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WO2014129464A1 - Corps stratifié, élément de cellule solaire, cellule solaire, élément de dispositif d'affichage, dispositif d'affichage, et procédé de fabrication de corps stratifié - Google Patents

Corps stratifié, élément de cellule solaire, cellule solaire, élément de dispositif d'affichage, dispositif d'affichage, et procédé de fabrication de corps stratifié Download PDF

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Publication number
WO2014129464A1
WO2014129464A1 PCT/JP2014/053791 JP2014053791W WO2014129464A1 WO 2014129464 A1 WO2014129464 A1 WO 2014129464A1 JP 2014053791 W JP2014053791 W JP 2014053791W WO 2014129464 A1 WO2014129464 A1 WO 2014129464A1
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Prior art keywords
layer
laminate
polyimide
resin
laminate according
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PCT/JP2014/053791
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English (en)
Japanese (ja)
Inventor
友貴 須藤
正和 片山
平石　克文
拓平 太田
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Nippon Steel Chemical and Materials Co Ltd
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Nippon Steel and Sumikin Chemical Co Ltd
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Priority to JP2015501462A priority Critical patent/JP6445965B2/ja
Publication of WO2014129464A1 publication Critical patent/WO2014129464A1/fr
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    • 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
    • B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
    • B32B7/02—Physical, chemical or physicochemical properties
    • 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
    • B32B15/00—Layered products comprising a layer of metal
    • B32B15/18—Layered products comprising a layer of metal comprising iron or steel
    • 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
    • B32B33/00—Layered products characterised by particular properties or particular surface features, e.g. particular surface coatings; Layered products designed for particular purposes not covered by another single class
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10F—INORGANIC SEMICONDUCTOR DEVICES SENSITIVE TO INFRARED RADIATION, LIGHT, ELECTROMAGNETIC RADIATION OF SHORTER WAVELENGTH OR CORPUSCULAR RADIATION
    • H10F19/00—Integrated devices, or assemblies of multiple devices, comprising at least one photovoltaic cell covered by group H10F10/00, e.g. photovoltaic modules
    • H10F19/30—Integrated devices, or assemblies of multiple devices, comprising at least one photovoltaic cell covered by group H10F10/00, e.g. photovoltaic modules comprising thin-film photovoltaic cells
    • H10F19/31—Integrated devices, or assemblies of multiple devices, comprising at least one photovoltaic cell covered by group H10F10/00, e.g. photovoltaic modules comprising thin-film photovoltaic cells having multiple laterally adjacent thin-film photovoltaic cells deposited on the same substrate
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10F—INORGANIC SEMICONDUCTOR DEVICES SENSITIVE TO INFRARED RADIATION, LIGHT, ELECTROMAGNETIC RADIATION OF SHORTER WAVELENGTH OR CORPUSCULAR RADIATION
    • H10F77/00—Constructional details of devices covered by this subclass
    • H10F77/10—Semiconductor bodies
    • H10F77/16—Material structures, e.g. crystalline structures, film structures or crystal plane orientations
    • H10F77/169—Thin semiconductor films on metallic or insulating substrates
    • H10F77/1698—Thin semiconductor films on metallic or insulating substrates the metallic or insulating substrates being flexible
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10F—INORGANIC SEMICONDUCTOR DEVICES SENSITIVE TO INFRARED RADIATION, LIGHT, ELECTROMAGNETIC RADIATION OF SHORTER WAVELENGTH OR CORPUSCULAR RADIATION
    • H10F77/00—Constructional details of devices covered by this subclass
    • H10F77/10—Semiconductor bodies
    • H10F77/16—Material structures, e.g. crystalline structures, film structures or crystal plane orientations
    • H10F77/169—Thin semiconductor films on metallic or insulating substrates
    • H10F77/1698—Thin semiconductor films on metallic or insulating substrates the metallic or insulating substrates being flexible
    • H10F77/1699—Thin semiconductor films on metallic or insulating substrates the metallic or insulating substrates being flexible the films including Group I-III-VI materials, e.g. CIS or CIGS on metal foils or polymer foils
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10F—INORGANIC SEMICONDUCTOR DEVICES SENSITIVE TO INFRARED RADIATION, LIGHT, ELECTROMAGNETIC RADIATION OF SHORTER WAVELENGTH OR CORPUSCULAR RADIATION
    • H10F77/00—Constructional details of devices covered by this subclass
    • H10F77/93—Interconnections
    • H10F77/933—Interconnections for devices having potential barriers
    • H10F77/935—Interconnections for devices having potential barriers for photovoltaic devices or modules
    • H10F77/937—Busbar structures for modules
    • 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
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/30—Properties of the layers or laminate having particular thermal properties
    • B32B2307/306—Resistant to heat
    • 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
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/70—Other properties
    • B32B2307/732—Dimensional properties
    • B32B2307/734—Dimensional stability
    • 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
    • B32B2457/00—Electrical equipment
    • 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
    • B32B2457/00—Electrical equipment
    • B32B2457/20—Displays, e.g. liquid crystal displays, plasma displays
    • B32B2457/202—LCD, i.e. liquid crystal displays
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K77/00—Constructional details of devices covered by this subclass and not covered by groups H10K10/80, H10K30/80, H10K50/80 or H10K59/80
    • H10K77/10—Substrates, e.g. flexible substrates
    • H10K77/111—Flexible substrates
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00—Energy generation through renewable energy sources
    • Y02E10/50—Photovoltaic [PV] energy
    • Y02E10/541—CuInSe2 material PV cells
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product

Definitions

  • the present invention relates to a laminate, a solar cell member, a solar cell, a display device member, a display device, and a method for manufacturing the laminate.
  • Patent Document 1 discloses that a polyimide resin layer is directly formed on a conductor to be a circuit wiring by coating (hereinafter abbreviated as a coating method) as a method for manufacturing a polyimide laminate, and heat A method of forming a plurality of polyimide resin layers having different expansion coefficients by multilayering is disclosed. According to this method, it is possible to provide a flexible printed board having excellent reliability in terms of dimensional stability with respect to temperature change, adhesive strength, flatness after etching, and the like.
  • the coating method means that after applying a polyimide precursor resin solution or a polyimide resin solution to be a polyimide resin layer to the metal layer, the metal layer and the polyimide resin layer are dried only or by heat treatment for drying and imidization. Is a method of adhering.
  • Patent Document 2 discloses a method of forming a flexible printed circuit board by bonding a conductor layer and a resin substrate by thermocompression bonding, and a copper foil surface as a conductor layer is subjected to a roughening process by plating made of copper-cobalt-nickel. And improving the adhesion by roughening the surface of the copper foil.
  • thermocompression bonding method the method of bonding the conductor layer and the resin substrate by thermocompression bonding.
  • solder material with a melting temperature higher than that of lead solder has been used for environmental considerations.
  • the contacting polyimide resin layer is highly heat resistant.
  • Patent Document 3 discloses a method of controlling the plating layer on the copper foil roughening treatment surface, which is a metal layer, to suppress the roughening treatment height, that is, the degree of roughening treatment.
  • this method has a problem that the peel strength between the copper foil and the polyimide resin layer is lowered.
  • the subject of making adhesiveness and heat resistance in a double-sided metal-clad laminate compatible is left.
  • Patent Document 4 discloses an example in which a metal thin film-resin material laminate is applied as a flexible substrate for a CIS solar cell.
  • polyimide resin is used as a resin material.
  • a molybdenum (Mo) film is sputtered as a back electrode on the polyimide resin surface.
  • a light absorption layer is formed above this Mo film.
  • the film formation of the light absorption layer represented by CIGS or CIS is performed at about 500 ° C.
  • the resin material that is an organic substance is a single material or a high-level design of a laminate. Has been.
  • oxygen resistance / water vapor permeability which is an important characteristic when used as a substrate for a solar cell, is hereinafter referred to as barrier property.
  • the present invention solves the above-described problems, and the resin layer in contact with the barrier protective layer made of an inorganic material such as metal has high heat resistance, and further, peeling occurs between the barrier protective layer and the heat resistant resin layer. It aims at providing the laminated body which suppressed generation
  • the present inventors have solved the above problems with a laminate of a combination of a resin layer having specific heat resistance and adhesiveness and a barrier protective layer made of an inorganic material. As a result, the present invention has been completed.
  • the laminate of the present invention is a laminate in which a second layer made of a resin and a first layer made of an inorganic material are laminated, and the thermal weight loss of the resin at 545 ° C. is 1.0% or less. And the peel strength at the interface between the second layer and the first layer is 100 N / m or more. With such a configuration, preferable heat resistance of the second layer is obtained, and high adhesion (peeling resistance) between the second layer and the first layer is obtained.
  • the thermal weight loss of the resin at 545 ° C. is 0.7% or less.
  • the linear thermal expansion coefficient in the plane direction of the first layer is preferably 15 ppm / K or less.
  • a TFT Thin formed of a lower electrode layer or a power generation layer for a device formed on a substrate, for example, a compound semiconductor solar cell, or polysilicon or an oxide for a display device, etc. This is because the thermal stress generated between the semiconductor layer for driving such as a film transistor is reduced, and the occurrence of warpage and peeling during heat treatment can be suppressed.
  • the second layer is formed of one or more resin materials selected from the group consisting of polyimide and derivatives thereof. According to such a condition, the second layer having a small thermogravimetric decrease, heat resistance, and high adhesion to the first layer can be obtained.
  • the first layer is preferably formed of one or two or more metal materials selected from the group consisting of metals, and the group consisting of ferritic stainless steel and titanium. More preferably, it is formed of one or more inorganic materials selected from the above. According to such conditions, the second layer can be supported and high barrier properties can be ensured.
  • the laminate of the present invention is preferably obtained by applying a heat treatment at 300 ° C. or higher after applying the resin or its precursor to the surface of the first layer. It is preferably obtained by performing a heat treatment at a concentration of 10% or less. According to such conditions, the second layer having a small thermogravimetric decrease and heat resistance can be obtained. In particular, when heat treatment is performed under a condition where the oxygen concentration is 10% or less, the resin-inorganic matter in the laminate is obtained. This is because the adhesive strength of the is increased.
  • the present invention is applicable to a solar cell member or solar cell including the laminate.
  • the present invention is applicable to a display device member or a display device including the laminate.
  • the manufacturing method of the laminated body of this invention is the surface of this 1st layer by the process of apply
  • the step of forming the second layer made of the resin on the side surface is performed by roll-to-roll.
  • the heat treatment is preferably performed at an oxygen concentration of 10% or less.
  • the laminate of the present invention is suitable for various applications that require flexibility and heat resistance. Therefore, it is suitable for flexible substrates such as display members such as organic EL having TFT semiconductors that require high-temperature processing, power semiconductor-mounted inverter members characterized by high-temperature operation, and compound semiconductor solar cells typified by chalcopyrites. Applicable to.
  • the resin layer has high heat resistance and not only exhibits excellent dimensional stability, but also suppresses peeling between the inorganic layer and the resin layer in contact therewith and has high adhesiveness.
  • the method for producing a laminate of the present invention is a laminate in which the resin layer has high heat resistance and not only exhibits excellent dimensional stability but also suppresses peeling between the inorganic layer and the resin layer in contact therewith and has high adhesion.
  • the body can be easily manufactured.
  • FIG. 1 is a cross-sectional view of the laminate according to the embodiment.
  • the laminate 10 of the present embodiment is a polyimide layer-containing flexible substrate, and is a laminate obtained by laminating a second layer 2 made of resin and a first layer 1 made of an inorganic substance.
  • the thermal weight loss at 545 ° C. is 1.0% or less, and the peel strength at the interface between the second layer 2 and the first layer 1 is 100 N / m or more.
  • the thermal weight loss at 545 ° C. is a weight reduction rate when heating is performed at a temperature rising rate of 10 ° C./min under a temperature rising range from room temperature to 545 ° C. in a nitrogen stream.
  • the thermal weight reduction is 1.0% or less, the heat resistance of the second layer 2 is high.
  • a flexible substrate used for a compound semiconductor solar cell including CIGS (CuInGaSe) or CIS (CuInSe) In addition, it can be preferably applied to a flexible substrate used in a display device or the like on which a driving semiconductor layer such as a TFT formed of polysilicon or oxide is mounted.
  • the thermal weight reduction at 545 ° C. is preferably 0.7% or less, more preferably 0.4% or less.
  • the peel strength at the interface between the second layer 2 and the first layer 1 is a test piece having a processing line width suitable for the purpose of measurement by patterning and etching the laminate to a line width of 1 to 10 mm. This is the peel strength when the second layer is peeled off in the 180 ° direction using.
  • the higher peel strength is preferably 300 N / m or more, and more preferably 700 N / m or more.
  • the peel strength after heat treatment at 500 ° C. for 60 minutes is preferably 100 N / m or more, more preferably 300 N / m or more, and even more preferably 700 N / m or more.
  • the thermal weight loss exceeds 1.0 or the peel strength is less than 100 N / m, for example, when forming a CIGS solar cell, which is a kind of compound semiconductor solar cell, or for a display device, the TFT There is a possibility that the high temperature condition during the formation of the driving semiconductor layer cannot be endured, or the handling property during the processing process is not sufficiently ensured, and the resin layer-inorganic layer interface peels off.
  • the laminate When the laminate is commercially produced using a substrate of a specific product, such as a display device or a solar cell, it is accompanied by conveyance before and after various processes and treatments required in the production line.
  • a peel of 100 N / m or more is required. By ensuring the strength, the substrate does not peel off as an interlayer adhesion.
  • the laminated body of this invention may arrange
  • the second layer 2 is arranged on both surfaces of the first layer 1, for example, occurrence of warpage of the laminate due to a difference in linear expansion between the first layer and the second layer due to a change in surrounding environment such as temperature. It can also be a suppression means against
  • the laminate of the present invention has a lower electrode layer or a device formed on a substrate, for example, a compound solar cell.
  • a power generation layer or a display device thermal stress generated between the driving semiconductor layer such as a TFT formed of polysilicon or oxide is reduced.
  • a solar cell member or display during high-temperature heat treatment Since generation
  • the linear thermal expansion coefficient in the surface direction of the first layer 1 is more preferably 13 ppm / K or less.
  • the linear thermal expansion coefficient means that the first layer 1 is removed from the produced laminate and only the second layer 2 is taken out as a measurement specimen, and the measurement specimen is 200 ° C. in a nitrogen stream.
  • the temperature of the test piece (second layer 2) is lowered at a constant rate after the temperature is raised to a high temperature range exceeding 50 ° C., and is obtained from the relationship between the temperature difference at that time and the measurement length of the test piece.
  • the 2nd layer 2 will not have a restriction
  • it is 1 type, or 2 or more types of resin materials selected from the group which consists of a polyimide and those derivatives. Can be formed. These are preferable from the viewpoints of heat resistance and adhesion to the first layer 1.
  • the thickness of the second layer 2 is not particularly limited, but the average film thickness is preferably 1 to 100 ⁇ m, more preferably 2 to 8 ⁇ m, and even more preferably 2 to 4 ⁇ m.
  • the average film thickness is less than 1 ⁇ m, the electric insulation tends to be insufficient, and when the average film thickness exceeds 100 ⁇ m, the productivity tends to be impaired.
  • the surface roughness of the second layer 2 on the opposite side of the interface with the first layer 1 is not particularly limited, but preferably there is a problem with the electrode layer formed on the resin layer, such as a crack.
  • Ra average roughness
  • the polyimide used as the second layer and derivatives thereof are obtained by reacting an aromatic diamino compound represented by NH 2 —Ar 1 —NH 2 with a tetracarboxylic acid compound, and are said to be easy to synthesize.
  • an aromatic diamino compound represented by NH 2 —Ar 1 —NH 2 with a tetracarboxylic acid compound, and are said to be easy to synthesize.
  • the first aryl group Ar 1 substituted with two amino groups can be selected from any one , but because it has both heat resistance and a low linear thermal expansion coefficient, the following formula (1) to It is preferable that it is selected from the group represented by (3).
  • the following formula (1) shows bonds and side chains composed of primary to tertiary carbons that are expected to have low heat resistance, and elements other than carbon and carbon that are also expected to have low heat resistance (BC, O—
  • Examples include fluorene-9,10-bisaniline.
  • the following formula (2) shows an example of Ar 1 constituting a monomer for polyimide in which a halogeno group, a trihalogenomethyl group, a dihalogenomethylene group, or a hexahalogenoisopropylidene group is directly bonded to an aromatic ring.
  • a halogeno group a trihalogenomethyl group, a dihalogenomethylene group, or a hexahalogenoisopropylidene group is directly bonded to an aromatic ring.
  • Specific examples include diaminobistrihalogenomethylbiphenyl. These groups may have a plurality of bonds directly bonded to the aromatic ring.
  • X represents a halogen element, preferably fluorine.
  • the following formula (3) shows an example of Ar 1 constituting a monomer that provides a polyimide that does not contain a structure other than an aromatic ring and an imide ring.
  • terphenyldiamine, diaminodiphenylbiphenyl, and the like Can be mentioned.
  • a structure represented by the formula (3) is more preferred, and a structure constituting a phenylenediamine compound is more preferred.
  • the phenylenediamine compound has a plurality of isomers, and may be the same isomer or a combination of a plurality of isomers.
  • Ar 1 may have a substituent, but preferably has no substituent or is substituted with a halogeno group.
  • One or more of these aromatic diamino compounds may be used.
  • tetracarboxylic acid compound to be reacted with the diamino compound examples include aromatic tetracarboxylic acid and acid anhydrides, esterified products, halides, etc., but aromatic tetracarboxylic acid compounds are preferred and are precursors of polyimide resins. In terms of ease of synthesis of the polyamic acid (polyamic acid), the acid anhydride is preferable.
  • aromatic tetracarboxylic acid compound O (CO) 2 Ar 2 (CO) a compound represented by 2 O is mentioned as suitable.
  • the second aryl group Ar 2 substituted with two (CO) 2 O groups can be selected from any one, but for the reason that it has both heat resistance and a low linear thermal expansion coefficient, the following formula: Preferred are those selected from the groups represented by (4) to (6).
  • the substitution position of the acid anhydride group [(CO) 2 O] is arbitrary, but a symmetric position around Ar 2 is preferable.
  • the following formula (4) shows bonds and side chains composed of primary to tertiary carbons that are expected to have low heat resistance, and elements other than carbon and carbon that are also expected to have low heat resistance (BC, O— Constructs a monomer for polyimide as shown in the following formula (7) excluding a monomer that gives a polyimide structure having a bond (excluding an imide ring bond) consisting of C, S—C, N—C, P—C, and Se—C)
  • Ar 2 include fluorene-9,10-bisphthalic anhydride.
  • the following formula (5) shows an example of Ar 2 constituting a monomer for polyimide in which a halogeno group, a trihalogenomethyl group, a dihalogenomethylene group, or a hexahalogenoisopropylidene group is directly bonded to an aromatic ring.
  • a halogeno group a trihalogenomethyl group, a dihalogenomethylene group, or a hexahalogenoisopropylidene group is directly bonded to an aromatic ring.
  • Specific examples include halogenopyromellitic anhydride and 4,4′-hexahalogenoisopropylidenebisphthalic anhydride. These groups may have a plurality of bonds directly bonded to the halogenoaromatic ring.
  • X represents a halogen element, preferably fluorine.
  • Ar 2 constituting a monomer that provides a polyimide that does not contain a structure other than an aromatic ring and an imide ring.
  • pyromellitic anhydride, 1, 6, Examples include 7,12-perylenetetracarboxylic dianhydride.
  • Ar 2 represented by the above formulas (4) to (6) more preferably the structure represented by the formula (6), more preferably a biphenyltetracarboxylic dianhydride or a naphthalenetetracarboxylic dianhydride. It is a structure to do.
  • Biphenyltetracarboxylic dianhydride and naphthalenetetracarboxylic dianhydride each have a plurality of isomers, both of which may be the same isomer or a combination of isomers, biphenyltetracarboxylic dianhydride and A combination of naphthalenetetracarboxylic dianhydrides may be used.
  • Ar 2 may have a substituent, but preferably does not have a substituent or is substituted with a halogeno group.
  • aromatic acid anhydride compounds may be used.
  • a more preferable combination of the aromatic diamino compound and the tetracarboxylic acid compound is a combination of a biphenyltetracarboxylic acid compound and a phenylenediamine compound, or biphenyltetracarboxylic acid.
  • the content of 4,4′-diamino-2,2′-bis (trifluoromethyl) biphenyl is preferably 5% or less with respect to the total amount of the aromatic diamino compound, more preferably 2. 5% or less.
  • the polyimide resin constituting the second layer 2 is prepared by reacting, for example, the aromatic diamino compound and the tetracarboxylic acid compound in an approximately equimolar amount in a solvent, and polyamic acid (polyamic acid) which is a polyimide resin precursor. ) And an imidization reaction.
  • the synthesis of the polyamic acid which is a precursor of the polyimide resin
  • the polyamic-acid solution or polyimide resin solution which is a precursor is apply
  • the coating layers of the polyamic acid solution and the polyimide resin solution, which are precursors are collectively referred to as a pre-polyimide resin layer.
  • the polyimide used as the second layer 2 can be manufactured by the following method, for example. That is, the aromatic diamino compound and tetracarboxylic dianhydride are mixed in a solvent at an approximately equimolar ratio, and reacted in a reaction temperature range of 0 to 200 ° C., preferably in a range of 0 to 100 ° C. There is a method for obtaining a polyimide resin by obtaining a polyamic acid solution as a precursor and imidizing the solution.
  • NMP N-methylpyrrolidone
  • DMF dimethylformamide
  • DMAc dimethylacetamide
  • DMSO dimethyl sulfoxide
  • examples include dioxane, tetrahydrofuran, diglyme, and triglyme.
  • imidization may be performed after applying the precursor polyamic acid solution to the first layer 1.
  • the pre-polyimide resin layer applied to the first layer 1 may be either the polyamic acid solution that is the precursor or the polyimide resin solution that has been imidized, but if the polyimide is not solvent-soluble, a viscosity adjustment viewpoint. Therefore, a polyamic acid solution as a precursor is preferable.
  • the first layer 1 is an inorganic substance, and the type of the first layer 1 is not limited as long as the performance as a laminate can be ensured.
  • copper, aluminum, stainless steel, iron, silver, palladium, nickel, chromium It is formed of one or more metal materials or glass selected from the group consisting of molybdenum, tungsten, zirconium, gold, cobalt, titanium, tantalum, zinc, lead, tin, silicon, bismuth, indium or alloys thereof. From the viewpoints of heat resistance and adhesiveness to the second layer 2, it is preferable.
  • the base material is difficult to break, and particularly preferably at the time of preparing a laminate or assembling a display device or a solar cell or Austenitic stainless steel, martensitic stainless steel, duplex stainless steel, precipitation hardened stainless steel, ferritic stainless steel and titanium in terms of resistance to rust during use, and more preferably ferritic stainless steel in terms of low linear thermal expansion And titanium.
  • the layer thickness of the first layer 1 is preferably 5 to 300 ⁇ m, more preferably 20 to 200 ⁇ m.
  • the layer thickness exceeds 300 ⁇ m, continuous processes such as roll-to-roll tend to be difficult, and when the layer thickness is less than 20 ⁇ m, the self-supporting property tends to decrease.
  • sizing, chromium plating, nickel plating, chromium ⁇ are applied to the surface for the purpose of adjusting and modifying the suitability of the surface properties and improving the adhesive strength with the second layer 2.
  • the laminate manufacturing method of the present invention will be described below by taking a laminate in which the second layer is polyimide as an example of the embodiment, but the present invention is not limited to the embodiment.
  • FIG. 2 is a flowchart showing the method for manufacturing the laminate according to the present embodiment.
  • a polyamic acid solution or a polyimide resin solution that is a precursor to be the second layer 2 is applied to an inorganic material to be the first layer 1, and a pre-polyimide resin is then applied.
  • a layer is formed (S1).
  • the polyamic acid solution and the polyimide resin solution which are precursors are collectively referred to as a pre-polyimide resin layer.
  • the second layer 2 and the pre-polyimide resin layer are bonded together by drying [heat removal of the solvent] (S2) and imidization [heat curing treatment] (S3), and the second layer 2 is formed.
  • Polyimide is formed on the inorganic material.
  • drying and imidization are performed when a polyamic acid solution as a precursor is applied, and only drying is performed when a polyimide resin solution is applied.
  • a laminate made of polyimide and an inorganic material is formed. A detailed manufacturing method will be described later.
  • Step (S1) of continuously applying a resin or a precursor thereof to the surface of the first layer made of an inorganic substance, and a second step made of the resin on the surface of the first layer by heat treatment at 300 ° C. or higher.
  • Steps (S2, S3) for forming the layer can be performed roll-to-roll.
  • a pre-polyimide resin layer is applied to the first layer 1.
  • the pre-polyimide resin layer applied to the first layer 1 becomes the second layer 2.
  • an arbitrary method can be selected as a coating method for forming a plurality of pre-polyimide resin layers on the first layer 1, but the following three methods are preferable from the viewpoint of coating accuracy.
  • pre-polyimide resin layers are simultaneously coated on a conductor by a multilayer die.
  • another pre-polyimide resin layer is applied onto the undried application surface by a knife coating method, a die method, or the like.
  • a pre-polyimide resin layer is applied by an arbitrary method and dried, and then another pre-polyimide resin layer is applied to the dry coated surface by an arbitrary method.
  • the knife coating method described here is a method in which a resin solution is leveled and applied with a bar, squeegee, knife or the like.
  • any method can be utilized. After the pre-polyimide resin layer is applied and formed, a laminate including a pre-dried uncured pre-polyimide resin layer, Heat treatment at a high temperature (200 ° C. or higher) by allowing it to stand for a certain period of time in a hot air drying furnace that can be set to a predetermined temperature, or by continuously moving within the drying furnace area range to ensure a predetermined drying and curing time ), A stacked body having one or more second layers can be formed.
  • a high temperature 200 ° C. or higher
  • the pre-polyimide resin layer is applied, and then the pre-dried uncured laminate is wound into a roll and then dried at a high temperature and heat-cured. Processing methods are also possible.
  • the solvent is removed from the pre-polyimide resin layer by heat treatment, and when the polyimide precursor resin solution is used, the imide ring is further closed.
  • a final heat treatment temperature for making an imidized (cured) polyimide resin layer and for volatilizing an adsorbed component derived from atmospheric components and moisture distributed on the surface of the first inorganic material Is preferably 300 ° C. or higher. More preferably, it is 370 degreeC or more, More preferably, it is 430 degreeC or more.
  • the heat treatment can be performed under any conditions in an inert gas such as nitrogen or argon and in the air. Moreover, it can carry out under any conditions of normal pressure, reduced pressure, increased pressure and vacuum. Among these, it is preferable to perform the heat treatment under the condition that the oxygen concentration is 10% or less because the adhesive force between the laminate and the inorganic substance including the resin-metal is increased. In nitrogen or argon, the oxygen concentration of 5% or less is more preferable because the adhesive strength between the laminate and the resin-metal-containing inorganic substance is further increased. The lower the oxygen concentration, the higher the adhesive strength between the laminate and the resin-metal-containing inorganic substance, and the oxygen concentration is more preferably 1% or less, and most preferably 0.5% or less.
  • the heat treatment in a control condition range where the oxygen concentration is 10% or less because it becomes possible to appropriately manage the adhesive force expression between the resin-metal-containing inorganic substance in the laminate.
  • the inorganic layer of the laminate is copper
  • copper is a highly active metal species, so it is easy to form an oxide by reaction with oxygen, and the oxide suppresses or attenuates further reaction with oxygen.
  • the oxygen in the surrounding atmosphere is small, that is, the oxygen concentration is close to 0%.
  • the oxide film produced by reacting with oxygen in the surrounding atmosphere exerts an action of suppressing or attenuating further reaction with oxygen. Therefore, it is possible to prevent the occurrence of corrosion and rust.
  • the resin solution concentration when using the precursor polyamic acid solution as the pre-polyimide resin layer is a polyimide precursor and depends on the degree of polymerization of the polyamic acid which is a polymer, but is usually 5 to 30% by weight, preferably Is 10 to 20% by weight. If the polymer concentration is higher than 5% by weight, a sufficient film thickness can be obtained by one application. If the polymer concentration is lower than 30% by weight, the viscosity of the resin solution does not become too high, and it is good in terms of uniformity and smoothness. It is because it can apply
  • a single polyimide layer is formed as the second layer on the surface.
  • An inorganic material may be bonded.
  • thermocompression bonding when the polyimide layer and the inorganic material are bonded together. That is, a hydro press, a vacuum type hydro press, an autoclave pressurizing vacuum press, a continuous thermal laminator, or the like can be used.
  • the vacuum hydropress is a preferable thermocompression bonding method because a sufficient pressing pressure can be obtained and oxidation of the conductor when a metal foil is used as the first layer can be prevented.
  • the hot press temperature at the time of thermocompression bonding is not particularly limited, but it is preferably higher than the glass transition temperature of the polyimide resin used.
  • the hot press pressure is suitably 0.1 to 50 MPa (1 to 500 kg / cm 2), although it depends on the type of press equipment used. If the press temperature during thermocompression bonding becomes too high, there is a concern that problems such as deterioration of the inorganic layer and the polyimide resin layer may occur.
  • the resin layer has a thermal weight reduction at 545 ° C. of 1.0% or less, and the peel strength at the interface between the inorganic material and the resin layer is 100 N / m or more. Bond strength is very good. In other words, the compatibility with high heat resistance is achieved. For this reason, display members such as organic EL having TFT (Thin Film Transistor) semiconductors that require high temperature processing, inverter members equipped with power semiconductors characterized by high temperature operation, compound semiconductor solar cell substrates represented by chalcopyrite systems, etc. It can be suitably used for various materials that require heat resistance and flexibility.
  • TFT Thin Film Transistor
  • the above-mentioned display member requires different heat resistance levels depending on the type of TFT material used. For example, when the material type is LTPS [Low Temperature Polysilicon], heat resistance of about 450 to 460 ° C. is required.
  • IGZO semiconductor oxide which is an oxide of indium (In), gallium (Ga) and zinc (Zn)
  • the required laminated body of this embodiment can be used suitably as said display member.
  • FIG. 3 is a cross-sectional view of an example of the flexible solar cell of the present embodiment, and is formed using the laminate 10 that is the polyimide layer-containing flexible substrate described with reference to FIG.
  • the solar cell 20 includes a lower electrode (back electrode) 6 on the second layer 2 which is a polyimide layer (insulating layer) of the laminate 10 which is a polyimide layer-containing flexible substrate, and a photoelectric conversion layer (light) on the lower electrode 6.
  • the structure has a transparent electrode (upper electrode) 8, and a lower electrode 6 and a takeout electrode 9 connected to the transparent electrode 8 on the absorption layer 7 and the photoelectric conversion layer 7.
  • the lower electrode 6 is not particularly limited as long as it is a conductive material.
  • a metal or semiconductor having a volume resistivity of 6 ⁇ 10 6 ⁇ ⁇ cm or less can be used.
  • molybdenum (Mo) can be used.
  • the thickness of the lower electrode 6 is preferably 0.1 to 1 ⁇ m from the viewpoint of flexibility.
  • the photoelectric conversion layer 7 preferably has a good light absorption, that is, a large light absorption coefficient.
  • a compound semiconductor is preferable, and a chalcopyrite-based I-III-VI group compound composed of Cu, In, Ga, Al, Se, S or the like is used.
  • the thickness of the photoelectric conversion layer 7 is preferably 0.1 to 4 ⁇ m from the viewpoint of achieving both power generation efficiency and flexibility.
  • the transparent electrode 8 is an electrode on the light incident side, a material having high transparency is used so that the light can be efficiently collected.
  • a material having high transparency is used so that the light can be efficiently collected.
  • zinc oxide (ZnO) or indium tin oxide (ITO) is used.
  • the thickness of the transparent electrode 8 is 0.1 to 0.3 ⁇ m from the viewpoint of flexibility.
  • an antireflection film may be formed in contact with the transparent electrode 8.
  • the extraction electrode 9 for example, metals and alloys such as Ni, Al, Ag, Au, and NiCr can be used as materials.
  • a Cd-based material such as CdS, ZnS, ZnO, ZnO 1-X S X , Zn (S, O, OH) X , Zn 1-X Mg X O, etc.
  • An In-based buffer layer (not shown) such as Zn-based, InS, In (S, OH) X may be provided.
  • FIG. 4 is a flowchart showing a method for manufacturing the flexible solar cell of the present embodiment.
  • an electrode material for example, molybdenum is laminated on the second layer 2 that is a polyimide layer of the laminate 10 that is a polyimide layer-containing flexible substrate to form the lower electrode 6 (S11).
  • molybdenum is stacked on the second layer 2 by sputtering or vapor deposition.
  • the compound semiconductor material is laminated on the lower electrode 6 by any method such as sintering, chemical precipitation, sputtering, proximity sublimation, multi-source deposition, and selenization.
  • a method of forming a thin film by sequentially applying a CdS paste and a CdTe paste and sintering at 600 ° C. or lower can be exemplified. Further, instead of this method, a method of forming a CdTe film by proximity sublimation after forming a CdS film by chemical precipitation or sputtering can be employed.
  • zinc (Zn) may be mixed into the compound semiconductor film.
  • zinc By mixing zinc, the photoelectric conversion efficiency can be improved.
  • a method of applying an aqueous solution such as zinc sulfate, zinc chloride, or zinc iodide to the compound semiconductor film can be used. Or you may immerse the laminated body which formed even the photoelectric converting layer 7 in these aqueous solution.
  • a transparent electrode 8 of zinc oxide (ZnO) or indium tin oxide (ITO) doped with aluminum is laminated thereon by a sputtering method or the like (S13). Then, it connects with each of the lower electrode 6 and the transparent electrode 8, and each taking-out electrode 9 is formed (S14).
  • Aluminum or nickel can be used as the material for the extraction electrode.
  • an alkali metal supply layer may be formed between the second layer 2 and the lower electrode 6.
  • the effect of improving the photoelectric conversion efficiency can be expected when a part of the alkali metal permeates and diffuses into the photoelectric conversion layer 7 from the alkali metal supply layer.
  • the thickness of the stainless steel foil manufactured by Nippon Steel & Sumikin Materials Co., Ltd. is 30 ⁇ m
  • the coefficient of thermal expansion is 11 ppm / K
  • the surface roughness on the side in contact with the first layer (Ra ) was 0.08 ⁇ m ferritic stainless steel foil.
  • peel strength The adhesive force between the inorganic layer and the polyimide resin layer is such that the laminate is subjected to a pattern etching process with a line width of 1 mm, and the resin layer is applied using a tensile tester (Strograph-M1) manufactured by Toyo Seiki Co., Ltd.
  • the peel strength was measured by peeling off in the 180 ° direction.
  • attachment between a process fine wire and a resin interface and being difficult to peel was made impossible to peel.
  • the surface roughness of the stainless steel layer was measured using a laser microscope (VK-8710) manufactured by Keyence Corporation on a stainless steel foil cut to 2 cm ⁇ 2 cm.
  • the surface roughness (Ra) on the side in contact with the first layer of the stainless steel foil manufactured by Nippon Steel & Sumikin Materials Co., Ltd. used as the first layer was 0.08 ⁇ m.
  • Performance evaluation Example 1 Prepare the ferritic stainless steel foil having a thickness of 30 ⁇ m described above, and apply the polyamic acid a solution prepared in advance in Synthesis Example 1 and heat at a temperature of 100 to 140 ° C. for 5 minutes, In a nitrogen atmosphere (controlled oxygen concentration of 1% or less), the temperature was raised to 370 ° C. at 4 ° C./min, then raised to 500 ° C. at 20 ° C./min and held for 40 minutes, 50-60 ° C. After cooling, a laminate having a polyimide layer a having a film thickness of about 8 ⁇ m was obtained.
  • Example 2 Prepare the 30 ⁇ m-thick ferritic stainless steel foil described above, and apply the polyamic acid b solution prepared in advance in Synthesis Example 2 and heat at a temperature of 100 to 140 ° C. for 5 minutes, In a nitrogen atmosphere (controlled oxygen concentration of 1% or less), the temperature was raised to 370 ° C. at 4 ° C./min, then raised to 500 ° C. at 20 ° C./min and held for 40 minutes, 50-60 ° C. After cooling, a laminate comprising a polyimide layer b having a film thickness of about 8 ⁇ m was obtained.
  • Example 3 Prepare the 30 ⁇ m-thick ferritic stainless steel foil described above, and apply the polyamic acid c solution prepared in advance in Synthesis Example 2 and heat at a temperature of 100 to 140 ° C. for 5 minutes, In a nitrogen atmosphere (controlled oxygen concentration of 1% or less), the temperature was raised to 370 ° C. at 4 ° C./min, then raised to 500 ° C. at 20 ° C./min and held for 40 minutes, 50-60 ° C. After cooling, a laminate having a polyimide layer c having a film thickness of about 8 ⁇ m was obtained.
  • Example 4 A laminate including the polyimide layer d was obtained in the same manner as in Example 1 except that the polyamic acid d solution prepared in advance in Synthesis Example 4 was used.
  • Example 5 Prepare the ferritic stainless steel foil having a thickness of 30 ⁇ m described above, and apply the polyamic acid e solution prepared in advance in Synthesis Example 5 and heat at a temperature of 100 to 140 ° C. for 5 minutes, In a nitrogen atmosphere (controlled oxygen concentration of 1% or less), the temperature was raised to 370 ° C. at 4 ° C./min, then raised to 500 ° C. at 20 ° C./min and held for 40 minutes, 50-60 ° C. A laminated body having a polyimide layer e having a film thickness of about 8 ⁇ m after curing was obtained.
  • Comparative Example 1 A laminate including the polyimide layer f was obtained in the same manner as in Example 1 except that the polyamic acid f solution prepared in advance in Synthesis Example 6 was used.
  • Comparative Example 2 A laminate including the polyimide layer g was obtained in the same manner as in Example 1 except that the polyamic acid g solution prepared in advance in Synthesis Example 7 was used.
  • Comparative Example 3 A laminate including the polyimide layer h was obtained in the same manner as in Example 1 except that the polyamic acid h solution prepared in advance in Synthesis Example 8 was used.
  • Comparative Example 4 A laminate was obtained in the same manner as in Example 1 except that the heating condition was changed from the nitrogen atmosphere to the atmosphere.
  • the thermal weight reduction shown in Table 1 is a case where the resin layer thickness is about 8 ⁇ m.
  • the thermal weight reduction is further reduced. Reduce and improve.
  • the thermal weight loss at 545 ° C. is 1.0% or less, and the peel strength at the interface between the second layer and the first layer is 100 N / m. Strong adhesion was exhibited, and in the measurement of peel strength, it was a strong adhesion state that could not be peeled off. Further, as shown in Table 1 above, in Examples 1, 3 and 4, the thermal weight loss at 545 ° C. is 0.7% or less, and the peel strength at the interface between the second layer and the first layer is Strong adhesion was developed exceeding 100 N / m, and in the measurement of peel strength, it was in a strong adhesion state that could not be peeled off.
  • Comparative Example 1 has a thermal weight reduction of 10.1%, and Comparative Examples 2 and 3 also have a thermal weight reduction greatly exceeding 1.0%, which is insufficient in heat resistance. Further, the resin layer was broken during the peel strength measurement, and the peel strength at the interface could not be measured. Comparative Example 4 has a peel strength of 10 N / m, less than 100 N / m, and is inferior in adhesion performance with peeling.
  • Applications include display substrate materials such as liquid crystal and organic EL that involve TFT fabrication, SiC power device substrate materials that are subject to high-temperature use, organic EL lighting substrate materials that continue for long periods of time, and compounds that require high-temperature conditions in the manufacturing process Examples include products, parts, members, and the like, such as semiconductor-based solar cell substrate materials.

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  • Laminated Bodies (AREA)
  • Parts Printed On Printed Circuit Boards (AREA)
  • Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)
  • Photovoltaic Devices (AREA)

Abstract

Afin de fournir un corps stratifié à résistance thermique et capacité d'adhésion équilibrées qui possède une couche de résine et une couche barrière protectrice comprenant une substance inorganique telle qu'un métal, un élément de cellule solaire utilisant le corps stratifié, une cellule solaire, un élément de dispositif d'affichage, un dispositif d'affichage, et un procédé de fabrication du corps stratifié, la présente invention concerne un corps stratifié dans lequel sont stratifiées une première couche comprenant une substance inorganique telle qu'un métal, et une seconde couche comprenant une résine, une configuration étant adoptée dans laquelle la réduction thermique en poids de la résine à 545°C est inférieure à 1,0 %, et la force de décollement de la frontière entre la seconde couche et la première couche est d'au moins 100 N/m.
PCT/JP2014/053791 2013-02-19 2014-02-18 Corps stratifié, élément de cellule solaire, cellule solaire, élément de dispositif d'affichage, dispositif d'affichage, et procédé de fabrication de corps stratifié Ceased WO2014129464A1 (fr)

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WO2020044405A1 (fr) * 2018-08-27 2020-03-05 シャープ株式会社 Procédé de fabrication de dispositif d'affichage et appareil de fabrication de dispositif d'affichage
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