substrate for being intended to fitting, which is covered on the hard glass substrate for be coated with adhesive, carries out curing process,
It is temporarily fixed on flexible electronic substrate on hard glass substrate；
(4) it is processed on flexible electronic substrate；
(5) 6000-10000mW/cm is used2High-pressure sodium lamp, ultraviolet light irradiate 60-80s, make the modified acroleic acid in adhesive
Ester resin is photocured cross-linked, since gluing oxidant layer cross-linking shrinkage makes adhesive lose viscosity, thus remove hard glass substrate and
Lose the adhesive of viscosity, the flexible electronic substrate after obtaining working process.
2. application of the flexible electronic substrate adhesive according to claim 1 in flexible electronic substrate processing procedure, special
Sign is that the modified acrylic ester resin selects epoxy modification acrylate resin and/or polyurethane-modified polyacrylate.
3. application of the flexible electronic substrate adhesive according to claim 2 in flexible electronic substrate processing procedure, special
Sign is that the epoxy modification acrylate resin selects bisphenol type epoxy modified acrylic ester resin and/or phenolic aldehyde type ring
Oxygen modified acrylic ester resin.
4. application of the flexible electronic substrate adhesive according to claim 1 in flexible electronic substrate processing procedure, special
Sign is, the epoxy resin select bisphenol A type epoxy resin, bisphenol f type epoxy resin, bisphenol-A epoxy resin,
One of methylol bisphenol A type epoxy resin, o-cresol formaldehyde type epoxy resin and resorcinol type epoxy resin are a variety of.
5. application of the flexible electronic substrate adhesive according to claim 1 in flexible electronic substrate processing procedure, special
Sign is that the photoinitiator is radical polymerization mould assembly photoinitiator, including benzoin and its derivatives, acetophenones light draw
Send out the one or more of agent and acylphosphine oxide.
6. application of the flexible electronic substrate adhesive according to claim 1 in flexible electronic substrate processing procedure, special
Sign is that the reactive diluent selects glycidyl methacrylate, hexamethylene -1,2- dicarboxylic acids 2-glycidyl
Ester, 4,5- 7-oxa-bicyclo[4.1.0-1,2- diformazan acid glycidyl ester, ethoxylated bisphenol a diacrylate, dimethoxy propane four
One of acrylate and dipentaerythritol hexaacrylate are a variety of.
7. application of the flexible electronic substrate adhesive according to claim 1 in flexible electronic substrate processing procedure, special
Sign is that the thermal curing agents are aliphatic amine curing agent, alicyclic amines curing agent or aromatic amine curing agent.
8. application of the flexible electronic substrate adhesive according to claim 1 in flexible electronic substrate processing procedure, special
Sign is that the preparation method of flexible electronic substrate adhesive includes: to mix epoxy resin and modified acrylic ester resin
It closes uniformly, reactive diluent and photoinitiator is added, be uniformly mixed under the conditions of being protected from light, component A obtained, using thermal curing agents as component
B to get two-component flexible electronic substrate adhesive.
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| CN108822788A (en) * | 2018-06-13 | 2018-11-16 | 上海昀通电子科技有限公司 | Ultraviolet cured adhesive composition, preparation method and its usage |
| CN108997588B (en) * | 2018-06-25 | 2020-10-16 | 同济大学 | Pentaerythritol tetra ((N, N-di (6-aminohexylidene)) -3-aminopropionate) and preparation method and application thereof |
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