CN104592924A - Adhesive composition, adhesive film, adhesive film roll and preparation methods thereof - Google Patents
Adhesive composition, adhesive film, adhesive film roll and preparation methods thereof Download PDFInfo
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- CN104592924A CN104592924A CN201510017200.2A CN201510017200A CN104592924A CN 104592924 A CN104592924 A CN 104592924A CN 201510017200 A CN201510017200 A CN 201510017200A CN 104592924 A CN104592924 A CN 104592924A
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Abstract
The invention provides an adhesive film. The adhesive film has the characteristic of simple assembling, the adhesive film also has the characteristics of high relative dielectric constant, good light proofness, adjustable color, strong adhesive strength, and the like, and the relative dielectric constant in over 6, therefore, the adhesive film is especially applicable to the adhering of capacitive fingerprint recognition chip module encapsulation. The adhesive film is a semi-cured adhesive film which has low viscosity at room temperature, but has high viscosity in the process of thermal curing; compared with a common dispensed adhering mode, the adhesive film provided by the invention has the advantages of uniform film-forming thickness, controllable adhering shape, no bubble produced, simple assembling process, and the like, therefore, the adhesive film is especially suitable for plane adhesive assembly. The invention provides an adhesive composition for forming the adhesive film. The adhesive composition has the characteristics of high relative dielectric constant, and the like. The invention also provides an adhesive film roll. The adhesive film is protected by covering PET release liner or release paper on both sides of the adhesive film in the adhesive film roll, thereby preventing the environment from polluting the adhesive film.
Description
Technical field
The present invention relates to a kind of adhesive composite, be specifically related to a kind of to there is the adhesive composite of high-k, the adhesive film formed by adhesive composite, the adhesive film volume be made up of adhesive film and their preparation method.
Background technology
The relative permittivity of Gumming glue film is in the market very low, such as, mentions a kind of adhesive film in patent CN201310258538.8, and its characteristic is relative permittivity low (about 2.0), and is transparent material; The adhesive film that patent CN 201110301385.1 mentions adds alumina powder and obtains, and because aluminum oxide specific inductivity is lower, the relative permittivity of the adhesive film obtained is less, obviously can not meet relative permittivity ε
rthe requirement of>=6.Patent CN201010003397.1 mentions a kind of preparation method of felting agent coil, but is mainly used in conductive film purposes.
The adhesive composite that above-mentioned prior art makes all is difficult to obtain corresponding high dielectric characteristics, and its major cause is, organic resin is because the characteristic of himself chemical bond is difficult to polarized, and its specific inductivity is difficult to improve.And the method for usually adding the powder such as aluminum oxide, silicon oxide in organism is also difficult to reach relative permittivity ε
rthe requirement of>=6, reason is that the specific inductivity of of the powder such as aluminum oxide, silicon oxide itself is lower, has dragged down the relative permittivity of Gumming glue film further after adding organic resin.And common bonding glue easily produces the defects such as bubble and causes Signal transmissions to be interfered in encapsulation process.
Summary of the invention
The object of the invention is to overcome weak point that prior art exists and provide a kind of adhesive film volume that there is the adhesive composite of high relative dielectric constant, the adhesive film formed by this adhesive composite and be made up of this adhesive film, present invention also offers the preparation method of described adhesive composite.
For achieving the above object, the technical scheme taked: a kind of adhesive composite, described adhesive composite comprises the component of following weight part: matrix resin 100 parts, solidifying agent 5-70 part, curing catalyst 0-3 part, 10 ~ 500 parts, high dielectric ceramic powder, organic solvent 9 ~ 99 parts, dispersion agent 0.1 ~ 5 part, coupling agent 0.1 ~ 10 part, toning agent 0 ~ 100 part.
Preferably, described matrix resin is at least one in styrene-isoprene block copolymer, styrene-butadiene block copolymer, polyorganosiloxane resin, polyvinylidene fluoride resin, epoxy resin, thermosetting acrylic resin and their composite modified resin, at least containing a kind of thermosetting resin in described matrix resin.
Preferably, described solidifying agent is modified sulphur alkylol cpd, imidazoles, modified multicomponent amine, Dyhard RU 100, dicyandiamide modified thing, at least one in modified polyamide and diaminodiphenylsulfone(DDS), described curing catalyst is organic urea or imidazoles, described organic solvent is dehydrated alcohol, acetone, butanone, toluene, Virahol, ethyl acetate, butylacetate, ethylene glycol monoethyl ether, at least one in ethylene glycol monobutyl ether, described dispersion agent is at least one in negatively charged ion and non-ionic dispersing agent, described coupling agent is silane coupling agent or titanate coupling agent, described toning agent is carbon black, one in titanium dioxide and gas-phase silica.Solidifying agent of the present invention is inertia under referring to and solidifying slow or normal temperature at normal temperatures, does not occur crosslinked with matrix resin, and the solidifying agent that curing speed is fast at 100 ~ 180 DEG C.Described solvent is low boiling point solvent.The preferred silane coupling agent of described coupling agent or titanate coupling agent, such as KH-550, KH-560, KH-570, TM-58 etc.Described dispersion agent is selected from negatively charged ion and non-ionic dispersing agent, preferred anionic type macromolecule dispersing agent, the dispersion agent of such as polyacrylic acid sodium salt or phosphoric acid ester.For playing toning and interception, Gumming glue film of the present invention also added toning agent, as carbon black, titanium dioxide, gas-phase silica etc.
Preferably, described high dielectric ceramic powder is TiO
2, ZrO
2, BaTiO
3, CaTiO
3, ZnO, CaZrO
3, MgZrO
3, Ba
xsr
1-xti
yzr
1-yo
3(x, y=0 ~ 1), Ca
yba
1-yzr
xti
1-xo3 (x, y=0 ~ 1), K
xna
1-xnbO
3at least one in (x=0 ~ 1).More preferably, described high dielectric ceramic powder is by the pretreated high dielectric inorganic ceramic powder of disperse modified, disperse modified comprises interpolation suitable organic solvent, dispersion agent, coupling agent etc., and dispersing apparatus used is selected from one or more in high speed disintegrator, ball mill, planet mill, sand mill and planetary mixer.
Preferably, described high dielectric ceramic powder is spherical or class is spherical, and its particle diameter is 0.01 μm ~ 2 μm.
The invention provides a kind of adhesive film, described adhesive film is by being shaped to membranaceous by adhesive composite described above.In moulding process, eliminate the organic solvent in described adhesive composite, and shaping adhesive film is a kind of semicure film.
Preferably, described molding mode is flow casting molding.In capacitance type fingerprint identification chip module, need higher relative permittivity sticky object adhering chip module, to prevent capacitance signal conductively-closed or to be reflected, general requirement relative permittivity ε
r>=6, guarantee capacitance signal can be transferred on chip smoothly.In addition, also need that the thickness of sticky object is smooth, good uniformity, paste shape is controlled, is not easy to produce bubble, and adhesive film of the present invention, owing to being by flow casting molding, can control thickness and the outward appearance of adhesive film easily, is convenient to control defect and produces.
Preferably, the thickness of described adhesive film is 2 μm ~ 100 μm.
The invention provides a kind of adhesive film volume, the three-decker of described adhesive film volume for being formed by respectively covering one deck PET release film or separate-type paper on the two sides of adhesive film described above.The present invention covers PET release film or separate-type paper protection on adhesive film two sides, can prevent the pollution of the environment adhesive film.
The invention provides a kind of preparation method of adhesive composite described above, described preparation method comprises the following steps:
(1a) in high dielectric ceramic powder, add organic solvent, dispersion agent, coupling agent, toning agent, be uniformly dispersed;
(2a) after then adding matrix resin, solidifying agent, curing catalyst, redispersion is carried out to it, stirs, obtain described caking agent;
Or described preparation method comprises the following steps:
(1b) disperse after matrix resin, solidifying agent, curing catalyst, dispersion agent, coupling agent, high dielectric ceramic powder, toning agent and organic solvent being mixed;
(2b) carry out redispersion after dispersion, obtain described adhesive composite.
Preferably, in step (1a), (1b), dispersing apparatus used is selected from one or more in high speed disintegrator, ball mill, planet mill, sand mill and planetary mixer; Redispersion equipment used in step (2a), (2b) is selected from one or more in high speed disintegrator, ball mill, planet mill, sand mill, planetary mixer and three-high mill.
The present invention is by adding the inorganic ceramic powder of high-k, and disperse modified process has been carried out to ceramic powder, improve the consistency of ceramic powder, can be dispersed in matrix resin, do not affect solidification and the adhesion properties of matrix resin, and interference can not be caused to Signal transmissions.Meanwhile, by adding toning agent, making it also have shading and toning effect, simplifying packaging process.Adhesive composite is made adhesive film by the mode of flow casting molding by the present invention, and the adhesive film made has the advantages such as film forming thickness is even, paste shape is controlled, can not produce bubble, assembly technology is simple, is particularly suitable for plane adhesion assembling.
The using method of adhesive film volume of the present invention is as follows: first adhesive film volume is die-cut into required shape, then removes the release film on adhesive film two sides, then assembled by the mode being attached to element surface, can be bonding by being heating and curing.Solidification value preferably solidifies 10 ~ 60min at 100 ~ 180 DEG C.
Beneficial effect of the present invention is: the invention provides a kind of adhesive film, be characterized in that assembling is simple, there is relative permittivity simultaneously high, its relative permittivity is more than 6, the features such as opacifying property is good, Color tunable, bonding force are strong, be specially adapted to the bonding of capacitance type fingerprint identification chip module packaging, can transmit capacitance signal and can not cause capacitance signal conductively-closed or be reflected after encapsulation, its adhering object can be bonding etc. between sapphire, glass, pottery, plastic cement, silicon.This adhesive film is a kind of semicure adhesive film, at room temperature viscosity is lower, but has very strong viscosity when thermofixation, and its using method is be die-cut into required shape in advance, mode again by being attached to element surface is assembled, can be bonding by being heating and curing.Compare common some glue formula bonding way, adhesive film provided by the invention has the advantages such as film forming thickness is even, paste shape is controlled, can not produce bubble, assembly technology is simple, is particularly suitable for plane adhesion assembling.The invention provides a kind of adhesive composite for the formation of described adhesive film, described adhesive composite has relative permittivity high.Present invention also offers a kind of adhesive film volume, protected by described adhesive film by the PET release film or separate-type paper being covered in described adhesive film two sides in described adhesive film volume, can prevent the pollution of the environment adhesive film.
Embodiment
For better the object, technical solutions and advantages of the present invention being described, below in conjunction with specific embodiment, the invention will be further described.
Embodiment 1
A kind of embodiment of adhesive film of the present invention, the adhesive composite for the preparation of described adhesive film comprises the component of following weight part: barium titanate (BaTiO
3) 50 parts, titanium dioxide (TiO
2) 10 parts, Yelkin TTS dispersion agent 1.0 parts, silane resin acceptor kh-550 is 5 parts, each 8 parts of toluene, dehydrated alcohol, butanone, SBS resin 20 parts, epoxy resin 80 parts, Dyhard RU 100 1 part, imidazoles curing catalyst 0.2 part.
Described high dielectric ceramic powder is barium titanate (BaTiO
3), described dispersion agent is Yelkin TTS dispersion agent, described coupling agent is silane resin acceptor kh-550, described organic solvent is the mixture of toluene, dehydrated alcohol and butanone, described matrix resin is the mixture of styrene-butadiene block copolymer (SBS) resin and epoxy resin, described solidifying agent is Dyhard RU 100, and described curing catalyst is imidazoles, and described toning agent is titanium dioxide.
A kind of embodiment of the preparation method of adhesive film described above, said method comprising the steps of:
(1) after barium titanate, titanium dioxide, Yelkin TTS dispersion agent, silane resin acceptor kh-550 being mixed with toluene, dehydrated alcohol, butanone in ball mill ball milling 6h;
(2) add SBS resin, epoxy resin, Dyhard RU 100, imidazoles curing catalyst continuation ball milling 8h, obtain adhesive composite;
(3) the adhesive composite film casting machine curtain coating in step (2) is become the adhensive membrane of 5 μm.
After the two sides of above-mentioned adhesive film respectively being covered one deck PET release film, obtain adhensive membrane volume, vacuumize packaging.
Embodiment 2
A kind of embodiment of adhesive film of the present invention, the adhesive composite for the preparation of described adhesive film comprises the component of following weight part: strontium-barium titanate (Sr
0.2ba
0.8tiO
3) 60 parts, superfine amorphousn carbon black 5 parts, dispersion agent KD-1 be 1.0 parts, silane coupling agent KH-560 is 5 parts, each 6 parts of toluene, Virahol, ethylene glycol monobutyl ether, SBS resin 20 parts, polyurethane modified epoxy resin 80 parts, diaminodiphenylsulfone(DDS) 3 parts, imidazoles curing catalyst 0.5 part.
Described high dielectric ceramic powder is strontium-barium titanate (Sr
0.2ba
0.8tiO
3), described dispersion agent is dispersion agent KD-1, described coupling agent is silane coupling agent KH-560, described organic solvent is the mixture of toluene, Virahol and ethylene glycol monobutyl ether, described matrix resin is the mixture of SBS resin and polyurethane modified epoxy resin, described solidifying agent is diaminodiphenylsulfone(DDS), and described curing catalyst is imidazoles, and described toning agent is superfine amorphousn carbon black.
A kind of embodiment of the preparation method of adhesive film of the present invention, said method comprising the steps of:
1) after strontium-barium titanate, superfine amorphousn carbon black, dispersion agent KD-1, silane coupling agent KH-560 being mixed with toluene, Virahol, ethylene glycol monobutyl ether in sand mill sand milling 2h;
2) add SBS resin, polyurethane modified epoxy resin, diaminodiphenylsulfone(DDS), imidazoles curing catalyst continuation sand milling 2h, obtain adhesive composite;
3) the adhesive composite film casting machine curtain coating in step (2) is become the adhensive membrane of 20 μm.
After the two sides of above-mentioned adhesive film respectively being covered one deck PET release film, obtain adhensive membrane volume, vacuumize packaging.
Embodiment 3
A kind of embodiment of adhesive film of the present invention, the adhesive composite for the preparation of described adhesive film comprises the component of following weight part: zirconium barium calcium titanate (Ca
0.2ba
0.8zr
0.1ti
0.9o
3) 40 parts, titanium dioxide (TiO
2) 15 parts, dispersion agent KD-4 is 1.0 parts, titanate coupling agent TM-33 is 3 parts, each 6 parts of toluene, butylacetate, ethylene glycol monobutyl ether, poly(vinylidene fluoride) (PVDF) 20 parts, modified epoxy 80 parts, diaminodiphenylsulfone(DDS) 2 parts, organic urea 1 part.
Described high dielectric ceramic powder is zirconium barium calcium titanate (Ca
0.2ba
0.8zr
0.1ti
0.9o
3), described dispersion agent is dispersion agent KD-4, described coupling agent is titanate coupling agent TM-33, described organic solvent is the mixture of toluene, butylacetate and ethylene glycol monobutyl ether, described matrix resin is the mixture of poly(vinylidene fluoride) (PVDF) and modified epoxy, described solidifying agent is diaminodiphenylsulfone(DDS), and described curing catalyst is organic urea, and described toning agent is titanium dioxide (TiO
2).
A kind of embodiment of the preparation method of adhesive film of the present invention, said method comprising the steps of:
(1) after zirconium barium calcium titanate, titanium dioxide, dispersion agent KD-4, titanate coupling agent TM-33 being mixed with toluene, butylacetate and ethylene glycol monobutyl ether in sand mill sand milling 2h;
(2) poly(vinylidene fluoride) (PVDF), modified epoxy, diaminodiphenylsulfone(DDS) continuation sand milling 3h is added;
(3) add promotor organic urea planet stirring 0.5h, obtain adhesive composite;
(4) the adhesive composite film casting machine curtain coating in step (3) is become the adhensive membrane of 10 μm.
After the two sides of above-mentioned adhesive film respectively being covered one deck PET release film, obtain adhensive membrane volume, vacuumize packaging.
Embodiment 4
A kind of embodiment of adhesive film of the present invention, the adhesive composite for the preparation of described adhesive film comprises the component of following weight part: potassium-sodium niobate (K
0.5na
0.5nbO
3) 80 parts, superfine amorphousn carbon black 3 parts, dispersion agent KD-1 be 1.0 parts, titanate coupling agent TM-58 is 1.5 parts, each 8 parts of toluene, butanone and ethylene glycol monobutyl ether, SIS resin 10 parts, Hydroxylated acrylic resin 90 parts, amino curing agent 10 parts.
Described high dielectric ceramic powder is potassium-sodium niobate (K
0.5na
0.5nbO
3), described dispersion agent is dispersion agent KD-1, described coupling agent is titanate coupling agent TM-58, described organic solvent is the mixture of toluene, butanone and ethylene glycol monobutyl ether, described matrix resin is the mixture of SIS resin and Hydroxylated acrylic resin, described solidifying agent is amino curing agent, and described toning agent is superfine amorphousn carbon black.
A kind of embodiment of the preparation method of adhesive film of the present invention, said method comprising the steps of:
(1) after potassium-sodium niobate, superfine amorphousn carbon black, dispersion agent KD-1, titanate coupling agent TM-58 being mixed with toluene, butanone and ethylene glycol monobutyl ether in ball mill ball milling 4h;
(2) add SIS resin, Hydroxylated acrylic resin etc. and continue ball milling 4h;
(3) add amino curing agent stirrer and stir 0.5h, obtain adhesive composite;
(4) by step, (the adhesive composite film casting machine curtain coating in 3 becomes the adhensive membrane of 25 μm.
After the two sides of above-mentioned adhesive film respectively being covered one deck PET release film, obtain adhensive membrane volume, vacuumize packaging.
Embodiment 5
A kind of embodiment of adhesive film of the present invention, the adhesive composite for the preparation of described adhesive film comprises the component of following weight part: barium titanate (BaTiO
3) 70 parts, superfine amorphousn carbon black 5 parts, dispersion agent KD-4 be 0.5 part, silane resin acceptor kh-550 is 2.0 parts, toluene and each 15 parts of ethylene glycol monoethyl ether, SIS resin 10 parts, phenol aldehyde modified epoxy resin 90 parts, amino curing agent 10 parts.
Described high dielectric ceramic powder is barium titanate (BaTiO
3), described dispersion agent is dispersion agent KD-4, described coupling agent is silane resin acceptor kh-550, described organic solvent is the mixture of toluene and ethylene glycol monoethyl ether, described matrix resin is the mixture of SIS resin and phenol aldehyde modified epoxy resin, described solidifying agent is amino curing agent, and described toning agent is superfine amorphousn carbon black.
A kind of embodiment of the preparation method of adhesive film of the present invention, said method comprising the steps of:
(1) after barium titanate, superfine amorphousn carbon black, dispersion agent KD-4, silane resin acceptor kh-550 being mixed with toluene and ethylene glycol monoethyl ether in ball mill ball milling 4h;
(2) add SIS resin, phenol aldehyde modified epoxy resin continues ball milling 4h;
(3) add amino curing agent stirrer and stir 0.5h, obtain adhesive composite;
(4) the adhesive composite film casting machine curtain coating in step (3) is become the adhensive membrane of 15 μm.
After the two sides of above-mentioned adhesive film respectively being covered one deck PET release film, obtain adhensive membrane volume, vacuumize packaging.
Embodiment 6
A kind of embodiment of adhesive film of the present invention, the adhesive composite for the preparation of described adhesive film comprises the component of following weight part: zirconium barium calcium titanate (Ca
0.1ba
0.9zr
0.1ti
0.9o
3) 60 parts, superfine titanic oxide 10 parts, dispersion agent KD-1 be 1.5 parts, silane resin acceptor kh-550 is 3 parts, each 12 parts of toluene, ethylene glycol monobutyl ether, SIS resin 20 parts, phenol aldehyde modified epoxy resin 80 parts, amino curing agent 10 parts.
Described high dielectric ceramic powder is zirconium barium calcium titanate (Ca
0.1ba
0.9zr
0.1ti
0.9o
3), described dispersion agent is dispersion agent KD-1, described coupling agent is silane resin acceptor kh-550, described organic solvent is the mixture of toluene and ethylene glycol monobutyl ether, described matrix resin is the mixture of SIS resin and phenol aldehyde modified epoxy resin, described solidifying agent is amino curing agent, and described toning agent is superfine titanic oxide.
A kind of embodiment of the preparation method of adhesive film of the present invention, said method comprising the steps of:
(1) after mineral filler zirconium barium calcium titanate, superfine amorphousn carbon black, dispersion agent KD-4, silane resin acceptor kh-550 being mixed with toluene, ethylene glycol monobutyl ether in ball mill ball milling 4h;
(2) add SIS resin, phenol aldehyde modified epoxy continues ball milling 4h;
(3) add amino curing agent stirrer and stir 0.5h, obtain adhesive composite;
(4) the adhesive composite film casting machine curtain coating in step (3) is become the adhensive membrane of 20 μm.
After the two sides of above-mentioned adhesive film respectively being covered one deck PET release film, obtain adhensive membrane volume, vacuumize packaging.
Embodiment 7
A kind of embodiment of adhesive film of the present invention, the adhesive composite for the preparation of described adhesive film comprises the component of following weight part: SrTiO
310 parts, Yelkin TTS dispersion agent 0.1 part, silane resin acceptor kh-550 is 0.1 part, each 3 parts of toluene, dehydrated alcohol, butanone, SBS resin 20 parts, epoxy resin 80 parts, Dyhard RU 100 5 parts, imidazoles curing catalyst 0.2 part.
Described high dielectric ceramic powder is SrTiO
3described dispersion agent is Yelkin TTS dispersion agent, described coupling agent is silane resin acceptor kh-550, described organic solvent is the mixture of toluene, dehydrated alcohol and butanone, described matrix resin is the mixture of styrene-butadiene block copolymer (SBS) resin and polyorganosiloxane resin, described solidifying agent is Dyhard RU 100, and described curing catalyst is imidazoles.
A kind of embodiment of the preparation method of adhesive film described above, said method comprising the steps of:
(1) by SrTiO
3, Yelkin TTS dispersion agent, silane resin acceptor kh-550 mix with toluene, dehydrated alcohol, butanone after in ball mill ball milling 6h;
(2) add SBS resin, polyorganosiloxane resin, Dyhard RU 100, imidazoles curing catalyst continuation ball milling 8h, obtain adhesive composite;
(3) the adhesive composite film casting machine curtain coating in step (2) is become the adhensive membrane of 5 μm.
After the two sides of above-mentioned adhesive film respectively being covered one deck PET release film, obtain adhensive membrane volume, vacuumize packaging.
Embodiment 8
A kind of embodiment of adhesive film of the present invention, the adhesive composite for the preparation of described adhesive film comprises the component of following weight part: MgZrO
3500 parts, superfine amorphousn carbon black 100 parts, dispersion agent KD-1 be 5 parts, silane coupling agent KH-560 is 10 parts, each 33 parts of toluene, Virahol, ethylene glycol monobutyl ether, SBS resin 20 parts, epoxy modified acrylic resin 80 parts, diaminodiphenylsulfone(DDS) 70 parts, imidazoles curing catalyst 3 parts.
Described high dielectric ceramic powder is MgZrO
3described dispersion agent is dispersion agent KD-1, described coupling agent is silane coupling agent KH-560, described organic solvent is the mixture of toluene, Virahol and ethylene glycol monobutyl ether, described matrix resin is the mixture of SBS resin and epoxy modified acrylic resin, described solidifying agent is diaminodiphenylsulfone(DDS), and described curing catalyst is imidazoles, and described toning agent is superfine amorphousn carbon black.
A kind of embodiment of the preparation method of adhesive film of the present invention, said method comprising the steps of:
1) by MgZrO
3, superfine amorphousn carbon black, dispersion agent KD-1, silane coupling agent KH-560 mix with toluene, Virahol, ethylene glycol monobutyl ether after in sand mill sand milling 2h;
2) add SBS resin, epoxy modified acrylic resin, diaminodiphenylsulfone(DDS), imidazoles curing catalyst continuation sand milling 2h, obtain adhesive composite;
3) the adhesive composite film casting machine curtain coating in step (2) is become the adhensive membrane of 20 μm.
After the two sides of above-mentioned adhesive film respectively being covered one deck PET release film, obtain adhensive membrane volume, vacuumize packaging.
Embodiment 9
A kind of embodiment of adhesive film of the present invention, the adhesive composite for the preparation of described adhesive film comprises the component of following weight part: SrZrO
3300 parts, titanium dioxide (TiO
2) 50 parts, dispersion agent KD-4 is 4 parts, titanate coupling agent TM-33 is 8 parts, each 20 parts of toluene, butylacetate, ethylene glycol monobutyl ether, poly(vinylidene fluoride) (PVDF) 20 parts, modified epoxy 80 parts, diaminodiphenylsulfone(DDS) 40 parts, organic urea 2 parts.
Described high dielectric ceramic powder is SrZrO
3described dispersion agent is dispersion agent KD-4, described coupling agent is titanate coupling agent TM-33, described organic solvent is the mixture of toluene, butylacetate and ethylene glycol monobutyl ether, described matrix resin is the mixture of poly(vinylidene fluoride) (PVDF) and modified epoxy, described solidifying agent is diaminodiphenylsulfone(DDS), and described curing catalyst is organic urea, and described toning agent is titanium dioxide (TiO
2).
A kind of embodiment of the preparation method of adhesive film of the present invention, said method comprising the steps of:
(1) by SrZrO
3, titanium dioxide, dispersion agent KD-4, titanate coupling agent TM-33 mix with toluene, butylacetate and ethylene glycol monobutyl ether after in sand mill sand milling 2h;
(2) poly(vinylidene fluoride) (PVDF), modified epoxy, diaminodiphenylsulfone(DDS) continuation sand milling 3h is added;
(3) add promotor organic urea planet stirring 0.5h, obtain adhesive composite;
(4) the adhesive composite film casting machine curtain coating in step (3) is become the adhensive membrane of 10 μm.
After the two sides of above-mentioned adhesive film respectively being covered one deck PET release film, obtain adhensive membrane volume, vacuumize packaging.
Embodiment 10
A kind of embodiment of adhesive film of the present invention, the adhesive composite for the preparation of described adhesive film comprises the component of following weight part: CaZrO
3200 parts, superfine amorphousn carbon black 3 parts, dispersion agent KD-1 be 3 parts, titanate coupling agent TM-58 is 6 parts, each 20 parts of toluene, butanone and ethylene glycol monobutyl ether, SIS resin 10 parts, Hydroxylated acrylic resin 90 parts, amino curing agent 30 parts.
Described high dielectric ceramic powder is CaZrO
3described dispersion agent is dispersion agent KD-1, described coupling agent is titanate coupling agent TM-58, described organic solvent is the mixture of toluene, butanone and ethylene glycol monobutyl ether, described matrix resin is the mixture of SIS resin and Hydroxylated acrylic resin, described solidifying agent is amino curing agent, and described toning agent is superfine amorphousn carbon black.
A kind of embodiment of the preparation method of adhesive film of the present invention, said method comprising the steps of:
(1) by CaZrO
3, superfine amorphousn carbon black, dispersion agent KD-1, titanate coupling agent TM-58 mix with toluene, butanone and ethylene glycol monobutyl ether after in ball mill ball milling 4h;
(2) add SIS resin, Hydroxylated acrylic resin etc. and continue ball milling 4h;
(3) add amino curing agent stirrer and stir 0.5h, obtain adhesive composite;
(4) by step, (the adhesive composite film casting machine curtain coating in 3 becomes the adhensive membrane of 25 μm.
After the two sides of above-mentioned adhesive film respectively being covered one deck PET release film, obtain adhensive membrane volume, vacuumize packaging.
Embodiment 11
A kind of embodiment of adhesive film of the present invention, adhesive composite for the preparation of described adhesive film comprises the component of following weight part: ZnO 100 parts, superfine amorphousn carbon black 5 parts, dispersion agent KD-4 are 2 parts, silane resin acceptor kh-550 is 4 parts, toluene and each 30 parts of ethylene glycol monoethyl ether, SIS resin 10 parts, phenol aldehyde modified epoxy resin 90 parts, amino curing agent 10 parts.
Described high dielectric ceramic powder is ZnO, described dispersion agent is dispersion agent KD-4, described coupling agent is silane resin acceptor kh-550, described organic solvent is the mixture of toluene and ethylene glycol monoethyl ether, described matrix resin is the mixture of SIS resin and phenol aldehyde modified epoxy resin, described solidifying agent is amino curing agent, and described toning agent is superfine amorphousn carbon black.
A kind of embodiment of the preparation method of adhesive film of the present invention, said method comprising the steps of:
(1) after ZnO, superfine amorphousn carbon black, dispersion agent KD-4, silane resin acceptor kh-550 being mixed with toluene and ethylene glycol monoethyl ether in ball mill ball milling 4h;
(2) add SIS resin, phenol aldehyde modified epoxy resin continues ball milling 4h;
(3) add amino curing agent stirrer and stir 0.5h, obtain adhesive composite;
(4) the adhesive composite film casting machine curtain coating in step (3) is become the adhensive membrane of 15 μm.
After the two sides of above-mentioned adhesive film respectively being covered one deck PET release film, obtain adhensive membrane volume, vacuumize packaging.
Embodiment 12
A kind of embodiment of adhesive film of the present invention, the adhesive composite for the preparation of described adhesive film comprises the component of following weight part: CaTiO
360 parts, superfine titanic oxide 10 parts, dispersion agent KD-1 be 1.5 parts, silane resin acceptor kh-550 is 3 parts, each 12 parts of toluene, ethylene glycol monobutyl ether, SIS resin 20 parts, phenol aldehyde modified epoxy resin 80 parts, amino curing agent 10 parts.
Described high dielectric ceramic powder is CaTiO
3described dispersion agent is dispersion agent KD-1, described coupling agent is silane resin acceptor kh-550, described organic solvent is the mixture of toluene and ethylene glycol monobutyl ether, described matrix resin is the mixture of SIS resin and phenol aldehyde modified epoxy resin, described solidifying agent is amino curing agent, and described toning agent is superfine titanic oxide.
A kind of embodiment of the preparation method of adhesive film of the present invention, said method comprising the steps of:
(1) by CaTiO
3, superfine amorphousn carbon black, dispersion agent KD-4, silane resin acceptor kh-550 mix with toluene and ethylene glycol monobutyl ether after in ball mill ball milling 4h;
(2) add SIS resin, phenol aldehyde modified epoxy continues ball milling 4h;
(3) add amino curing agent stirrer and stir 0.5h, obtain adhesive composite;
(4) the adhesive composite film casting machine curtain coating in step (3) is become the adhensive membrane of 20 μm.
After the two sides of above-mentioned adhesive film respectively being covered one deck PET release film, obtain adhensive membrane volume, vacuumize packaging.
Embodiment 13
A kind of embodiment of adhesive film of the present invention, the adhesive composite for the preparation of described adhesive film comprises the component of following weight part: barium titanate (BaTiO
3) 50 parts, titanium dioxide (TiO
2) 10 parts, Yelkin TTS dispersion agent 1.0 parts, silane resin acceptor kh-550 is 5 parts, each 8 parts of toluene, dehydrated alcohol, butanone, SBS resin 20 parts, epoxy resin 80 parts, Dyhard RU 100 1 part, imidazoles curing catalyst 0.2 part.
Described high dielectric ceramic powder is barium titanate (BaTiO
3), described dispersion agent is Yelkin TTS dispersion agent, described coupling agent is silane resin acceptor kh-550, described organic solvent is the mixture of toluene, dehydrated alcohol and butanone, described matrix resin is the mixture of styrene-butadiene block copolymer (SBS) resin and epoxy resin, described solidifying agent is Dyhard RU 100, and described curing catalyst is imidazoles, and described toning agent is titanium dioxide.
A kind of embodiment of the preparation method of adhesive film described above, said method comprising the steps of:
(1) by SBS resin, epoxy resin, Dyhard RU 100, imidazoles curing catalyst, Yelkin TTS dispersion agent, silane resin acceptor kh-550, barium titanate, titanium dioxide and toluene, dehydrated alcohol, butanone mixing after in ball mill ball milling 6h;
(2) continue ball milling 8h, obtain described adhesive composite.
(3) the adhesive composite film casting machine curtain coating in step (2) is become the adhensive membrane of 5 μm.
After the two sides of above-mentioned adhesive film respectively being covered one deck PET release film, obtain adhensive membrane volume, vacuumize packaging.
Embodiment 14
A kind of embodiment of adhesive film of the present invention, the adhesive composite for the preparation of described adhesive film comprises the component of following weight part: strontium-barium titanate (Sr
0.2ba
0.8tiO
3) 60 parts, superfine amorphousn carbon black 5 parts, dispersion agent KD-1 be 1.0 parts, silane coupling agent KH-560 is 5 parts, each 6 parts of toluene, Virahol, ethylene glycol monobutyl ether, SBS resin 20 parts, polyurethane modified epoxy resin 80 parts, diaminodiphenylsulfone(DDS) 3 parts, imidazoles curing catalyst 0.5 part.
Described high dielectric ceramic powder is strontium-barium titanate (Sr
0.2ba
0.8tiO
3), described dispersion agent is dispersion agent KD-1, described coupling agent is silane coupling agent KH-560, described organic solvent is the mixture of toluene, Virahol and ethylene glycol monobutyl ether, described matrix resin is the mixture of SBS resin and polyurethane modified epoxy resin, described solidifying agent is diaminodiphenylsulfone(DDS), and described curing catalyst is imidazoles, and described toning agent is superfine amorphousn carbon black.
A kind of embodiment of the preparation method of adhesive film of the present invention, said method comprising the steps of:
1) by SBS resin, polyurethane modified epoxy resin, diaminodiphenylsulfone(DDS), imidazoles curing catalyst, strontium-barium titanate, superfine amorphousn carbon black, dispersion agent KD-1, silane coupling agent KH-560 and toluene, Virahol and ethylene glycol monobutyl ether mixing after in sand mill sand milling 2h;
2) continue sand milling 2h, obtain adhesive composite;
3) the adhesive composite film casting machine curtain coating in step (2) is become the adhensive membrane of 20 μm.
After the two sides of above-mentioned adhesive film respectively being covered one deck PET release film, obtain adhensive membrane volume, vacuumize packaging.
Embodiment 15
Relative permittivity measures:
By gold-plated for the adhesive film top and bottom obtained in embodiment 1-14, at frequency 1MHz, under voltage 1V condition, measure electric capacity, drawn the relative permittivity of above 14 examples by formulae discovery.
Cohesive strength measures:
Cohesive strength measures required equipment: ZrO pottery Eight characters mould (contact area 15*15mm), tensilon.
Cohesive strength measuring method: the binder film prepared by embodiment 1-14 covers in the contact area on Eight characters mould, leaves standstill 24h after solidification, tests cohesive strength with tensilon.
The relative permittivity of adhesive film prepared by embodiment 1-14 and the measurement result of cohesive strength as shown in table 1, from the test result of table 1, the relative permittivity of adhesive film prepared by the present invention meets relative permittivity ε r >=6 completely, can ensure that capacitance signal can be transferred on chip smoothly, and maintain high cohesive strength.
The performance test of the adhesive film obtained in table 1 embodiment 1-14
Finally to should be noted that; above embodiment is only in order to illustrate technical scheme of the present invention but not limiting the scope of the invention; although be explained in detail the present invention with reference to preferred embodiment; those of ordinary skill in the art is to be understood that; can modify to technical scheme of the present invention or equivalent replacement, and not depart from essence and the scope of technical solution of the present invention.
Claims (10)
1. an adhesive composite, it is characterized in that, described adhesive composite comprises the component of following weight part: matrix resin 100 parts, solidifying agent 5-70 part, curing catalyst 0-3 part, 10 ~ 500 parts, high dielectric ceramic powder, organic solvent 9 ~ 90 parts, dispersion agent 0.1 ~ 5 part, coupling agent 0.1 ~ 10 part, toning agent 0 ~ 100 part.
2. adhesive composite according to claim 1, it is characterized in that, described matrix resin is at least one in styrene-isoprene block copolymer, styrene-butadiene block copolymer, polyorganosiloxane resin, polyvinylidene fluoride resin, epoxy resin, thermosetting acrylic resin and their composite modified resin, at least containing a kind of thermosetting resin in described matrix resin.
3. adhesive composite according to claim 1, it is characterized in that, described solidifying agent is modified sulphur alkylol cpd, imidazoles, modified multicomponent amine, Dyhard RU 100, dicyandiamide modified thing, at least one in modified polyamide and diaminodiphenylsulfone(DDS), described curing catalyst is organic urea or imidazoles, described organic solvent is dehydrated alcohol, acetone, butanone, toluene, Virahol, ethyl acetate, butylacetate, ethylene glycol monoethyl ether, at least one in ethylene glycol monobutyl ether, described dispersion agent is at least one in negatively charged ion and non-ionic dispersing agent, described coupling agent is silane coupling agent or titanate coupling agent, described toning agent is carbon black, one in titanium dioxide and gas-phase silica.
4. adhesive composite according to claim 1, is characterized in that, described high dielectric ceramic powder is TiO
2, ZrO
2, BaTiO
3, CaTiO
3, ZnO, CaZrO
3, MgZrO
3, Ba
xsr
1-xti
yzr
1-yo
3(x, y=0 ~ 1), Ca
yba
1-yzr
xti
1-xo3 (x, y=0 ~ 1), K
xna
1-xnbO
3at least one in (x=0 ~ 1).
5. adhesive composite according to claim 4, is characterized in that, described high dielectric ceramic powder is spherical or class is spherical, and its particle diameter is 0.01 μm ~ 2 μm.
6. an adhesive film, is characterized in that, described adhesive film is by being shaped to membranaceous by the adhesive composite as described in as arbitrary in claim 1-5.
7. adhesive film according to claim 6, is characterized in that, described molding mode is flow casting molding.
8. adhesive film according to claim 6, is characterized in that, the thickness of described adhesive film is 2 μm ~ 100 μm.
9. adhesive film volume, is characterized in that, the three-decker that described adhesive film volume is formed for all being covered one deck PET release film or separate-type paper by the two sides of the adhesive film as described in as arbitrary in claim 6-8.
10. a preparation method for the adhesive composite as described in as arbitrary in claim 1-5, it is characterized in that, described preparation method comprises the following steps:
(1a) in high dielectric ceramic powder, add organic solvent, dispersion agent, coupling agent, toning agent, be uniformly dispersed;
(2a) after then adding matrix resin, solidifying agent, curing catalyst, redispersion is carried out to it, stirs, obtain described caking agent;
Or described preparation method comprises the following steps:
(1b) disperse after matrix resin, solidifying agent, curing catalyst, dispersion agent, coupling agent, high dielectric ceramic powder, toning agent and organic solvent being mixed;
(2b) carry out redispersion after dispersion, obtain described adhesive composite.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106519992A (en) * | 2016-11-18 | 2017-03-22 | 广东昭信照明科技有限公司 | Adhesive and preparation method thereof |
| CN106630975A (en) * | 2016-12-28 | 2017-05-10 | 广东昭信照明科技有限公司 | Flexible composite ceramic material and preparation method thereof |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002060514A (en) * | 2000-08-17 | 2002-02-26 | Mitsubishi Gas Chem Co Inc | Method for producing prepreg |
| US20050137293A1 (en) * | 2003-12-23 | 2005-06-23 | Industrial Technology Research Institute | Organic-inorganic hybrid compositions with high dielectric constant and high thermal stability, and cured compositions thereof |
| CN101503558A (en) * | 2008-02-04 | 2009-08-12 | 财团法人工业技术研究院 | Deflectivity and low dielectric loss composition and preparation thereof |
| CN101855074A (en) * | 2007-09-14 | 2010-10-06 | 奥克-三井有限公司 | Polymer-ceramic composites with excellent TCC |
| CN103374204A (en) * | 2012-04-25 | 2013-10-30 | 富葵精密组件(深圳)有限公司 | Epoxy resin composite material, film and circuit substrate |
| CN103374202A (en) * | 2012-04-23 | 2013-10-30 | 富葵精密组件(深圳)有限公司 | Epoxy resin composite material, film and circuit board |
-
2015
- 2015-01-13 CN CN201510017200.2A patent/CN104592924A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002060514A (en) * | 2000-08-17 | 2002-02-26 | Mitsubishi Gas Chem Co Inc | Method for producing prepreg |
| US20050137293A1 (en) * | 2003-12-23 | 2005-06-23 | Industrial Technology Research Institute | Organic-inorganic hybrid compositions with high dielectric constant and high thermal stability, and cured compositions thereof |
| CN101855074A (en) * | 2007-09-14 | 2010-10-06 | 奥克-三井有限公司 | Polymer-ceramic composites with excellent TCC |
| CN101503558A (en) * | 2008-02-04 | 2009-08-12 | 财团法人工业技术研究院 | Deflectivity and low dielectric loss composition and preparation thereof |
| CN103374202A (en) * | 2012-04-23 | 2013-10-30 | 富葵精密组件(深圳)有限公司 | Epoxy resin composite material, film and circuit board |
| CN103374204A (en) * | 2012-04-25 | 2013-10-30 | 富葵精密组件(深圳)有限公司 | Epoxy resin composite material, film and circuit substrate |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2017191528A1 (en) * | 2016-05-06 | 2017-11-09 | Sabic Global Technologies, B.V. | Barium titanate particles incorporated in polyetherimide based composite films with enhanced remnant polarization and methods of making same |
| CN109071849A (en) * | 2016-05-06 | 2018-12-21 | 沙特基础工业全球技术公司 | It include the barium titanate particles and preparation method thereof in the polyetherimide based coextruded film of the residual polarization with enhancing |
| CN106519992A (en) * | 2016-11-18 | 2017-03-22 | 广东昭信照明科技有限公司 | Adhesive and preparation method thereof |
| CN106630975A (en) * | 2016-12-28 | 2017-05-10 | 广东昭信照明科技有限公司 | Flexible composite ceramic material and preparation method thereof |
| CN106897709A (en) * | 2017-03-08 | 2017-06-27 | 广东欧珀移动通信有限公司 | Fingerprint recognition module and electronic installation |
| CN107316034A (en) * | 2017-07-18 | 2017-11-03 | 广东越众光电科技有限公司 | A kind of fingerprint module and preparation method thereof |
| CN108102583A (en) * | 2017-12-20 | 2018-06-01 | 江苏斯瑞达新材料科技有限公司 | The lithium battery agent of acid-resistant sealant gluing and its preparation process |
| CN109054709A (en) * | 2018-06-29 | 2018-12-21 | 安徽尼古拉电子科技有限公司 | A kind of microelectronic product corrosion-resistant packaging plastic and preparation method thereof |
| CN110387209A (en) * | 2019-07-15 | 2019-10-29 | 天津大学 | A kind of high-voltage isulation barium titanate-Silica hydrogel composite material and preparation method and application |
| CN110436863A (en) * | 2019-08-15 | 2019-11-12 | 中都工程设计有限公司 | A kind of laying rural highway concrete special and preparation method thereof |
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Application publication date: 20150506 |