CN106553352A - The manufacture method of the duplexer with polyimide layer, the manufacture method of polyimide film - Google Patents
The manufacture method of the duplexer with polyimide layer, the manufacture method of polyimide film Download PDFInfo
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- CN106553352A CN106553352A CN201610873323.0A CN201610873323A CN106553352A CN 106553352 A CN106553352 A CN 106553352A CN 201610873323 A CN201610873323 A CN 201610873323A CN 106553352 A CN106553352 A CN 106553352A
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- Prior art keywords
- base material
- layer
- supporting base
- polyimide
- duplexer
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Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/06—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the heating method
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C69/00—Combinations of shaping techniques not provided for in a single one of main groups B29C39/00 - B29C67/00, e.g. associations of moulding and joining techniques; Apparatus therefore
- B29C69/02—Combinations of shaping techniques not provided for in a single one of main groups B29C39/00 - B29C67/00, e.g. associations of moulding and joining techniques; Apparatus therefore of moulding techniques only
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C41/00—Shaping by coating a mould, core or other substrate, i.e. by depositing material and stripping-off the shaped article; Apparatus therefor
- B29C41/24—Shaping by coating a mould, core or other substrate, i.e. by depositing material and stripping-off the shaped article; Apparatus therefor for making articles of indefinite length
- B29C41/30—Shaping by coating a mould, core or other substrate, i.e. by depositing material and stripping-off the shaped article; Apparatus therefor for making articles of indefinite length incorporating preformed parts or layers, e.g. moulding around inserts or for coating articles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C41/00—Shaping by coating a mould, core or other substrate, i.e. by depositing material and stripping-off the shaped article; Apparatus therefor
- B29C41/34—Component parts, details or accessories; Auxiliary operations
- B29C41/46—Heating or cooling
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C55/00—Shaping by stretching, e.g. drawing through a die; Apparatus therefor
- B29C55/02—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets
- B29C55/04—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets uniaxial, e.g. oblique
- B29C55/08—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets uniaxial, e.g. oblique transverse to the direction of feed
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C55/00—Shaping by stretching, e.g. drawing through a die; Apparatus therefor
- B29C55/02—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets
- B29C55/10—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets multiaxial
- B29C55/12—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets multiaxial biaxial
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B15/00—Layered products comprising a layer of metal
- B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B15/08—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B27/08—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/28—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42
- B32B27/281—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42 comprising polyimides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B38/00—Ancillary operations in connection with laminating processes
- B32B38/18—Handling of layers or the laminate
- B32B38/1825—Handling of layers or the laminate characterised by the control or constructional features of devices for tensioning, stretching or registration
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29K2079/00—Use of polymers having nitrogen, with or without oxygen or carbon only, in the main chain, not provided for in groups B29K2061/00 - B29K2077/00, as moulding material
- B29K2079/08—PI, i.e. polyimides or derivatives thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29L—INDEXING SCHEME ASSOCIATED WITH SUBCLASS B29C, RELATING TO PARTICULAR ARTICLES
- B29L2009/00—Layered products
- B29L2009/005—Layered products coated
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2379/00—Other polymers having nitrogen, with or without oxygen or carbon only, in the main chain
- B32B2379/08—Polyimides
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Laminated Bodies (AREA)
- Moulding By Coating Moulds (AREA)
- Manufacture Of Macromolecular Shaped Articles (AREA)
- Shaping By String And By Release Of Stress In Plastics And The Like (AREA)
- Application Of Or Painting With Fluid Materials (AREA)
Abstract
The present invention provides a kind of manufacture method of the duplexer with polyimide layer for being continuously manufactured by and reducing with curling, the manufacture method of polyimide film.A kind of manufacture method of the duplexer with polyimide layer, which is the manufacture method of the duplexer with more than one layer of polyimide layer in supporting base material, wherein：Including the flexible membrane using strip as supporting base material, polyamic acid solution or polyimide solution are coated in supporting base material and the application step of more than one layer of coating layer is formed；The heat treatment step heated when supporting base material of the conveyance with coating layer；In heat treatment step, by the mechanism for gripping the end of the width of supporting base material, simultaneously the end of the width of the supporting base material with coating layer is fixed or stretched in the direction of the width, simultaneously transport supporting base material in the transmission direction, and form polyimide layer.
Description
Technical field
The present invention relates to a kind of manufacture method of duplexer with polyimide layer and the polyamides Asia using the duplexer
The manufacture method of amine film and be provided with polyimide layer functional layer duplexer manufacture method.
Background technology
Polyimide film is excellent with polyimide film as flexible member.The present invention be suitable as touch panel, Obstruct membrane,
Liquid crystal indicator, organic electroluminescent (Electroluminescence, EL) display, organic EL illuminating, Electronic Paper, coloured silk
The manufacture method of the very thin polyimide film used in the flexible members such as colo(u)r filter, circuit substrate, coating.
For example, the display device such as liquid crystal indicator or organic EL display is used for the large-scale display as television set
Device, or the various display applications headed by the miniscopes such as mobile phone, personal computer, smart mobile phone.Wherein, for example having
In machine EL display devices, formation thin film transistor (TFT) (Thin Film Transistor, TFT) on the glass substrate, and then successively
Electrode, luminescent layer, electrode are formed, finally separately is hermetically sealed to make using glass substrate or plural layers etc..Having
In the structure of machine EL devices, with the bottom-emission structure for going out light from the glass substrate side draw as supporting base material and from work
The top lighting structure of light is taken out in glass substrate opposition side for supporting base material, and use is distinguished according to purposes.In addition, in structure
On, it would however also be possible to employ ambient light directly through structure, therefore it is also proposed that have can be from the transparent of the electronic components such as outside perspective TFT
Structure.Can be realized by the electrode with the transparency or selecting for baseplate material.
In these display devices, by glass substrate is substituted for resin substrate, it is capable of achieving more slim, light than existing
Amount, flexibility, can further expand purposes or the change of display device.But, compared with glass, resin general size is stable
Property, the transparency, heat resistance, moisture-proof, gas barrier property etc. be not good enough, therefore is just carrying out the various researchs to improve these characteristics.
For example, disclose to have in patent document 1 and use the base material film for possessing polyimide layer in supporting base material, by roller
Roller mode etc. is formed after functional layer, fid is separated and removed with the interface of fid using polyimide layer, thus
The laminate component for possessing functional layer on the thin resin film comprising polyimide layer can be obtained.
In addition, in non-patent literature 1 and non-patent literature 2, proposition has a kind of by the transparency high resin material application
In the organic EL display of supporting substrate.
Having recorded in patent document 2 and patent document 3 makes polyamic acid solution be cast on supporter, and carries out adding
Heat, is derived from the self-supporting film of Jing parts imidizate, which is peeled off from supporter, is growing which using extension apparatus
Extend on degree direction and width, and heated and obtained the polyimide film that completes imidizate.In the extension
In, using the stenter for possessing the mechanism for stretching in the direction of the width.Stenter possesses the mechanism of the end for gripping width,
Thus having makes film of strip etc. move in the longitudinal direction, and stretches in the direction of the width, thus carries out width
The function of extension.Generally with moving in the longitudinal direction, gradually expand the width of holding mechanism of two sides carrying out
The extension of the width.
[prior art literature]
[patent document]
[patent document 1] Japanese Patent Laid-Open 2014-166722 publication
[patent document 2] Japanese Patent Laid-Open 2013-82149 publication
[patent document 3] Japanese Patent Laid-Open 2004-2880 publication
[non-patent literature]
[non-patent literature 1] S.An et al.., " 2.8 inches of high performance low temperature multi-crystal TFT are used on plastic base
WQVGA flexibility AMOLED (2.8-inch WQVGA Flexible AMOLED Using High Performance Low
Temperature Polysilicon TFT on Plastic Substrates) ", SID2010DIGEST, p706 (2010)
[non-patent literature 2] Oishi et al.., " for clear polyimides (the Transparent PI of flexible display
For flexible display) ", IDW ' 11FLX2/FMC4-1
The content of the invention
[invention problem to be solved]
The duplexer for possessing polyimide layer in supporting base material lifts the operability of thin polyimide film, if but supporting
Base material is different with the linear expansion coefficient (Coefficient ofthermal expansion, CTE) of polyimide layer, then hard
Warpage is produced during cooling after change, process becomes difficult.
It is an object of the invention to provide a kind of in the duplexer for being attained in supporting base material the polyimide layer for possessing thin
Aspect, simplifies its drying, heat treatment step, and even CTE different combinations, also suppresses the manufacture method for crimping.
[technological means of solve problem]
The present inventor et al. carries out the result for making great efforts research to solve the problem, and having been found advantageous that will in holding
Polyamic acid solution or polyimide solution are hardened in the state of coating the two ends of the supporting base material in supporting base material, excellent
Choosing is hardened when extending, so as to complete the present invention.
The present invention is a kind of manufacture method of the duplexer with polyimide layer, and which is that in supporting base material have one layer
The manufacture method of the duplexer of polyimide layer above, wherein：Including using the flexible membrane of strip as supporting base material,
Polyamic acid solution or polyimide solution are coated in supporting base material and the application step of more than one layer of coating layer is formed；
The heat treatment step heated when supporting base material of the conveyance with coating layer；In the heat treatment step
In, the mechanism of the end of the width by gripping supporting base material, simultaneously by the width side of the supporting base material with coating layer
Fix to end or stretch in the direction of the width, simultaneously transport supporting base material in the transmission direction, and with the acyl of polyamic acid
The temperature and time or maximum temperature that imidization is completed becomes more than 200 DEG C of condition to carry out the heating, and is formed
Polyimide layer.
In the manufacture method of the duplexer with polyimide layer, 1 of following necessary conditions is preferably met
Or more than 2.
1) in heat treatment step, when supporting base material of the conveyance with coating layer in the transmission direction, in sender
Transport when stretching upwards.
2) more than one layer of coating layer in application step, is formed on the one or both sides of supporting base material.
3) flexible membrane is the resin film or metal forming of 25 μm～200 μ m-thicks.
4) supporting base material is polyimide resin film.
5) difference of the thermal coefficient of expansion of supporting base material and polyimide layer be more than 1ppm/K, or supporting base material with it is adjacent
The difference of the thermal coefficient of expansion of polyimide layer is more than 1ppm/K.
6) in heat treatment step, by the stretched film on the width of supporting base material, and prolonging with width
The rate of stretching becomes 100%～120% mode and is extended.
After heat treatment step, functional layer forming step is set, and it is this that functional layer is arranged on polyimide layer
The preferred form of the manufacture method of the duplexer of invention.
In addition, the present invention is a kind of manufacture method of polyimide film, wherein：By by described with polyimide layer
The duplexer obtained by the manufacture method of duplexer, peels off polyimides on interface of the supporting base material layer with polyimide layer
Layer, and make polyimide film.
When the duplexer obtained by the manufacture method of the duplexer with polyimide layer is with multilayer
During polyimide layer person, polyimide film is peeled off at least one interface at the interface of the polyimides interlayer to make
Polyimide film is other forms of the manufacture method of the polyimide film of the present invention.
[The effect of invention]
The manufacture method of the duplexer with polyimide layer of the invention, not from coated polyimides
Coating layer is temporarily separated with supporting base material in the supporting base material of layer or precursor layer (coating layer), and is directly heated
To complete hardening, therefore manufacturing step is simplified.In addition, one side be also carried out in the direction of the width extending or give tension force or
Confining force, is simultaneously heated, and thus can not only reduce the CTE of polyimide layer, and even each layer of duplexer
The different combinations of CTE, it is also possible to reduce curling, the stripping of the polyimide layer in roller conveyance step can be prevented, and make stacking
The process of body or roller becomes easy.
If after heat treatment step, arranging functional layer forming step, and functional layer being arranged on polyimide layer, its
Polyimide layer is peeled off on interface of the supporting base material layer with polyimide layer afterwards and the polyimide film with functional layer is made,
The flexible member with functional layer on thin polyimide film can then be effectively obtained.
Description of the drawings
Fig. 1 is the schematic diagram of of the device of the duplexer for representing the manufacture present invention.
Fig. 2 is the schematic diagram of another of the device of the duplexer for representing the manufacture present invention.
Fig. 3 is the plan of another of the device of the duplexer for representing the manufacture present invention.
[explanation of reference]
1：Apparatus for coating
2：Rotating roller
3：Takers-in
4：Supporting base material
5：Resin bed
6：2nd heating furnace
7：Grip tool
8：Roller
22、23：Rotating roller
61：Heating furnace
Specific embodiment
In the manufacture method of the duplexer with polyimide layer of the present invention, including by polyamic acid solution or polyamides
Imide liquor (hereinafter referred to as resin solution) be coated in supporting base material and formed the application step of more than one layer of coating layer, one
The heat treatment step heated by the conveyance one side of the supporting base material with coating layer in face.Herein, coating layer is at heating
Become polyimide layer after reason, but due to being resin bed, therefore resin bed is referred to as with the implication comprising both also.
Resin solution in polyamic acid solution and polyimide solution is coated in supporting base material.The coating can
One side, or two sides for supporting base material.If being arranged on two sides, 2 polyimide films can be obtained simultaneously.In addition,
Resin solution can be coated with one layer, it is also possible to be coated into multilayer, corresponding to polyimide film purposes determining.If being coated into many
Layer, and be set to strippable interlayer in polyimides interlayer, then by being peeled off in the interlayer, 2 polyamides can be obtained simultaneously
Imines film.
Polyamic acid or polyimides in polyamic acid solution or polyimide solution can be from the diamines as raw material
The polyamic acid obtained with tetracarboxylic dianhydride and/or tricarboxylic acid anhydride or polyimides.The diamines and tetracarboxylic dianhydride and/or
Tricarboxylic acid anhydride respectively can only comprising one kind, it is also possible to comprising various.
Generally, polyimides is to make to be polymerized with diamines as the acid anhydrides of raw material and obtained, can be by following formulas (1) table
Show.Polyamic acid is the predecessor of polyimides, can be made polyimides by being delivered to heating etc..Therefore,
Can understand polyamic acid according to the explanation of polyimides, thus by polyimides explanation representing.
[changing 1]
In formula, Ar1It is denoted as the organic group of the tetravalence of anhydride residue, Ar2It is the organic of divalence as diamines residue
Base, for the viewpoint of heat resistance, it is generally desirable to Ar1、Ar2At least one be aromatic residue.
There is no particular restriction for polyimides used in the present invention, as the 1st, can enumerate with following repetitive structures
The polyimides of unit (a).
[changing 2]
If the polyimides with constitutional repeating unit (a), then can form glass transition temperature as the 1st
(Tg) be more than 300 DEG C of heat resistant poly imide layer, and by forming this kind of polyimide layer, can make polyimide layer with
Separation on the interface of fid becomes easy.
In addition, as the 2nd of the polyimides that suitably can be used, fluorinated polyimide can be enumerated.Herein, it is so-called to contain
Fluorine polyimides, refers to there is fluorine atom in polyimide structures, and is in the acid anhydrides as polyimides raw material and two
In at least one composition of amine, with fluorine.As this kind of fluorinated polyimide, for example, can illustrate：By the formula (1) institute table
Ar among showing, in formula1For the organic group of tetravalence, Ar2Divalence by represented by with following formulas (2) or formula (3) it is organic
Basis representation.
[changing 3]
R in the formula (2) or formula (3)1～R8Independently of one another hydrogen atom, fluorine atom, the alkyl of carbon number 1～5
Or alkoxyl or fluorine substituted hydrocarbon radical, in formula (2), R1～R4At least one of be fluorine atom or fluorine substituted hydrocarbon radical, in addition, logical
In formula (3), R1～R8At least one of be fluorine atom or fluorine substituted hydrocarbon radical.Wherein, as R1～R8Suitable concrete example,
- H ,-CH can be enumerated3、-OCH3、-F、-CF3Deng, preferably in formula (2) or formula (3), at least one substituent be-F or-CF3's
Any one.
As polyimides be fluorinated polyimide when formula (1) in Ar1Concrete example, can for example be listed below
The anhydride residue of tetravalence.
[changing 4]
It is excellent comprising the transparency in fluorinated polyimide as described, it is thus suitable for expecting the poly- of the transparency
The purposes of acid imide film.For example, headed by the display device such as liquid crystal indicator or organic EL display, it is suitable as obtaining
Used in these display devices and require the transparency laminate component when polyimide layer.If consideration obtains its hyalinosis
It is more excellent, or further lift fissility on the interface of polyimide layer and fid etc., then following presentation offer formula (1)
In Ar2Specific diamines residue preference.
[changing 5]
In addition, when in this kind of fluorinated polyimide, with the ratio of 80 moles of more than % have act set forth below by formula
(4), formula (5) or the construction unit represented by formula (6) any one when, in addition to the transparency and fissility are excellent, thermal expansivity
Low and excellent in dimensional stability, therefore more preferably.That is, if with represented by following formulas (4), formula (5) or formula (6)
Construction unit polyimides, then the light penetration in the wavelength region of 440nm～780nm show more than 70%,
More than 80% is desirably shown, therefore gathering in transparent laminate component is required as display device etc. as being formed
Imide layer it is more favourable.In addition, becoming the glass transition temperature with more than 300 DEG C, and become thermal coefficient of expansion
Below 25ppm/K, desirably becomes below 10ppm/K.Therefore, by using this kind of polyimides, even if receiving in operation
To temperature change, both thermal coefficient of expansions are also close to therefore can preventing warpage or fold from concentrating.And, using polyimides
Resin film is used as supporting base material, and the polyimide resin film is together set to this kind of containing with the polyimide layer being formed thereon
Fluorine polyimides, thus prevents the effect that warpage or fold are concentrated from further being lifted.
[changing 6]
Comprising described 1st and the 2nd, polyimides can be containing producing from the diamines or acid anhydrides of alicyclic structure
Unit, as its example, can enumerate：CBDA (cyclobutane -1,2,3,4- tetracarboxylic dianhydrides), CHDA (1,2,4,5- hexamethylene dicarboxyls
Acid anhydrides) or anti-form-1,4- DACHs etc..
Comprising described 1st and the 2nd, imidizate can be carried out to polyamic acid and obtain polyimides.Herein,
The resin solution of polyamic acid using by substantial equimolar using the diamines as raw material and tetracarboxylic dianhydride and/or tricarboxylic acids
Acid anhydride, and reacted to be advisable in organic solvent.Specifically, can be by, under stream of nitrogen gas, being dissolved in diamines
After in the polar organic solvent such as DMA, add tetracarboxylic dianhydride and/or tricarboxylic acid anhydride, and react at room temperature
5 hours or so and obtain.For the viewpoint of the mechanical strength of uniform film thicknessization and the polyimide film for being obtained when applying,
The weight average molecular weight of the polyamic acid for being obtained preferably 10,000～300,000.Furthermore, the polyimide layer for being obtained it is preferred
Molecular weight ranges are also and the polyamic acid identical molecular weight ranges.In addition, polyimide layer can be formed by individual layer, it is also possible to
Formed by multilayer.When being formed by multilayer, the layer at least contacting with supporting base material is to use such as described 1st and the 2nd
Cited polyimides is advisable.
Supporting base material with flexibility, and can coating resin solution, heat terminate before, or shape behind
Will not peel off before terminating into steps such as functional layers, be advisable with the power person of being easily peeled off for fixing the above after terminating.And, properly
Be the polyimide resin that can be together extended with the resin being coated with or poly terephthalic acid second two when being extended
The resin films such as alcohol ester (Polyethylene terephthalate, PET).In addition, heretofore described flexible membrane is included
Copper Foil or SUS paper tinsels etc. have flexual metal forming etc., including sheet.The thickness of supporting base material is with 20 μm～500 μm of scope
It is advisable, preferably 25 μm～200 μm, more preferably 50 μm～100 μm of scope.
As supporting base material, preferred polyimide resin film.Dividing on the interface of polyimide layer and supporting base material is made just
For easy viewpoint is become, the surface roughness Ra on the surface of the supporting base material for preferably contacting with polyimide layer with
Below 100nm is advisable, preferred below 30nm.In addition, when being extended, supporting base material is suitably stretchy.
In the manufacture method of the present invention, it is advisable with heat treatment step with being continuously coated step, therefore, in order to
Continuously carry out sending, batch using roller, and application step and heat treatment step are set in a period of roller is moved, support
Base material is necessary for strip.So-called strip, be and comparing for supporting base material and the longer state in another side, when roller is formed,
Roller is formed in the way of long side is as direction of transfer.Furthermore, can have between application step and heat treatment step and be dried step
Suddenly other steps, drying steps are waited to carry out by different heating furnaces from the heating of heat treatment step.
In addition, in the manufacture method of the present invention, when the difference of the supporting base material thermal coefficient of expansion overall with polyimide layer
For more than 1ppm/K when or when the difference of supporting base material and the thermal coefficient of expansion of adjacent polyimide layer is more than 1ppm/K timeliness
Fruit is big.If the difference of thermal coefficient of expansion is big, curling is easily produced, but in the manufacture method of the present invention, curling can be reduced.Especially
Which, when the thermal coefficient of expansion of polyimide layer is more than supporting base material, easily produces curling, but manufacturer of the invention
Method, suppresses the increase of the thermal coefficient of expansion of polyimide layer, and prevents curling.In addition, by grip supporting base material end come
Prevent the warpage in heat treatment step.
In application step, coating thickness is not particularly limited, but in order to be applied to touch panel, liquid crystal display dress
Put, the purposes to the polyimide layer requirement transparency such as organic el display, organic EL illuminating, colored filter, and require poly-
The transmitance of imide layer is more than 80%, therefore preferably less than 30 μm of the thickness of polyimide layer, more preferably less than 20 μm, because
This is advisable with becoming this kind of thickness.
Preferred 5wt%～the 30wt% of concentration of the resin solution being coated with.Used as coating process, cast coat is suitably
Scraper coating machine or lip type coating machine, die coating machine etc..
After application step terminates, after being optionally dried, heat treatment step is delivered to.For example with 150 DEG C～160 DEG C
Left and right carries out heating to be dried, but part or all that can be dried in heat treatment step.Heating is
Carried out in the way of becoming to complete in maximum temperature the imidizate of polyamic acid at a temperature of 300 DEG C～450 DEG C.In acid imide
As long as what is carried out during change heats for example from 160 DEG C or so of temperature to 400 DEG C or so of temperature continuously or the stage
Heated up to property.
In application step, when using polyimide solution as resin solution, it is not necessary to imidizate, but need dry
Dry and heating, becomes under conditions of more than 200 DEG C in maximum temperature, preferably becomes more than 300 DEG C of bar in maximum temperature
Carry out under part.If being heated under the conditions of the temperature higher than drying condition or time etc., the spy of polyimide film
Property lifted.
In the heat treatment step, the mechanism of the end of the width by gripping supporting base material will simultaneously have
The width end of the supporting base material of coating layer is fixed or is stretched in the direction of the width, simultaneously transports film in the transmission direction.
As a result, the little polyimide film of (also referred to as amount of warpage) or CTE can be crimped.As by width end fix or
The device stretched on width, can use known tenter frame apparatus.It is so-called that the end of width is fixed, refer to enter
Row extends, but applies confining force or tensile force, and tension force is given to supporting base material or the position (for example, horizontal level) of end is protected
Hold as fixed power.It is so-called to stretch in the direction of the width, it is included on width and is extended.
By using stenter, can not only reduce the CTE of polyimide layer, and it is strong to increase the stretching of polyimide film
Degree.
Grip the end mechanism or shape there is no particular restriction, can illustrate grip both ends fixture or be pierced into two ends
The pin in portion etc..
The operation that width end is fixed or stretched in the direction of the width is preferably set to into following scope：Become 80 DEG C
More than, preferably become more than 160 DEG C of temperature, after maximum temperature is reached, become below the glass transition temperature of polyimides
Till scope.Specifically, preferably one side, by the gripping or stretching of supporting base material, simultaneously raises maximum temperature, is reaching
After maximum temperature, the glass transition temperature～glass transition temperature for being cooled to the polyimides for constituting polyimide layer subtracts 100 DEG C
Temperature range, while 90%～50% when the power of the stretching of width to be relaxed to intensification, and form polyimide layer.
By forming polyimide layer in this approach, the difference of the CTE and the CTE of width of the direction of transfer of polyimide layer can be obtained
It is little, and the little duplexer of amount of warpage.
Extending for length direction can be by adjustment takers-in and the speed of outlet roller, in the transmission direction when stretching
Moving is carried out.Therefore, in the manufacture method of the present invention, preferably entered in the way of becoming uniaxial extension film or biaxial stretchable film
Row extends.As elongation percentage, more than 1 times, preferably 1.2 times of scope.Can be crimped or CTE by the extension of length direction
Little polyimide film.
Referring to the drawings the manufacture method of the duplexer with polyimide layer of the present invention is illustrated.
Fig. 1 is the schematic diagram of that represents the device for manufacturing the duplexer, is extracted out by rotating roller 2 and prop up from roller 8
Support group material 4, is coated on resin solution on two sides using 2 apparatus for coating 1, and forms resin bed 5.It is formed with propping up for resin bed
Support group material is dried by heating furnace 61, is heated by the 2nd heating furnace 6 after multiple rotating rollers 22, rotating roller 23,
Then batched by takers-in 3.From in front of the entrance of the 2nd heating furnace 6 to the dead astern of outlet, possess with gripping tool 7
Stenter, the two ends of the supporting base material for keeping being formed with resin bed by the stenter, and be fixed or extend.
Fig. 2 represents another example of the device of manufacture duplexer, has identical implication with the symbol that Fig. 1 is shared.In the example
In, not with the heating furnace for drying, and in the 2nd heating furnace 6 it is dried and is heat-treated.Fig. 3 is the plane of stenter
Figure, the gripping tool 7 for being configured in two ends have the interval (distance) at two ends towards the part, the expansion for becoming larger that outlet side is fixation
Big portion and become fixed part.And, the expansion section is present in the 2nd heating furnace 6, and is extended wherein.Again
Person, when not extended, not with expansion section, but the supporting base material to being formed with resin bed gives certain tension force and comes in addition
It is fixed.
The duplexer with polyimide layer obtained through heat treatment step is peeled off with supporting base material and is made poly-
Acid imide film.When with multilayer polyimide layer, as long as polyimides interlayer is set to strippable, just can carry out wherein
Peel off.
In the present invention, by using polyimides illustrated above etc., can suitably by polyimide layer and support
Bonding strength on the interface of base material becomes 0.1N/m～20N/m, for example, can be easily peeled off by staff.From polyimides
The upper limit of peel strength when peeling off supporting base material on layer is according to the thickness of polyimide layer, the species of functional layer, stripping means
Deng and it is different, be not particularly limited.In order to prevent polyimide layer when duplexer is transported using roll-to-roll mode with a support group
Stripping on the interface of material, is advisable with being set to more than 0.1N/m.On the other hand, in order to be easily peeled off, to be set to below 20N/m it is
Preferably.
Further, when functional layer is arranged on polyimide film, as long as the duplexer before being peeled off arranges functional layer,
Then even thin polyimide film, the formation of functional layer also become easy.
Herein, called function layer, refers to composition liquid crystal indicator or organic EL display, Electronic Paper, touch panel
Etc. display device, vapor deposition mask, fan-out wafer level encapsulation (Fan-out Wafer Level Packaging, FOWLP) use base
The layer of plate, lighting device, detection means, or its constituent part constitutes various functions material layer, specifically, refer to as
One kind of electrode layer, luminescent layer, gas barrier layer, adhesive layer, adhesion coating, thin film transistor (TFT), wiring layer, transparency conducting layer etc. or by two
Plant combination of the above.
The polyimide film for being provided with functional layer can be used in organic el illumination device, or as being laminated with ITO's etc.
Conductive film, the gas barrier film of infiltration for preventing moisture or oxygen etc., constituent part of flexible circuit board etc. have various functions
Functional material.Desirably it is used as flexible member.
The polyimide film for being provided with functional layer is referred to as into flexible member, which is with the degree that can be bent by staff
Bendability e-machine element or e-machine component.The form that flexible member is mounted in e-machine can be
The bending purposes of Curvature varying during use, can be the indeclinable fixed curved surface of curvature, alternatively, it is also possible to being plane.
Herein, if the duplexer warpage with polyimide layer, operation becomes difficult, and not only its manufacture becomes tired
Difficulty, and the stacking of functional layer or the stripping etc. of polyimide layer become difficult, it is therefore important that curling is little.In order to suppress volume
Song, effectively makes supporting base material consistent with the CTE of polyimide layer, but supporting base material is limited with the selection of polyimides
System, it is therefore desirable that being controlled using additive method.Therefore, in heat treatment step, in order to reduce polyimide layer
CTE, and suppress curling, effectively width end is fixed or towards the stretched operation of width.
[embodiment]
Hereinafter, according to embodiment, the present invention is described in detail, but the present invention is not by the scope of below example
Limit.
The assay method of abbreviation and various physical property in following presentation embodiment and its condition.
TFMB：2,2 '-bis- (trifluoromethyl) -4,4 '-benzidine
6FDA：2,2 '-bis- (3,4- dicarboxyphenyi) hexafluoropropane dianhydrides
PMDA：Pyromellitic acid dianhydride
DMAc：DMA
Amount of warpage
Duplexer with polyimide layer is set to into lower section with supporting base material side, after cutting out into the size of 10cm × 10cm
Be placed on it is flat where, and judge the situation of the warpage of duplexer.By the mean value of 4 jiaos of duplexer piece of floatation volume (mm)
Numerical value be set to amount of warpage.Furthermore, negative value (-) is set to when supporting base material side tilts, be set to set when polyimide layer is tilted
It is on the occasion of (+).
Thermal coefficient of expansion：CTE
Polyimide layer is peeled off from the duplexer with polyimide layer to make polyimide film, and is set to width
Size of the direction (TD directions) as the 3mm × 15mm on long side, using thermo-mechanical analysis (Thermomechanical
Analysis, TMA) device, simultaneously apply 5.0g load, simultaneously with fixed programming rate (10 DEG C/min) 30 DEG C～
Tension test, and stretching according to the polyimide film relative to temperature are carried out within the temperature range of 280 DEG C to the polyimide film
It is long to measure the thermal coefficient of expansion (ppm/K) for determining width.In addition, being set to direction of transfer (MD directions) as the 3mm on long side
The size of × 15mm, with identical assay method, determines the thermal coefficient of expansion (ppm/K) of direction of transfer.
Synthesis example 1
In the reactor of 30L, the TFMB of 849g is dissolved in the DMAc of 7kg.Secondly, add 147g in the solution
6FDA and be stirred, add then the PMDA of 504g, and add 1.5kg's in the way of solid constituent becomes 15wt%
DMAc, is stirred at room temperature 5 hours to carry out polymerisation.After reaction, sticky transparent polyamic acid solution A is obtained.
Synthesis example 2
In the reactor of 30L, the TFMB of 765g is dissolved in the DMAc of 7kg.Secondly, add 423g in the solution
6FDA and be stirred, add then the PMDA of 311g, and add 1.5kg's in the way of solid constituent becomes 15wt%
DMAc, is stirred at room temperature 5 hours to carry out polymerisation.After reaction, sticky transparent polyamic acid solution B is obtained.
Synthesis example 3
In the reactor of 30L, the TFMB of 629g is dissolved in the DMAc of 7kg.Secondly, add 871g in the solution
6FDA and be stirred, add the DMAc of 1.5kg in the way of solid constituent becomes 15wt%, be stirred at room temperature 6 hours
To carry out polymerisation.After reaction, sticky water white polyamic acid solution C is obtained.
In below example and comparative example, as supporting base material, the use of thickness it is 75 μm, CTE gathering for 56ppm/K
Imide resin film (width 520mm, direction of transfer 200m).In addition, in addition to embodiment 9, the speed of roller will be rolled out
And the speed of takers-in is set to 0.5m/min.
Embodiment 1
Polyamic acid solution A obtained in synthesis example 1 is coated on into the polyimides of the strip as supporting base material
After on resin film, it is thermally dried at 120 DEG C and removes solvent.Then, simultaneously by the film of the width of supporting base material
End keeps, fixes, and is simultaneously heat-treated with the programming rate of about 30 DEG C/min to 360 DEG C from 180 DEG C, is consequently formed
Polyimide layer, and obtain the duplexer for possessing the polyimide layer that thickness is 10 μm.
Embodiment 2
Similarly to Example 1, the polyamic acid solution A obtained in synthesis example 1 is coated on as supporting base material
After on the polyimide resin film of strip, it is thermally dried at 120 DEG C and removes solvent.Then, simultaneously using gripping
Tool keeps the film end of the width of supporting base material, simultaneously supporting base material is moved into into heating furnace, and then one side is from 180 DEG C
It is heat-treated with the programming rate of about 30 DEG C/min to 360 DEG C, simultaneously makes supporting base material extend 2% in the direction of the width
To form polyimide layer.Acquisition possesses the duplexer of the polyimide layer that thickness is 10 μm.
Embodiment 3
Polyamic acid solution B obtained in synthesis example 2 is coated on into the polyimides of the strip as supporting base material
After on resin film, it is thermally dried at 120 DEG C and removes solvent.Then, simultaneously by the film of the width of supporting base material
End keeps, fixes, and is simultaneously heat-treated with the programming rate of about 30 DEG C/min to 360 DEG C from 180 DEG C, is consequently formed
Polyimide layer, and obtain the duplexer for possessing the polyimide layer that thickness is 10 μm.
Embodiment 4
Similarly to Example 3, the polyamic acid solution B obtained in synthesis example 2 is coated on as supporting base material
After on the polyimide resin film of strip, it is thermally dried at 120 DEG C and removes solvent.Then, simultaneously using gripping
Tool keeps the film end of the width of supporting base material, simultaneously supporting base material is moved into into heating furnace, and then one side is from 180 DEG C
It is heat-treated with the programming rate of about 30 DEG C/min to 360 DEG C, simultaneously makes supporting base material extend 2% in the direction of the width
To form polyimide layer.Acquisition possesses the duplexer of the polyimide layer that thickness is 10 μm.
Comparative example 1
Polyamic acid solution A obtained in synthesis example 1 is coated on into the polyimides of the strip as supporting base material
After on resin film, it is thermally dried at 120 DEG C and removes solvent.Then, film end is not kept and from 180 DEG C to 360 DEG C
Till be heat-treated with the programming rate of about 30 DEG C/min, be consequently formed polyimide layer, and obtain and possess thickness for 10 μm
Polyimide layer duplexer.
Comparative example 2
Polyamic acid solution B obtained in synthesis example 2 is coated on into the polyimides of the strip as supporting base material
After on resin film, it is thermally dried at 120 DEG C and removes solvent.Then, film end is not kept and from 180 DEG C to 360 DEG C
Till be heat-treated with the programming rate of about 30 DEG C/min, be consequently formed polyimide layer, and obtain and possess thickness for 10 μm
Polyimide layer duplexer.
Embodiment 5
Polyamic acid solution C obtained in synthesis example 3 is coated on into the polyimides of the strip as supporting base material
After on resin film, it is thermally dried at 120 DEG C and removes solvent.Then, simultaneously by the film of the width of supporting base material
End keeps, fixes, and is simultaneously heat-treated with the programming rate of about 30 DEG C/min to 360 DEG C from 180 DEG C, is consequently formed
Polyimide layer, and obtain the duplexer for possessing the polyimide layer that thickness is 10 μm.
Embodiment 6
Similarly to Example 5, the polyamic acid solution C obtained in synthesis example 3 is coated on as supporting base material
After on the polyimide resin film of strip, it is thermally dried at 120 DEG C and removes solvent.Then, simultaneously using gripping
Tool keeps the film end of the width of supporting base material, simultaneously supporting base material is moved into into heating furnace, and then one side is from 180 DEG C
It is heat-treated with the programming rate of about 30 DEG C/min to 360 DEG C, simultaneously makes supporting base material extend 2% in the direction of the width
To form polyimide layer.Acquisition possesses the duplexer of the polyimide layer that thickness is 10 μm.
Embodiment 7
Similarly to Example 6, the polyamic acid solution C obtained in synthesis example 3 is coated on as supporting base material
After on the polyimide resin film of strip, it is thermally dried at 120 DEG C and removes solvent.Then, simultaneously using gripping
Tool keeps the film end of the width of supporting base material, simultaneously supporting base material is moved into into heating furnace, and then one side is from 180 DEG C
It is heat-treated with the programming rate of about 30 DEG C/min to 360 DEG C, simultaneously makes supporting base material extend 5% in the direction of the width
To form polyimide layer.Acquisition possesses the duplexer of the polyimide layer that thickness is 10 μm.
Embodiment 8
Similarly to Example 6, the polyamic acid solution C obtained in synthesis example 3 is coated on as supporting base material
After on the polyimide resin film of strip, it is thermally dried at 120 DEG C and removes solvent.Then, simultaneously using gripping
Tool keeps the film end of the width of supporting base material, simultaneously supporting base material is moved into into heating furnace, and then one side is from 180 DEG C
It is heat-treated with the programming rate of about 30 DEG C/min to 360 DEG C, supporting base material is extended in the direction of the width
10% forming polyimide layer.Acquisition possesses the duplexer of the polyimide layer that thickness is 10 μm.
Embodiment 9
Polyamic acid solution A obtained in synthesis example 1 is coated on into the polyimides of the strip as supporting base material
After on resin film, it is thermally dried at 120 DEG C and removes solvent.Then, by with the speed (0.5m/ than rolling out roller
Min) fast 2% 0.51m/min is batched, simultaneously on longitudinal direction extend, simultaneously from 180 DEG C to 360 DEG C with about 30 DEG C/
The programming rate of min is heat-treated, and is formed polyimide layer, and is obtained the layer for possessing the polyimide layer that thickness is 10 μm
Stack.
Embodiment 10
Polyamic acid solution C obtained in synthesis example 3 is coated on into the polyimides of the strip as supporting base material
After on resin film, it is thermally dried at 120 DEG C and removes solvent.Then, the both ends of width are gripped, is simultaneously extended
20%, simultaneously it is heat-treated with the programming rate of about 30 DEG C/min to 360 DEG C from 180 DEG C, is then cooled to 250 DEG C,
Loosen the extension of width, elongation percentage is set to 16% to form polyimide layer.It is 10 μm poly- that acquisition possesses thickness
The duplexer of imide layer.
Comparative example 3
After polyamic acid solution C obtained in synthesis example 3 is coated on the polyimide resin film of strip,
It is thermally dried at 120 DEG C and removes solvent.Then, do not keep film end and from 180 DEG C to 360 DEG C with about 30 DEG C/
The programming rate of min is heat-treated, and is consequently formed polyimide layer, and is obtained and possess the polyimide layer that thickness is 10 μm
Duplexer.
During the result that various evaluations are carried out to the duplexer obtained in embodiment and comparative example is shown in table 1 and table 2.
[table 1]
[table 2]
Claims (10)
1. a kind of manufacture method of the duplexer with polyimide layer, which is with more than one layer of polyamides in supporting base material
The manufacture method of the duplexer of imine layer, it is characterised in that：, will gather as supporting base material including using the flexible membrane of strip
Acid amides acid solution or polyimide solution are coated in supporting base material and form the application step of more than one layer of coating layer；Simultaneously
The heat treatment step heated by the conveyance one side of the supporting base material with coating layer；In the heat treatment step,
By the mechanism for gripping the end of the width of supporting base material, simultaneously by the width of the supporting base material with coating layer
End is fixed or is stretched in the direction of the width, simultaneously transports supporting base material in the transmission direction, and sub- with the acyl of polyamic acid
The temperature and time or maximum temperature that amination is completed becomes more than 200 DEG C of condition to carry out the heating, and forms poly-
Imide layer.
2. the manufacture method of the duplexer with polyimide layer according to claim 1, it is characterised in that：At heating
In reason step, when supporting base material of the conveyance with coating layer in the transmission direction, remove when stretching in the transmission direction
Send.
3. the manufacture method of the duplexer with polyimide layer according to claim 1, it is characterised in that：In coating step
In rapid, each coating layer for forming more than a layer on the two sides of supporting base material.
4. the manufacture method of the duplexer with polyimide layer according to claim 1, it is characterised in that：Flexible membrane
For the resin film or metal forming of 25 μm～200 μ m-thicks.
5. the manufacture method of the duplexer with polyimide layer according to claim 1, it is characterised in that：Supporting base material
For polyimide resin film.
6. the manufacture method of the duplexer with polyimide layer according to claim 1, it is characterised in that：Supporting base material
With the difference of the thermal coefficient of expansion of polyimide layer be more than 1ppm/K, or supporting base material and adjacent polyimide layer thermal expansion
The difference of coefficient is more than 1ppm/K.
7. the manufacture method of the duplexer with polyimide layer according to claim 1, it is characterised in that：At heating
In reason step, by supporting base material is stretched on the width of supporting base material, and become 100% with the elongation percentage of width
～120% mode is extended.
8. the manufacture method of the duplexer with polyimide layer according to claim 1, it is characterised in that：At heating
After reason step, functional layer forming step is set, and functional layer is set on polyimide layer.
9. a kind of manufacture method of polyimide film, it is characterised in that：Will be by according to any one of claim 1 to 8
The duplexer with polyimide layer the duplexer that obtained of manufacture method, on the boundary of supporting base material layer and polyimide layer
Polyimide layer is peeled off on face and polyimide film is made.
10. a kind of manufacture method of polyimide film, it is characterised in that：By according to any one of claim 1 to 8
The duplexer obtained by the manufacture method of the duplexer with polyimide layer is the polyimide layer person with multilayer, described
Peel off polyimide film to make polyimide film at least one interface at the interface of polyimides interlayer.
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| CN110951104A (en) * | 2018-09-27 | 2020-04-03 | 东京应化工业株式会社 | Heat treatment apparatus, imide resin film production system, and heat treatment method |
| CN112074560A (en) * | 2019-02-01 | 2020-12-11 | 株式会社Lg化学 | Polyimide film, flexible substrate using the same, and flexible display including the flexible substrate |
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| KR101841416B1 (en) * | 2018-02-07 | 2018-03-22 | 권경대 | Polyimide film and process for producing the same |
| KR101912455B1 (en) * | 2018-04-10 | 2018-10-26 | (주)아이피아이테크 | Polyimide surface treated aerogel insulation materials and method of manufacturing the same |
| WO2020159035A1 (en) * | 2019-02-01 | 2020-08-06 | 주식회사 엘지화학 | Polyimide film, flexible substrate using same, and flexible display comprising flexible substrate |
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| JP2017064709A (en) | 2017-04-06 |
| TW201712054A (en) | 2017-04-01 |
| JP6937557B2 (en) | 2021-09-22 |
| KR20170038718A (en) | 2017-04-07 |
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