WO2023282228A1 - 電池電極用導電性基板及びその製造方法 - Google Patents
電池電極用導電性基板及びその製造方法 Download PDFInfo
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- WO2023282228A1 WO2023282228A1 PCT/JP2022/026603 JP2022026603W WO2023282228A1 WO 2023282228 A1 WO2023282228 A1 WO 2023282228A1 JP 2022026603 W JP2022026603 W JP 2022026603W WO 2023282228 A1 WO2023282228 A1 WO 2023282228A1
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Images
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
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/64—Carriers or collectors
- H01M4/66—Selection of materials
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K1/00—Printed circuits
- H05K1/02—Details
- H05K1/03—Use of materials for the substrate
-
- 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
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Definitions
- the present invention relates to a conductive substrate for battery electrodes and a manufacturing method thereof.
- Batteries mounted in means of transportation such as aircraft and automobiles are required to be lightweight from the viewpoint of improving fuel efficiency and the like.
- it is desirable that the weight of various batteries is reduced from the point of view of ease of handling, regardless of the application.
- an electrode substrate also referred to as a current collector or the like.
- a metal film electrode substrate can be replaced with a metal-plated resin film, a significant weight reduction can be achieved.
- the density of the electrode substrate made of copper film is about 8.9 g/cm 3 .
- a conductive composite film with a thickness of 7 ⁇ m in which a copper plating film with a thickness of 1 ⁇ m is formed on each side of a polyimide film with a thickness of 5 ⁇ m (density: about 1.4 g/cm 3 ), has a density of about 3.5 g. / cm3 . That is, when the electrode substrate is replaced from the copper film having a thickness of 7 ⁇ m with the conductive composite film having the same thickness, the weight can be reduced to less than half.
- Patent Document 1 discloses an electrode current collector in which a conductive layer is formed by electroless nickel plating on both sides of a resin thin plate, and a nickel-hydrogen storage battery equipped with such an electrode current collector as a hydrogen storage electrode that is a negative electrode. is described.
- a method of roughening a thin resin plate by blasting is employed in order to improve the adhesion of a conductive layer formed by nickel plating.
- Patent Document 1 describes that, as Example 4, a polyvinyl chloride thin plate with a thickness of 70 ⁇ m was subjected to blasting treatment to increase the unevenness of the surface, and then nickel plating was applied to produce a current collector.
- the present invention has been made based on the above circumstances, and its object is to provide a conductive substrate for battery electrodes with high adhesion of a metal plating layer, and a method for manufacturing the same.
- One embodiment of the present invention includes a substrate layer and metal plating layers laminated on both sides of the substrate layer via a compound ⁇ , wherein the density of the substrate layer is lower than the density of the metal plating layer.
- the compound ⁇ has a first functional group capable of reacting and bonding with the substrate layer and a second functional group capable of reacting and bonding with the metal plating layer, the battery electrode It is a conductive substrate for
- Another aspect of the present invention includes a step of applying a surface treatment agent containing a compound ⁇ to both surfaces of a base material layer, and forming a metal plating layer by plating on both surfaces of the base material layer coated with the surface treatment agent. wherein the density of the base material layer is lower than the density of the metal plating layer, and the first functional group capable of reacting and bonding with the base material layer, and the metal A method for producing a conductive substrate for a battery electrode, which has a plating layer and a second functional group capable of reacting and bonding.
- a conductive substrate for battery electrodes with high adhesion of a metal plating layer it is possible to provide a conductive substrate for battery electrodes with high adhesion of a metal plating layer, and a method for manufacturing the same.
- FIG. 1 is a schematic cross-sectional view showing a conductive substrate for a battery electrode according to one embodiment of the present invention
- FIG. 1 is a flowchart of a method for manufacturing a conductive substrate for battery electrodes according to one embodiment of the present invention
- a conductive substrate for a battery electrode according to one embodiment of the present invention shown in FIG. It is a laminated body provided with metal plating layers 12a and 12b laminated on the rear surface side) with a compound ⁇ interposed therebetween. Between the substrate layer 11 and each of the metal plating layers 12a and 12b, the compound ⁇ is interposed, and intermediate layers 13a and 13b containing the compound ⁇ are present between the layers.
- the intermediate layers 13a and 13b may be laminated on the entire front surface or rear surface of the base material layer 11, as shown in FIG.
- the intermediate layers 13 a and 13 b may be laminated up to the side surfaces of the base material layer 11 .
- the intermediate layers 13a, 13b may be present as continuous layers or intermittent layers.
- the intermediate layers 13a and 13b are usually very thin layers, it may not be possible to confirm that they are layers with an optical microscope or the like. It is sufficient if the existence of ⁇ can be confirmed.
- the intermediate layers 13a and 13b may be layers derived from the compound ⁇ .
- the metal plating layers 12a and 12b may also be laminated to the side surfaces of the base material layer 11 via the compound ⁇ .
- the compound ⁇ having two kinds of predetermined functional groups is interposed between the base material layer 11 and the metal plating layers 12a and 12b, separation between the layers is difficult to occur, and the base material The adhesion of the metal plating layers 12a and 12b to the layer 11 is high.
- the compound ⁇ may react with the substance constituting at least one of the base material layer 11 and the metal plating layers 12a and 12b and exist between the layers in a chemically bonded state.
- the chemical bond means covalent bond, ionic bond, bond by intermolecular force, etc., preferably covalent bond or ionic bond.
- the density of the base material layer 11 is lower than that of the metal plating layers 12a and 12b.
- the densities of the substrate layer 11 and the metal plating layers 12a and 12b can be values measured by the Archimedes method.
- the density of each layer is the density of the substance itself forming the layer (true density ).
- a metal substrate (typically, a metal made of a material forming the metal plating layers 12a and 12b) is used.
- substrate can be a lower density substrate.
- the density of the substrate layer 11 should be lower than the density of at least one of the two metal plating layers 12a and 12b, and should be lower than the density of both. is preferred.
- the upper limit of the density of the base layer 11 is preferably 8 g/cm 3 , more preferably 6 g/cm 3 , still more preferably 4 g/cm 3 , 3 g/cm 3 , 2.5 g/cm 3 , 2.0 g/cm 3 . cm 3 or 1.5 g/cm 3 are even more preferred.
- the density of the base material layer 11 By setting the density of the base material layer 11 to the above upper limit or less, the density of the conductive substrate 10 can be sufficiently reduced.
- the lower limit of this density is preferably 0.5 g/cm 3 , more preferably 1.0 g/cm 3 .
- the material constituting the base material layer 11 can be appropriately selected from those having a density lower than that of the material constituting the metal plating layers 12a and 12b.
- the substance constituting the base material layer 11 is preferably resin, ceramic, glass fiber, paper, or a composite material containing one or more of these.
- Resins include polyimide (PI), polyamide, fluorine resin (polytetrafluoroethylene (PTFE), polyvinylidene fluoride (PVDF), etc.), liquid crystal polymer (LCP), polyetheretherketone (PEEK), polyphenylene sulfide ( PPS), polyphenylene oxide, polyphenylene ether, cycloolefin polymer (COP), bismaleimide triazine resin (BT), epoxy resin, phenolic resin, polyester (polyethylene terephthalate (PET), polyethylene naphthalate (PEN), etc.), nylon (nylon 6, 10, nylon 4, 6, etc.), acrylic resin (polymethyl methacrylate (PMMA), polyacrylate, sodium polyacrylate, polyacrylonitrile, polyacrylamide, etc.), ABS resin, polyvinyl chloride, polyolefin (polyethylene , polypropylene, etc.), polystyrene, polyurethane, and the like.
- PI polyimide
- Ceramics include alumina ceramics and the like.
- the glass fiber may be woven fabric or non-woven fabric.
- composite materials include woven or non-woven glass fiber, paper impregnated with resin, glass fiber dispersed in resin, and a mixture of multiple resins.
- the substance constituting the base material layer 11 preferably contains a resin, and more preferably contains a polyimide or a fluororesin.
- the base material layer 11 may be composed mainly of resin.
- the term "main component” means a component with the highest content on a mass basis, preferably a component with a content of 50% by mass or more, and more preferably a component with a content of 70% by mass or more. preferable.
- the lower limit of the resin content in the base material layer 11 is preferably 70% by mass, more preferably 80% by mass, and even more preferably 90% by mass.
- the upper limit of the resin content in the base material layer 11 may be 100% by mass or 99% by mass.
- the base material layer 11 may contain antioxidants, pigments, dyes, plasticizers, ultraviolet absorbers, fillers, flame retardants, antiblocking agents, etc., as necessary.
- the average thickness of the base material layer 11 is not particularly limited and can be appropriately set as necessary, but the lower limit is preferably 1 ⁇ m, more preferably 3 ⁇ m, and even more preferably 5 ⁇ m. Sufficient strength can be maintained by setting the average thickness of the base material layer 11 to the above lower limit or more.
- the upper limit of the average thickness of the substrate layer 11 may be, for example, 300 ⁇ m or 100 ⁇ m, preferably 50 ⁇ m, more preferably 30 ⁇ m, even more preferably 20 ⁇ m, and even more preferably 10 ⁇ m.
- the term "average thickness” means the average value of thicknesses measured at arbitrary 10 points.
- the lower limit of the ratio of the average thickness of the base layer 11 to the average thickness of the conductive substrate 10 is preferably 30%, more preferably 50%, even more preferably 60%, and even more preferably 70% or 80%. In some cases. By setting the ratio of the average thickness of the base material layer 11 to the average thickness of the conductive substrate 10 to be equal to or greater than the above lower limit, the density of the conductive substrate 10 can be sufficiently reduced.
- the upper limit of the ratio of the average thickness of the base material layer 11 to the average thickness of the conductive substrate 10 is preferably 99%, more preferably 90%, and even more preferably 80% in some cases. By setting the ratio of the average thickness of the base material layer 11 to the average thickness of the conductive substrate 10 to be equal to or less than the above upper limit, it is possible to improve adhesion, conductivity, etc. of the metal plating layers 12a and 12b.
- the surface of the base material layer 11 may be subjected to corona treatment, plasma treatment, blast treatment, solvent treatment, primer treatment, defluorination treatment, or the like.
- surface roughening treatment such as blasting treatment is not performed.
- the surface roughness (Ra) of the surface generally exceeds 1 ⁇ m, for example.
- the upper limit of the surface roughness (Ra) of the substrate layer 11 is preferably 1 ⁇ m, more preferably 0.5 ⁇ m, and even more preferably 0.1 ⁇ m.
- the lower limit of the surface roughness of the base material layer 11 may be, for example, 0.001 ⁇ m, 0.005 ⁇ m, or 0.01 ⁇ m.
- surface roughness (Ra) refers to a value (arithmetic mean roughness).
- the surface roughness of the base material layer 11 is the value in the region where the metal plating layers 12a and 12b are laminated via the compound ⁇ .
- the surface roughness (Ra) is a value measured in a region where the holes do not exist.
- the base material layer 11 may have a structure without pores (non-porous structure), or may have a porous structure. Having a structure is preferred. By using the substrate layer 11 having such a two-dimensional porous structure, the adhesion of the metal plating layers 12a and 12b can be further enhanced.
- the lower limit of the diameter of the holes (through holes) formed in the base material layer 11 is preferably 1 ⁇ m, more preferably 10 ⁇ m, for example.
- the upper limit of this diameter is preferably 200 ⁇ m, more preferably 100 ⁇ m.
- the metal plating layers 12a and 12b are metal layers formed by plating.
- the lower limit of the metal content in the metal plating layers 12a and 12b is preferably 90% by mass, more preferably 99% by mass.
- the upper limit of the metal content in the metal plating layers 12a and 12b may be 100% by mass.
- metal contained in the metal plating layers 12a and 12b it is possible to form a layer by plating, and metals or the like commonly used for substrates for battery electrodes can be used. It can be selected as appropriate. Specific examples of the metal contained in the metal plating layers 12, 12b include copper, nickel, silver, etc. Copper and nickel are preferred, and copper is more preferred.
- the metal plating layers 12a, 12b may be copper plating layers.
- the lower limit of the average thickness of each of the metal plating layers 12a and 12b is preferably 0.5 ⁇ m, more preferably 1 ⁇ m.
- the upper limit of the average thickness of each of the metal plating layers 12a and 12b may be, for example, 50 ⁇ m, but is preferably 20 ⁇ m, more preferably 10 ⁇ m, and even more preferably 3 ⁇ m in some cases.
- each metal plating layer 12a, 12b may have a single-layer structure or a multi-layer structure.
- the compound ⁇ interposed between the base material layer 11 and the metal plating layers 12a and 12b will be described below.
- the compound ⁇ forms the intermediate layers 13a, 13b.
- the intermediate layers 13a and 13b may contain components other than the compound ⁇ .
- the compound ⁇ contained in each of the two intermediate layers 13a and 13b may be the same or different.
- Compound ⁇ can be used alone or in combination of two or more.
- Compound ⁇ is considered to be a material for forming a conjugate (bond) of two substances through interfacial molecular bonding.
- Interfacial molecular bonding means intervening a certain compound at the interface of two substances and chemically bonding each substance and the compound by chemical reaction to bond the two substances, or a bond resulting therefrom. .
- the compound ⁇ has a first functional group capable of reacting and bonding with the base material layer 11 and a second functional group capable of reacting and bonding with the metal plating layers 12a and 12b.
- the first functional group is preferably a group that reacts and bonds with the resin.
- the first functional group include an amino group, a hydrazino group, a hydroxy group, a thiol group, an oxiranyl group, an oxetanyl group, a carboxy group, an aziridinyl group, an azide group, an azidosulfonyl group, and a diazomethyl group.
- group or diazomethyl group hereinafter, "azido group, azidosulfonyl group or diazomethyl group” is also referred to as azido group, etc.).
- An azide group or the like can form a chemical bond such as “—NC—type” mainly with an organic substance such as a resin through a chemical reaction.
- the first functional group is an azide group or the like, stronger bonding with the base material layer 11 is possible.
- Compound ⁇ preferably has an aromatic ring. More preferably, compound ⁇ has an aromatic ring, and the first functional group is an azide group, an azidosulfonyl group, or a diazomethyl group directly bonded to this aromatic ring.
- aromatic rings include aromatic carbocyclic rings such as benzene ring and naphthalene ring, and aromatic heterocyclic rings such as thiophene ring, furan ring and triazine ring.
- the aromatic ring is preferably an aromatic carbocyclic ring, more preferably a benzene ring.
- the rate of the reaction in which the nitrogen molecule (N 2 ) is eliminated from the azide group or the like by ultraviolet irradiation or heating is increased compared to the case where it is not. Therefore, by using the compound ⁇ in which an azide group or the like is directly bonded to the benzene ring, good adhesion can be obtained by heat treatment at a relatively low temperature for a short period of time without ultraviolet irradiation. Therefore, by using such a compound ⁇ , efficient treatment becomes possible.
- the second functional group is preferably a group that reacts with and bonds to the metal.
- the second functional group include an amino group, a thiol group, a catechol group, a carboxy group, a phosphonic acid group, a silanol group, an alkoxysilyl group, etc.
- a silanol group or an alkoxysilyl group is preferred.
- a silanol group and an alkoxysilyl group can mainly form a "-Si-OM-type" chemical bond with an inorganic material M such as a metal through a chemical reaction.
- An alkoxysilyl group is a group in which an alkoxy group (oxyhydrocarbon group) is bonded to a silicon atom.
- An alkoxy group refers to a group in which a hydrocarbon group is bonded to an oxygen atom, and examples thereof include a methoxy group, an ethoxy group, a propoxy group, a vinyloxy group, a phenoxy group, and a benzyloxy group.
- the number of alkoxy groups attached to the silicon atom may be 1, 2 or 3, with 3 being preferred.
- alkoxysilyl group a group other than an alkoxy group may be bonded to the silicon atom, and examples of such groups include an alkyl group, a phenyl group, a hydroxy group, and a hydrogen atom.
- alkoxy group an alkoxy group having 1 to 12 carbon atoms is preferable, an alkoxy group having 1 to 3 carbon atoms is preferable, and a methoxy group, an ethoxy group and a propoxy group are more preferable.
- alkoxysilyl groups include trimethoxysilyl groups, triethoxysilyl groups, tribenzyloxysilyl groups, and the like. Further, hydrolysis of an alkoxysilyl group usually produces a silanol group.
- a preferred form of the compound ⁇ is A compound ⁇ 1 represented by the following formula (1) or (2) and a compound ⁇ 2 obtained by hydrolytic condensation of a hydrolyzable silane compound containing the compound ⁇ 1 is mentioned.
- the compound ⁇ is at least one of the compound ⁇ 1 and the compound ⁇ 2
- good adhesion is exhibited by heat treatment at a relatively low temperature for a short period of time without UV irradiation. Therefore, the use of these compounds enables efficient treatment.
- Compound ⁇ 1 is a compound represented by the following formula (1) or (2). That is, the compound ⁇ 1 is an example of a compound ⁇ having an azide group or the like directly bonded to a benzene ring as the first functional group and a silanol group or an alkoxysilyl group as the second functional group.
- R 1 is a hydrogen atom, an alkyl group having 1 to 12 carbon atoms, a phenyl group, an alkoxy group having 1 to 12 carbon atoms, or a hydroxy group.
- a plurality of R 2 are each independently a hydrogen atom, a halogen atom, or a monovalent organic group.
- X 1 is an azide group, an azidosulfonyl group, or a diazomethyl group.
- Y 1 is a single bond, an ester group, an ether group, a thioether group, an amide group, a urethane group, a urea group, a group represented by —NHR 3 —, or a group represented by the following formula (3a) or (3b) is.
- R 3 is an alkyl group having 1 to 6 carbon atoms.
- Z 1 is a single bond, an alkanediyl group having 1 to 12 carbon atoms, or -NH-, -O-, -S- and -S between the terminal or carbon-carbon bond of an alkanediyl group having 1 to 12 carbon atoms It is a group containing one or more groups of (O)-.
- m is an integer from 1 to 3;
- R 1 , X 1 , Y 1 and Z 1 is plural, each independently satisfies the above definition.
- at least one of one or more R 1 is an alkoxy group having 1 to 12 carbon atoms.
- a plurality of R 4 , R 5 and R 6 are each independently a hydrogen atom, an alkyl group having 1 to 12 carbon atoms, a phenyl group, an alkoxy group having 1 to 12 carbon atoms, or a hydroxy group. and at least one of the plurality of R 4 , R 5 and R 6 is an alkoxy group having 1 to 12 carbon atoms.
- a plurality of R 7 are each independently a hydrogen atom, a halogen atom, or a monovalent organic group.
- X2 is an azide group, an azidosulfonyl group, or a diazomethyl group.
- a plurality of Z 2 are each independently a single bond, an alkanediyl group having 1 to 12 carbon atoms, or -NH-, -O- , -S- and -S(O)-.
- a methanediyl group which is an alkanediyl group having 1 carbon atom, is a group represented by —CH 2 — and may be referred to as a methylene group.
- a 2-12 carbon alkanediyl group may be referred to as a 2-12 carbon alkylene group.
- R8 is a hydrogen atom or a methyl group.
- alkyl groups having 1 to 12 carbon atoms represented by R 1 , R 4 , R 5 and R 6 include methyl group, ethyl group, propyl group, butyl group and octyl group.
- alkoxy group having 1 to 12 carbon atoms represented by R 1 , R 4 , R 5 and R 6 include the alkoxy groups described above.
- Halogen atoms represented by R 2 and R 7 include fluorine, chlorine and bromine atoms.
- the monovalent organic group represented by R 2 and R 7 includes a monovalent hydrocarbon group, an alkoxy group, and -Y 1 -Z 1 -Si-R 13 (Y 1 , Z 1 and R 1 are are the same as Y 1 , Z 1 and R 1 in formula (1)), a group represented by —COO—N—(—Z 2 —SiR 4 R 5 R 6 ) 2 (Z 2 , R 4 , R 5 and R 6 have the same meanings as Z 2 , R 4 , R 5 and R 6 in formula (2), respectively.), groups represented by formula (14) described later, and the like.
- Examples of the alkyl group having 1 to 6 carbon atoms represented by R 3 include methyl group, ethyl group, propyl group and butyl group.
- R 1 is preferably an alkoxy group having 1 to 12 carbon atoms, more preferably an alkoxy group having 1 to 6 carbon atoms, and still more preferably an alkoxy group having 1 to 3 carbon atoms.
- a hydrogen atom is preferred as R 2 .
- X 1 is preferably an azide group or an azidosulfonyl group. X 1 is preferably bonded to the group containing Y 1 and the like at the para-position or meta-position.
- Y 1 is preferably an amide group, more preferably an amide group represented by *-CONH- (* indicates a bonding site with a benzene ring).
- Z 1 is preferably an alkanediyl group (alkylene group) having 2 to 12 carbon atoms, more preferably an alkanediyl group (alkylene group) having 2 to 6 carbon atoms.
- m is preferably 3.
- R 4 , R 5 and R 6 are preferably alkoxy groups having 1 to 12 carbon atoms, more preferably alkoxy groups having 1 to 6 carbon atoms, and even more preferably alkoxy groups having 1 to 3 carbon atoms.
- a hydrogen atom is preferred as R7 .
- X2 is preferably an azide group or an azidosulfonyl group.
- X 2 is preferably bonded to the group represented by -COO-N-(-Z 2 -SiR 4 R 5 R 6 ) 2 at the para- or meta-position.
- Z 2 is preferably an alkanediyl group (alkylene group) having 2 to 12 carbon atoms, more preferably an alkanediyl group (alkylene group) having 2 to 6 carbon atoms.
- the compound ⁇ 1 may be a compound represented by the following formula (11), (12) or (13).
- X 10 , X 11 and X 12 are each independently an azide group, an azidosulfonyl group or a diazomethyl group.
- E 11 and E 12 are each independently a carbonyl group and an alkanediyl group having 1 to 12 carbon atoms.
- Y 11 , Y 12 , Y 13 and Y 14 are each independently a hydrogen atom, an alkyl group having 1 to 12 carbon atoms, or —J 13 —Si(OA 10 ) 3-k (R 10 ) k It is a group that is J 11 , J 12 and J 13 are each independently an alkanediyl group having 1 to 12 carbon atoms, or an oxygen atom (—O—) between the carbon-carbon bonds of an alkanediyl group having 2 to 12 carbon atoms.
- Y 15 is a group represented by -R 15 or -OA 15
- Y 16 is a group represented by -R 16 or -OA 16
- a 10 , A 15 and A 16 are each independently an alkyl group having 1 to 4 carbon atoms, a benzyl group or a hydrogen atom.
- R 10 , R 15 and R 16 are each independently an alkyl group having 1 to 4 carbon atoms or a benzyl group.
- k is an integer from 0 to 2;
- Q10 is a hydrogen atom or an organic group represented by formula (4).
- formulas (11) and (12) at least one of Y 11 and Y 12 contains an oxygen atom.
- formula (13) at least one of Y 15 and Y 16 contains an oxygen atom.
- the groups X 11 and X 12 attached to the benzene ring are each independently attached to the para or meta position.
- the method for synthesizing the compound ⁇ 1 is not particularly limited. b, and a compound B having a benzene ring and at least one group selected from the group consisting of an azide group, an azidosulfonyl group and a diazomethyl group, by a known method.
- Examples of the combination of the reactive group a and the reactive group b include a combination of an isocyanate group, an epoxy group, an amino group, etc., and a carboxy group.
- silane coupling agent A examples include 3-isocyanatopropyltriethoxysilane, 3-glycidoxypropyltriethoxysilane, 3-glycidoxypropylmethyldiethoxysilane, 3-glycidoxypropyltrimethoxysilane, 2-( 3,4-epoxycyclohexyl)ethyltriethoxysilane, 2-(3,4-epoxycyclohexyl)ethyltrimethoxysilane, N-2-(aminoethyl)-3-aminopropyltrimethoxysilane, N-2-( aminoethyl)-3-aminopropyltriethoxysilane, 3-aminopropyltrimethoxysilane, 3-aminopropyltriethoxysilane, bis(3-triethoxysilylpropyl)amine, bis(3-trimethoxysilylpropyl)amine, bis(3-aminopropy
- Examples of compound B include azidobenzoic acid, azidosulfonylbenzoic acid, diazomethylbenzoic acid, 3-(4-azidophenyl)propionic acid, chlorides of these carboxylic acids, azidoaniline, and azidophenol.
- Compound ⁇ 2 In compound ⁇ 2, an unreacted alkoxysilyl group usually remains. That is, the compound ⁇ 2 is also an example of the compound ⁇ having an azide group or the like directly bonded to a benzene ring as the first functional group and a silanol group or an alkoxysilyl group as the second functional group.
- a compound ⁇ 2 obtained by hydrolyzing and condensing a hydrolyzable silane compound containing the compound ⁇ 1 has a structural unit A derived from the compound ⁇ 1.
- the compound ⁇ 2 may be obtained by other synthetic methods as long as the structure is the same as that of a compound obtained by hydrolytic condensation of a hydrolyzable silane compound including the compound ⁇ 1.
- Compound ⁇ 2 is preferably a silsesquioxane compound.
- Compound ⁇ 2 preferably has at least one of an alkoxysilyl group and a hydroxysilyl group, more preferably a hydroxysilyl group.
- Structural unit A includes structural units represented by the following formula (4).
- the structural unit represented by the following formula (4) is a structural unit derived from the compound ⁇ 1 represented by the formula (1) in which m is 3.
- R 1 , R 2 , X 1 , Y 1 and Z 1 are synonymous with R 1 , R 2 , X 1 , Y 1 and Z 1 in formula (1).
- a is an integer from 0 to 2;
- R 1 , R 2 , X 1 , Y 1 and Z 1 in formula (4) are the same as specific examples of R 1 , R 2 , X 1 , Y 1 and Z 1 in formula (1) is.
- R 1 in formula (4) is preferably a hydroxy group or an alkoxy group, more preferably a hydroxy group.
- a 1 is preferable.
- the lower limit of the content of structural unit A relative to all structural units in compound ⁇ 2 is preferably 10 mol%, more preferably 20 mol%, and even more preferably 30 mol%.
- the upper limit of this content is preferably 90 mol%, more preferably 80 mol%, and even more preferably 70 mol%.
- Compound ⁇ 2 preferably has a structural unit B containing an amino group (—NH 2 ).
- Hydrolyzable silane compounds that give structural unit B include 3-aminopropyltrimethoxysilane, 3-aminopropyltriethoxysilane, N-2-(aminoethyl)-3-aminopropylmethyldimethoxysilane, N-2- (Aminoethyl)-3-aminopropyltrimethoxysilane and the like.
- the lower limit of the content of structural unit B relative to all structural units in compound ⁇ 2 is preferably 10 mol%, more preferably 20 mol%, and even more preferably 30 mol%.
- the upper limit of this content is preferably 90 mol%, more preferably 80 mol%, and even more preferably 70 mol%.
- the compound ⁇ 2 may have a structural unit C other than the structural unit A and the structural unit B.
- Examples of the hydrolyzable silane compound that provides the structural unit C include compounds represented by the following formula (C).
- R d is a hydrogen atom, an alkyl group having 1 to 10 carbon atoms, an alkenyl group having 2 to 10 carbon atoms, an aryl group having 6 to 15 carbon atoms, or an organic group having a reactive group.
- a plurality of R d may be the same or different.
- R e is a hydrogen atom, an alkyl group having 1 to 10 carbon atoms, an acyl group having 2 to 6 carbon atoms, or an aryl group having 6 to 15 carbon atoms, and a plurality of R e may be the same or different.
- x represents an integer of 0 to 3; Further, these alkyl groups, alkenyl groups and aryl groups may be either unsubstituted or substituted, and can be selected depending on the properties.
- alkyl groups represented by R d and R e include methyl group, ethyl group, n-propyl group, isopropyl group, n-butyl group, t-butyl group, n-hexyl group and n-decyl group. , trifluoromethyl group, 3,3,3-trifluoropropyl group, 3-glycidoxypropyl group, 2-(3,4-epoxycyclohexyl)ethyl group, [(3-ethyl-3-oxetanyl)methoxy]
- a propyl group, a 3-mercaptopropyl group, a 3-isocyanatopropyl group and the like can be mentioned.
- alkenyl group represented by R d include vinyl group, 3-acryloxypropyl group, 3-methacryloxypropyl group and the like.
- aryl group represented by R d and R e include a phenyl group, a tolyl group, a p-hydroxyphenyl group, a p-methoxyphenyl group, a 1-(p-hydroxyphenyl)ethyl group, a 2-(p -hydroxyphenyl)ethyl group, 4-hydroxy-5-(p-hydroxyphenylcarbonyloxy)pentyl group, naphthyl group and the like.
- Examples of the organic group having a reactive group represented by Rd include an isocyanate group, a group having an isocyanurate structure and an alkoxysilyl group, and the like.
- the number of carbon atoms in the organic group having a reactive group represented by Rd is preferably 1 or more and 40 or less.
- a specific example of the acyl group represented by Re is an acetyl group.
- hydrolyzable silane compounds represented by formula (C) include tetrafunctional silanes such as tetramethoxysilane, tetraethoxysilane, tetrapropoxysilane, tetraacetoxysilane and tetraphenoxysilane, methyltrimethoxysilane, methyltriethoxysilane, methyltriisopropoxysilane, methyltri-n-butoxysilane, ethyltrimethoxysilane, ethyltriethoxysilane, ethyltriisopropoxysilane, ethyltri-n-butoxysilane, n-propyltrimethoxysilane, n-propyltri ethoxysilane, n-butyltrimethoxysilane, n-butyltriethoxysilane, n-hexyltrimethoxysilane, n-hexyl
- hydrolyzable silane compound represented by the formula (C) has 5 or more silicon-bonded alkoxy groups such as 1,3,5-tris[3-(trimethoxysilyl)propyl]isocyanurate. Also included are compounds having
- the hydrolyzable silane compound may be used alone or in combination of two or more.
- the weight average molecular weight (Mw) of compound ⁇ 2 is not particularly limited, but is preferably 1,000 or more and 100,000 or less, more preferably 2,000 or more and 50,000 in terms of polystyrene measured by GPC (gel permeation chromatography). It is below.
- the compound ⁇ 2 is obtained by (i) a method of hydrolyzing and condensing a hydrolyzable silane compound containing the compound ⁇ 1, and (ii) a hydrolytic condensate of a hydrolyzable silane compound having a structural unit B.
- Compound X having a reactive group capable of binding reaction with an amino group, a benzene ring, and at least one group selected from the group consisting of an azide group, an azidosulfonyl group and a diazomethyl group (azidobenzoic acid, azidosulfonylbenzoic acid, diazomethylbenzoic acid, etc.).
- the amino group in structural unit B reacts with compound X to form structural unit A.
- General methods can be used for hydrolytic condensation to obtain compound ⁇ 2.
- a solvent, water, and optionally a catalyst are added to a hydrolyzable silane compound, and the mixture is heated and stirred at 30 to 150° C. for about 0.5 to 100 hours.
- hydrolysis by-products alcohol such as methanol
- condensation by-products water
- acid catalysts and base catalysts are preferably used.
- acid catalysts include hydrochloric acid, nitric acid, sulfuric acid, hydrofluoric acid, phosphoric acid, acetic acid, trifluoroacetic acid, formic acid, polyvalent carboxylic acids or their anhydrides, and ion exchange resins.
- basic catalysts include triethylamine, tripropylamine, tributylamine, tripentylamine, trihexylamine, triheptylamine, trioctylamine, diethylamine, triethanolamine, diethanolamine, sodium hydroxide, potassium hydroxide, amino alkoxysilanes having groups, ion-exchange resins, and the like.
- the amount of the catalyst to be added is preferably 0.01 to 10 parts by mass with respect to 100 parts by mass of the hydrolyzable silane compound.
- the solution after hydrolytic condensation does not contain a catalyst, and the catalyst can be removed as necessary.
- the removal method is not particularly limited, but preferably includes water washing and/or ion exchange resin treatment. Washing with water is a method of diluting a solution with a suitable hydrophobic solvent, washing with water several times, and concentrating the obtained organic layer with an evaporator.
- Ion exchange resin treatment is a method of contacting a solution with a suitable ion exchange resin.
- the solvent used for the hydrolytic condensation reaction is not particularly limited, but a compound having an alcoholic hydroxyl group is preferably used.
- the compound having an alcoholic hydroxyl group is not particularly limited, it is preferably a compound having a boiling point of 110 to 250°C under atmospheric pressure.
- compounds having an alcoholic hydroxyl group include acetol, 3-hydroxy-3-methyl-2-butanone, 4-hydroxy-3-methyl-2-butanone, 5-hydroxy-2-pentanone, 4-hydroxy- 4-methyl-2-pentanone (diacetone alcohol), ethyl lactate, butyl lactate, propylene glycol monomethyl ether, propylene glycol monoethyl ether, propylene glycol mono-n-propyl ether, propylene glycol mono-n-butyl ether, propylene glycol mono-t- Butyl ether, diethylene glycol monomethyl ether, diethylene glycol monoethyl ether, dipropylene glycol monomethyl ether, dipropylene glycol monoethyl ether, 3-methoxy-1-butanol, 3-methoxy-3-methyl-1-butanol and the like.
- These alcoholic hydroxyl-containing compounds may be used alone or in combination of two or more.
- solvents may be used together with the compound having an alcoholic hydroxyl group.
- Other solvents include ethyl acetate, n-propyl acetate, isopropyl acetate, n-butyl acetate, isobutyl acetate, propylene glycol monomethyl ether acetate, 3-methoxy-1-butyl acetate, 3-methyl-3-methoxy-1- Esters such as butyl acetate and ethyl acetoacetate, ketones such as methyl isobutyl ketone, diisopropyl ketone, diisobutyl ketone and acetylacetone, diethyl ether, diisopropyl ether, di-n-butyl ether, diphenyl ether, diethylene glycol methyl ethyl ether, diethylene glycol dimethyl ether, etc.
- Ethers ⁇ -butyrolactone, ⁇ -valerolactone, ⁇ -valerolactone, propylene carbonate, N-methylpyrrolidone, cyclopentanone, cyclohexanone, cycloheptanone and the like.
- the compound represented by the formula (19) is a silsesquioxane compound composed of 1, m, and n of the three types of structural units shown in the formula (19) bonded together, X is an azide group, l is any integer of 0 or more, m is any integer of 1 or more, and n is any integer of 0 or more.
- R a , R b and R c are each independently a hydrogen atom, a hydroxy group, an alkoxy group or —O—.
- R f is a hydrogen atom, a hydroxy group, an alkoxy group, an alkyl group having 1 to 10 carbon atoms, an alkenyl group having 2 to 10 carbon atoms, an aryl group having 6 to 15 carbon atoms, or an organic group having a reactive group group, and a plurality of R f may be the same or different.
- These alkyl groups, alkenyl groups, and aryl groups may be either unsubstituted or substituted, and can be selected depending on the properties.
- the compounds are water soluble except when the value of the ratio l/(m+n) is close to 0 (eg, less than 0.2 or less than 0.1). That is, the lower limit of the ratio l/(m+n) is preferably 0.2, more preferably 0.5, and even more preferably 1, from the viewpoint of water solubility.
- the upper limit of the ratio l/(m+n) is preferably 5, more preferably 2.
- compound ⁇ include: A compound ⁇ 3 represented by the following formula (5) and a compound ⁇ 4 obtained by hydrolyzing and condensing a hydrolyzable silane compound containing the compound ⁇ 3 is mentioned.
- Compound ⁇ 3 is a compound represented by the following formula (5).
- X21 is the first functional group.
- X 22 is a first functional group or a group represented by —N(R 21 ) 2 .
- a plurality of R 21 are each independently a hydrogen atom, a hydrocarbon group having 1 to 24 carbon atoms, or a group represented by —R 22 —Si(OR 23 ) 3-p (R 24 ) p .
- R 22 is an alkanediyl group having 1 to 12 carbon atoms.
- R 23 is a hydrogen atom or an alkyl group having 1 to 4 carbon atoms.
- R 24 is an alkyl group having 1 to 4 carbon atoms.
- p is an integer of 0 or more and 2 or less.
- at least one of the plurality of R 21 in the compound represented by formula (5) is a group represented by —R 22 —Si(OR 23 ) 3-p (R 24 ) p .
- the first functional group represented by X 21 or X 22 is preferably an amino group, a thiol group, an azide group, an azidosulfonyl group or a diazomethyl group, more preferably an azide group, an azidosulfonyl group or a diazomethyl group, and an azide group. More preferred.
- X 22 is preferably the first functional group.
- n-TES, P-TES, A-TES, etc. manufactured by Io Kagaku Kenkyusho Co., Ltd. can be used.
- compound ⁇ 3 examples include 2,4-diazido-6-(3-triethoxysilylpropyl)amino-1,3,5-triazine and 2,4-diazido-6-(4-triethoxysilylbutyl) Amino-1,3,5-triazine, 6-(3-triethoxysilylpropyl)amino-1,3,5-triazine-2,4-dithiol, 2,4-diamino-6-(3-triethoxysilyl propyl)amino-1,3,5-triazine and the like.
- Compound ⁇ 4 is a compound obtained by hydrolyzing and condensing a hydrolyzable silane compound containing compound ⁇ 3.
- Compound ⁇ 4 is a hydrolytic condensate similar to compound ⁇ 2 except that compound ⁇ 3 is used instead of compound ⁇ 1.
- the intermediate layers 13a and 13b may contain components other than the compound ⁇ . Other components include unreacted substances and side reaction products when synthesizing compound ⁇ .
- the lower limit of the content of compound ⁇ in intermediate layers 13a and 13b is preferably 50% by mass, more preferably 70% by mass, and even more preferably 90% by mass.
- the high content ratio of the compound ⁇ in the intermediate layers 13a and 13b can further enhance the bondability (cohesiveness) between the layers.
- the intermediate layers 13a and 13b are usually very thin layers, and if the compound ⁇ is present, a sufficient effect of improving adhesion can be confirmed. Therefore, the lower limit of the average thickness of one layer of the intermediate layers 13a and 13b is not particularly limited, and may be 1 nm, 10 nm, 50 nm, or 100 nm. On the other hand, the upper limit of the average thickness of one layer of the intermediate layers 13a and 13b may be, for example, 10 ⁇ m, 1 ⁇ m, 100 nm, 50 nm, or 10 nm. good too.
- the conductive substrate 10 is used as an electrode (positive electrode or negative electrode) of a battery.
- the battery may be a chemical battery such as a primary battery, a secondary battery, or a fuel cell. Since the conductive substrate 10 has high adhesion of the metal plating layer and is excellent in durability, it is particularly suitable as a substrate for an electrode of a secondary battery that is repeatedly charged and discharged for a long period of time.
- the conductive substrate 10 can be used as a positive electrode substrate and can also be used as a negative electrode substrate.
- the electrode (positive electrode or negative electrode) is manufactured, for example, by laminating a layer containing a positive electrode active material or a negative electrode active material on the surface of the conductive substrate 10 . Further, depending on the type of battery such as nickel-hydrogen battery, the conductive substrate 10 can be used as an electrode as it is.
- the upper limit of the density of the conductive substrate 10 is preferably 8 g/cm 3 , more preferably 6 g/cm 3 , still more preferably 5 g/cm 3 and even more preferably 4 g/cm 3 .
- the lower limit of the density of the conductive substrate 10 is preferably 1.5 g/cm 3 , more preferably 2.0 g/cm 3 , more preferably 2.5 g/cm 3 or 3.0 g from the viewpoint of strength. /cm 3 is more preferred.
- the lower limit of the average thickness of the conductive substrate 10 is preferably 3 ⁇ m, more preferably 5 ⁇ m, and even more preferably 7 ⁇ m. By setting the average thickness of the conductive substrate 10 to the lower limit or more, sufficient strength can be maintained.
- the upper limit of the average thickness of the conductive substrate 10 may be, for example, 100 ⁇ m, preferably 50 ⁇ m, more preferably 40 ⁇ m, and even more preferably 30 ⁇ m, 20 ⁇ m, 15 ⁇ m, or 12 ⁇ m. By making the average thickness of the conductive substrate 10 equal to or less than the upper limit, it is possible to reduce the thickness and weight of electrodes and batteries manufactured using the conductive substrate 10 .
- a method for manufacturing a conductive substrate for a battery electrode (conductive substrate) comprises: A step of applying a surface treatment agent containing a compound ⁇ to both surfaces of the substrate layer (surface treatment agent application step), and a step of forming a metal plating layer by plating on both surfaces of the substrate layer coated with the surface treatment agent. (Metal plating layer forming step) Prepare.
- the density of the base material layer (the material that forms the base material layer) is lower than the density of the metal plating layer (the metal material that forms the metal plating layer). That is, the materials for the base material layer and the metal plating layer are selected so as to achieve such a magnitude relationship in density. Suitable materials for the base material layer and the metal plating layer are as described above.
- the compound ⁇ contained in the surface treatment agent has a first functional group capable of reacting and bonding with the substrate layer and a second functional group capable of reacting and bonding with the metal plating layer.
- a first functional group capable of reacting and bonding with the substrate layer and a second functional group capable of reacting and bonding with the metal plating layer.
- Specific examples and suitable examples of the compound ⁇ are as described in the conductive substrate according to one embodiment of the present invention.
- the term “apply” means “adhering” or “existing in contact with” a liquid to a target object. It includes being “attached” or “being in contact with” by methods such as roll, ink-jet printing, dipping, and the like.
- the manufacturing method further includes a step (UV irradiation/heating step) of performing at least one of ultraviolet irradiation and heating on the applied compound ⁇ after the step of applying the surface treatment agent.
- the method for manufacturing a conductive substrate according to an embodiment of the present invention may include a degreasing cleaning step and a pretreatment step before the surface treatment agent coating step.
- the method for manufacturing a conductive substrate shown in the flow chart of FIG. 2 includes, in this order, a degreasing cleaning step S1, a pretreatment step S2, a surface treatment agent coating step S3, a UV irradiation/heating step S4, and a metal plating layer forming step S5. .
- Steps other than the surface treatment agent applying step S3 and the metal plating layer forming step S5 are optional steps.
- the combination of the surface treatment agent application step S3 and the UV irradiation/heating step S4 may be repeated multiple times. By doing so, a sufficient amount of the compound ⁇ can be provided on the substrate layer surface.
- the degreasing and washing step S1 is a step of washing the base layer (material to be the base layer) using a solvent or the like, for example.
- a solvent such as acetone or ethanol
- ultrasonically cleaning it and drying it.
- the pretreatment step S2 is a step of performing a pretreatment on the base material layer (material to be the base material layer).
- pretreatment include plasma treatment in which the base material layer is treated with plasma such as oxygen plasma and atmospheric plasma, corona discharge treatment in which both sides of the base material layer are irradiated with corona discharge, acid treatment, alkali treatment, ultraviolet irradiation treatment, Itro treatment in which both sides of the substrate layer are exposed to combustion flames of combustion gas mixed with a coupling agent such as a silane coupling agent, for example, when the substrate layer contains a fluororesin, the substrate layer is immersed in an alkali metal solution.
- a coupling agent such as a silane coupling agent
- Examples include defluorination treatment for defluorination. It is preferable to ultrasonically clean the pretreated base material layer by immersing it in a cleaning solvent such as a silicon cleaner or an acid cleaner. In addition, especially when the substrate layer is thin, it is preferable not to perform blasting as
- the surface treatment agent application step S3 is a step of applying a surface treatment agent containing the compound ⁇ to both surfaces of the substrate layer (material to be the substrate layer). This application may be performed on the entire surface of the base material layer.
- a surface treatment agent containing compound ⁇ is usually a solution containing compound ⁇ and a solvent.
- Solvents include alcohols such as methanol, ethanol, isopropanol, ethylene glycol, propylene glycol, cellosolve, carbitol and 3-methoxy-3-methyl-1-butanol, ketones such as acetone, methyl ethyl ketone and cyclohexanone, benzene, toluene and xylene.
- aliphatic hydrocarbons such as hexane, octane, decane, dodecane, octadecane, esters such as ethyl acetate, methyl propionate, methyl phthalate, tetrahydrofuran (THF), ethyl butyl ether, anisole, propylene glycol monomethyl Ethers such as ether acetate (PGMEA), water, and the like can be used.
- the solvent illustrated as a solvent used for hydrolytic condensation can also be used. Among these, alcohol, ether and water are preferred. Solvents can be used singly or in combination of two or more.
- the concentration of compound ⁇ in the surface treatment agent (solution containing compound ⁇ ) is preferably 0.05% by mass or more and 5% by mass or less.
- the surface treatment agent may contain components other than the compound ⁇ and the solvent. Examples of other components include unreacted substances, side reaction products, surfactants, and the like when synthesizing compound ⁇ .
- the content of the compound ⁇ relative to the total solid content (all components other than the solvent) in the surface treatment agent is preferably 50% by mass or more, more preferably 70% by mass or more, and even more preferably 90% by mass or more.
- the content of the compound ⁇ with respect to the total solid content in the surface treatment agent may be 100% by mass.
- the surface treatment agent As a method for applying the surface treatment agent to both surfaces of the substrate layer, conventionally known coating methods such as an inkjet method, a gravure coating method, a kiss coating method, a die coating method, a lip coating method, a comma coating method, a blade coating method, a roll coating method, and a Examples include a coating method, a knife coating method, a spray coating method, a bar coating method, a spin coating method, a dip coating method, and the like.
- the lower limit of the thickness (wet thickness) of the coating film when the surface treatment agent is applied is, for example, preferably 100 nm, more preferably 1 ⁇ m, and even more preferably 3 ⁇ m.
- the upper limit of the thickness (wet thickness) of this coating film is preferably 200 ⁇ m, more preferably 100 ⁇ m.
- the immersion time in the dip coating method is preferably, for example, 3 seconds or more and 60 seconds or less.
- UV irradiation/heating process In the UV irradiation/heating step S4, at least one of ultraviolet irradiation and heating is applied to the compound ⁇ (surface treatment agent containing the compound ⁇ ) applied to both sides of the substrate layer (material to be the substrate layer). It is a process to do. It is preferable to irradiate ultraviolet rays including, for example, a wavelength range of 230 nm to 300 nm. Moreover, as a lower limit of heating temperature, 80 degreeC is preferable and 90 degreeC is more preferable, for example.
- the upper limit of the heating temperature is preferably 150°C, more preferably 120°C.
- the lower limit of the heating time is preferably 1 minute, more preferably 3 minutes. Also, the upper limit of the heating time is preferably 60 minutes, more preferably 30 minutes, and even more preferably 20 minutes or 10 minutes.
- the UV irradiation/heating step S4 it may be preferable to perform only heat treatment in terms of production efficiency.
- the UV irradiation/heating step 4 does not perform UV irradiation, and heats at a relatively short time and at a low temperature (for example, 100° C. for 10 minutes). Even with the treatment, good adhesion of the metal plating layer is exhibited by the compound ⁇ .
- a step of drying the applied surface treatment agent may be separately provided before the UV irradiation/heating step S4, or the applied surface treatment agent may be dried in the UV irradiation/heating step S4. good.
- the metal plating layer forming step S5 is a step of forming a metal plating layer by plating on both surfaces of the substrate layer (material to be the substrate layer) coated with the surface treatment agent and provided with the compound ⁇ .
- the metal plating method is not particularly limited, and conventional wet plating such as electroless plating and electrolytic plating can be used.
- a plating catalyst may be adhered to both surfaces of the substrate layer coated with the surface treatment agent before plating.
- plating copper by electroless plating it is preferable to use a plating solution containing copper sulfate, a reducing agent, and a solvent such as an aqueous medium or an organic solvent.
- a plating solution containing copper sulfate, sulfuric acid, and an aqueous medium it is preferable to use a plating solution containing copper sulfate, sulfuric acid, and an aqueous medium. Both electroless plating and electrolytic plating may be performed in this order.
- the base layer (conductive substrate) provided with the metal plating layer may be subjected to annealing treatment or the like. That is, the manufacturing method may further include a step of annealing after the step of forming the metal plating layer.
- the heating temperature in the annealing treatment is preferably 70° C. or higher and 150° C. or lower, for example.
- the heating time in the annealing treatment is preferably 10 minutes or more and 2 hours or less.
- the conductive substrate for a battery electrode of the present invention may further have layers other than the base material layer, the metal plating layer, and the layer containing the compound ⁇ .
- Example 1-1 A polyimide (PI) film (average thickness: 5.0 ⁇ m: Toray DuPont “Kapton 20EN”) was used as the base layer.
- the substrate layer was immersed in ethanol and subjected to ultrasonic cleaning for 5 minutes to perform degreasing cleaning, followed by air blow drying. Then, oxygen plasma treatment was performed as a pretreatment on this base material layer. The conditions were oxygen flow rate of 200 mL/min, treatment time of 10 minutes, and treatment output of 500 W. Then, this substrate layer was immersed in the surface treatment agent obtained in Synthesis Example 1 for about 20 seconds. After that, the substrate layer coated with the surface treatment agent was subjected to heat treatment at 100° C. for 10 minutes.
- a metal plating layer (copper plating layer) was formed by the following procedure.
- the substrate layer was immersed in the pre-dip solution for 1 minute and then in the catalyst solution at 55° C. for 3 minutes. After that, the substrate layer was washed with water, immersed in an accelerator liquid, and washed with water to attach a plating catalyst (Pd catalyst) to the surface of the substrate layer.
- the substrate layer was immersed in an electroless copper plating solution (“ARG Copper”, pH 12.5, Okuno Seiyaku Co., Ltd.) to form a copper plating layer (average thickness 1 ⁇ m). After that, an annealing treatment was performed at 100° C. for 1 hour to obtain a conductive substrate of Example 1-1.
- Examples 1-2 to 1-1 were prepared in the same manner as in Example 1-1 except that the type of base material layer used and the average thickness of the formed metal plating layer (copper plating layer) were as shown in Table 1. -8 of each conductive substrate was obtained.
- the surface roughness (Ra) of each substrate layer used in Examples 1-1 to 1-8 was within the range of 0.01 to 0.07 ⁇ m as a catalog value.
- Example 2-1 A conductive substrate of Example 2-1 was obtained in the same manner as in Example 1-1, except that a metal plating layer (copper plating layer) was provided as follows. The substrate layer with the plating catalyst adhered to the surface was immersed in an electroless copper plating solution to provide an electroless copper plating film (average thickness 0.1 ⁇ m). Next, the surface of the electroless copper plating film obtained above was placed on the cathode, the phosphorous copper was placed on the anode, and electroplating was performed using an electroplating solution containing copper sulfate.
- a metal plating layer copper plating layer
- a solution containing 70 g/liter of copper sulfate, 200 g/liter of sulfuric acid, 50 mg/liter of chloride ion, and 5 g/liter of Top Lucina SF (a brightener available from Okuno Chemical Industry Co., Ltd.) was used.
- a metal plating layer (copper plating layer) having a total average thickness of 3 ⁇ m including the electroless copper plating film was provided.
- Example 2-2 to 2-8 Conductive substrates of Examples 2-2 to 2-8 were obtained in the same manner as in Example 2-1, except that the types of substrate layers used were as shown in Table 2.
- the surface roughness (Ra) of each base material layer used in Examples 2-1 to 2-8 was within the range of 0.01 to 0.07 ⁇ m as a catalog value.
- Cross-cut test A cross-cut test was performed on each of the conductive substrates of Examples 2-1 to 2-8. The cross-cut test conformed to the cross-cut method described in JIS-K5600-5-6, was performed by cutting 5 ⁇ 5 squares with a width of 1 mm, and was evaluated according to the following criteria. Table 2 shows the evaluation results. A: No peeling of the metal plating layer occurred (100% adhesion). B: Part of the metal plating layer was peeled off (adhesion of 50% or more and less than 100%). C: Half or more of the metal plating layer was peeled off (less than 50% adhesion).
- Example 3-1 After the application of the surface treatment agent and subsequent heat treatment, the surface treatment agent was applied again and the subsequent heat treatment was performed.
- a conductive substrate of Example 3-1 was obtained in the same manner as in Example 2-1 except that a metal plating layer (copper plating layer) having an average thickness of 20 ⁇ m was provided. That is, in Example 3-1, the treatment with the surface treatment agent was performed twice.
- Examples 3-2 to 3-13, Comparative Examples 3-1 to 3-5 were prepared in the same manner as in Example 3-1 except that the type of base material layer used and the number of treatments with the surface treatment agent were as shown in Table 3. 3 to 5 of each conductive substrate were obtained.
- the surface roughness (Ra) of each base layer used in Examples 3-1 to 3-13 and Comparative Examples 3-1 to 3-5 is a catalog value of 0.01 to 0.07 ⁇ m. It was within range.
- Peel strength The peel strength of the metal plating layer was measured for each of the conductive substrates of Examples 3-1 to 3-13 and Comparative Examples 3-1 to 3-5.
- a force gauge ZTA-50N was attached to a vertical electric measuring stand MX2-500N (Imada Co., Ltd.) to configure a peel strength tester for 90° peeling.
- the peeling speed was 50 mm/min. Table 3 shows the measurement results.
- Example 4-1 A polyimide (PI) film (average thickness: 25.0 ⁇ m: Toray DuPont “Kapton 100EN”) was formed with a large number of circular through-holes with a diameter of 60 ⁇ m in a two-dimensional lattice.
- a conductive substrate of Example 4-1 was obtained in the same manner as in Example 2-1, except that the substrate layer having this two-dimensional porous structure was used.
- Example 4-2 A polytetrafluoroethylene (PTFE) film (average thickness: 50 ⁇ m) was formed with a large number of circular through-holes with a diameter of 60 ⁇ m in a two-dimensional lattice.
- PTFE polytetrafluoroethylene
- Example 5-1 A metal plating layer (copper plating layer) with an average thickness of 20 ⁇ m was formed on a COP sheet (average thickness of 0.1 mm) as a substrate layer, and adhesion was tested. First, as degreasing cleaning, a treatment with acetone was performed. Then, as a pretreatment, an oxygen plasma treatment (100 mL/min, 2 minutes, 200 W) was applied. Then, it was immersed in an ethanol solution of IMB-4K for 30 seconds as a surface treatment agent coating.
- the sample was irradiated with ultraviolet rays from a UV-LED irradiation device at an irradiation energy of 200 mJ/cm 2 and then heated at 125° C. for 15 minutes.
- the application of the surface treatment agent and the UV irradiation/heating were repeated twice.
- electroless plating and electrolytic plating were performed to form a copper plating layer with an average thickness of 20 ⁇ m.
- an annealing treatment was performed at 110° C. for 60 minutes.
- a conductive substrate of Example 5-1 was obtained.
- Examples 5-2 to 5-5 The type of compound ⁇ used in coating the surface treatment agent, and whether only heating is performed by UV irradiation and heating (represented by “H"), or whether to perform both ultraviolet irradiation and heating (represented by "UV+H”).
- Conductive substrates of Examples 5-2 to 5-5 were obtained in the same manner as in Example 5-1 except that the points were as shown in Table 4.
- peel strength peel strength of the metal plating layer (copper plating layer) was measured in the same manner as in Example 3-1. . Three samples were prepared for each sample and measured for each to obtain an average value of peel strength. Table 4 shows the measurement results.
- Example 6-1 and 6-2 Formation of metal plating layers using various compounds ⁇ on defluorinated PTFE films
- Defluorinated PTFE films (average thickness 180 ⁇ m: Nitto Denko "900UL") were used as base layers. was used. The substrate layer was immersed in ethanol and subjected to ultrasonic cleaning for 3 minutes to perform degreasing cleaning, followed by air blow drying. Then, it was immersed in an ethanol solution of compound ⁇ for 30 seconds.
- IMB-4K was used as compound ⁇ .
- Example 6-2 2,4-diazido-6-(3-triethoxysilylpropyl)amino-1,3,5-triazine (IMB-P) was used as compound ⁇ .
- the substrate layer coated with the surface treatment agent was subjected to heat treatment at 100° C. for 10 minutes.
- a metal plating layer (copper plating layer) was formed by the following procedure.
- the substrate layer was immersed in a pre-dip liquid and then in a catalyst liquid ("Cataposit 44" by Rohm & Haas Electronic Materials Co., Ltd.).
- the substrate layer was immersed in hydrochloric acid having a concentration of 1 v/v %, and then subjected to electroless plating to form an electroless copper plating film having an average thickness of 0.1 ⁇ m. After that, an annealing treatment was performed at 110° C. for 1 hour. After that, electrolytic plating was applied to form a copper plating layer having an average thickness of 20 ⁇ m together with the electroless copper plating film.
- conductive substrates of Examples 6-1 and 6-2 were obtained.
- Comparative Example 6-1 A conductive substrate of Comparative Example 6-1 was obtained in the same manner as in Example 6-1, except that the immersion in the ethanol solution of compound ⁇ and the subsequent heat treatment were not performed.
- peel strength peel strength of the metal plating layer (copper plating layer) was measured in the same manner as in Example 3-1. . Three samples were prepared for each sample, and each measurement was performed to obtain the maximum value and average value of peel strength. Table 5 shows the evaluation results.
- the adhesion between the substrate layer and the metal plating layer can be improved by using various compounds ⁇ , and the obtained conductive substrates are suitable as substrates for battery electrodes. I was able to confirm that.
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Abstract
Description
図1に示す本発明の一実施形態に係る電池電極用導電性基板(以下、単に「導電性基板」とも称する。)10は、基材層11と、基材層11の両面(表面側及び裏面側)にそれぞれ化合物αを介して積層される金属めっき層12a、12bとを備える積層体である。基材層11と各金属めっき層12a、12bとの間には、化合物αが介在し、この層間には、化合物αを含む中間層13a、13bが存在する。中間層13a、13bは、図1に示されるように、基材層11の表面又は裏面の全面に積層されていてよい。中間層13a、13bは、基材層11の側面にまで積層されていてもよい。中間層13a、13bは、連続的な層として存在していてもよく、断続的な層として存在していてもよい。中間層13a、13bは、通常、非常に薄い層であるため、光学顕微鏡等によって層であることが確認できなくてもよく、基材層11と金属めっき層12a、12bとの間に、化合物αが存在することが確認できればよい。中間層13a、13bは、化合物αに由来する層であってもよい。金属めっき層12a、12bも、化合物αを介して基材層11の側面にまで積層されていてよい。
基材層11は、その密度が、金属めっき層12a、12bの密度より低い。なお、基材層11及び金属めっき層12a、12bの密度はアルキメデス法により測定される値とすることができる。各層の密度は、各層が中空部分を有さない層(例えば、無孔質の層又は貫通孔が形成された多孔質の層)である場合、その層を形成する物質自体の密度(真密度)であってよい。
金属めっき層12a、12bは、めっき処理により形成された金属層である。金属めっき層12a、12bにおける金属の含有量の下限は、90質量%が好ましく、99質量%がより好ましい。金属めっき層12a、12bにおける金属の含有量の上限は、100質量%であってよい。
以下、基材層11と金属めっき層12a、12bとの間に介在する化合物αについて説明する。導電性基板10において、化合物αは、基材層11と金属めっき層12a、12bとの間を接合している。換言すれば、化合物αは、中間層13a、13bを形成している。中間層13a、13bには、化合物α以外の成分が含まれていてもよい。2つの中間層13a、13bにそれぞれ含まれる化合物αは、同一であってもよく、異なっていてもよい。化合物αは、1種又は2種以上を用いることができる。
下記式(1)又は(2)で表される化合物α1、及び
化合物α1を含む加水分解性シラン化合物を加水分解縮合して得られる化合物α2
が挙げられる。化合物αが、化合物α1及び化合物α2のうちの少なくとも一方である場合、比較的低温度及び短時間の加熱処理で且つ紫外線照射を行わなくても、良好な密着性が発現される。このためこれらの化合物を用いることで、効率的な処理が可能となる。
化合物α1は、下記式(1)又は(2)で表される化合物である。すなわち、化合物α1は、第1官能基としてベンゼン環に直接結合したアジド基等を有し、第2官能基としてシラノール基又はアルコキシシリル基を有する化合物αの一例である。
R1、R4、R5及びR6で表される炭素数1から12のアルコキシ基としては、上記したアルコキシ基等が挙げられる。
R2及びR7で表されるハロゲン原子としては、フッ素原子、塩素原子、臭素原子等が挙げられる。
R2及びR7で表される1価の有機基としては、1価の炭化水素基、アルコキシ基、-Y1-Z1-Si-R1 3(Y1、Z1及びR1は、式(1)中のY1、Z1及びR1とそれぞれ同義である。)で表される基、-COO-N-(-Z2-SiR4R5R6)2(Z2、R4、R5及びR6は、式(2)中のZ2、R4、R5及びR6とそれぞれ同義である。)、後述する式(14)で表される基等が挙げられる。
R3で表される炭素数1から6のアルキル基としては、メチル基、エチル基、プロピル基、ブチル基等が挙げられる。
R1としては、炭素数1から12のアルコキシ基が好ましく、炭素数1から6のアルコキシ基がより好ましく、炭素数1から3のアルコキシ基がさらに好ましい。
R2としては、水素原子が好ましい。
X1としては、アジド基及びアジドスルホニル基が好ましい。X1は、Y1等を含む基に対してパラ位又はメタ位に結合していることが好ましい。
Y1としては、アミド基が好ましく、*-CONH-(*は、ベンゼン環との結合部位を示す。)で表されるアミド基がより好ましい。
Z1としては、炭素数2から12のアルカンジイル基(アルキレン基)が好ましく、炭素数2から6のアルカンジイル基(アルキレン基)がより好ましい。
mは、3が好ましい。
R4、R5及びR6としては、炭素数1から12のアルコキシ基が好ましく、炭素数1から6のアルコキシ基がより好ましく、炭素数1から3のアルコキシ基がさらに好ましい。
R7としては、水素原子が好ましい。
X2としては、アジド基及びアジドスルホニル基が好ましい。X2は、-COO-N-(-Z2-SiR4R5R6)2で表される基に対してパラ位又はメタ位に結合していることが好ましい。
Z2としては、炭素数2から12のアルカンジイル基(アルキレン基)が好ましく、炭素数2から6のアルカンジイル基(アルキレン基)がより好ましい。
化合物α1の合成方法は特に限定されないが、例えば、アルコキシシリル基と、アルコキシシリル基以外の反応性基aとを有するシランカップリング剤Aと、上記反応性基aと結合反応可能な反応性基bと、ベンゼン環と、アジド基、アジドスルホニル基及びジアゾメチル基からなる群より選ばれる少なくとも1種の基とを有する化合物Bとを公知の方法により反応させることにより得ることができる。反応性基aと反応性基bとの組み合わせとしては、イソシアネート基、エポキシ基、アミノ基等と、カルボキシ基との組み合わせなどが挙げられる。
化合物α2においては、通常、未反応のアルコキシシリル基が残存している。すなわち、化合物α2も、第1官能基としてベンゼン環に直接結合したアジド基等を有し、第2官能基としてシラノール基又はアルコキシシリル基を有する化合物αの一例である。
化合物α2は、(i)化合物α1を含む加水分解性シラン化合物を加水分解縮合して得る方法、(ii)加水分解性シラン化合物の加水分解縮合物であって、構造単位Bを有する化合物に対して、「アミノ基と結合反応可能な反応性基と、ベンゼン環と、アジド基、アジドスルホニル基及びジアゾメチル基からなる群より選ばれる少なくとも1種の基とを有する化合物X」(アジド安息香酸、アジドスルホニル安息香酸、ジアゾメチル安息香酸等)を反応させて得る方法などが挙げられる。上記(ii)においては、構造単位B中のアミノ基が化合物Xと反応することにより、構造単位Aが形成される。
下記式(5)で表される化合物α3、及び
化合物α3を含む加水分解性シラン化合物を加水分解縮合して得られる化合物α4
が挙げられる。
化合物α3は、下記式(5)で表される化合物である。
化合物α4は、化合物α3を含む加水分解性シラン化合物を加水分解縮合して得られる化合物である。化合物α4は、化合物α1に替えて化合物α3が用いられていること以外は化合物α2と同様の加水分解縮合物である。
導電性基板10は、電池の電極(正極又は負極)に用いられる。電池は、一次電池、二次電池、燃料電池等の化学電池であってよい。導電性基板10は、金属めっき層の密着性が高く耐久性に優れるため、充放電を繰り返し長期間使用される二次電池の電極用の基板として特に好適である。
本発明の一実施形態に係る電池電極用導電性基板(導電性基板)の製造方法は、
基材層の両面に化合物αを含む表面処理剤を塗布する工程(表面処理剤塗布工程)、及び
表面処理剤が塗布された基材層の両面に、めっき処理により金属めっき層を形成する工程(金属めっき層形成工程)
を備える。
脱脂洗浄工程S1は、例えば、溶剤等を用いて基材層(基材層となる材料)を洗浄する工程である。例えば、基材層をアセトン、エタノール等の溶剤に浸漬して超音波洗浄し、乾燥させることにより行うことができる。
前処理工程S2は、基材層(基材層となる材料)に対して前処理を行う工程である。前処理としては、基材層に対して酸素プラズマ、大気プラズマ等のプラズマで処理するプラズマ処理、基材層の両面にコロナ放電照射を行うコロナ放電処理、酸処理、アルカリ処理、紫外線照射処理、基材層の両面をシランカップリング剤等のカップリング剤を混入した燃焼ガスの燃焼炎にさらすイトロ処理、例えば基材層がフッ素樹脂を含む場合の基材層をアルカリ金属溶液に浸漬して脱フッ素化を行う脱フッ素化処理等が挙げられる。各前処理を施した基材層に対して、シリコンクリーナ、酸クリーナ等の洗浄溶剤に浸漬して超音波洗浄することが好ましい。なお、特に基材層が薄い場合などは、前処理としてブラスト処理を行わないことが好ましい。
表面処理剤塗布工程S3は、基材層(基材層となる材料)の両面に、化合物αを含む表面処理剤を塗布する工程である。この塗布は、基材層の全面に対して行ってもよい。
UV照射・加熱工程S4は、基材層(基材層となる材料)の両面に塗布された化合物α(化合物αを含む表面処理剤)に対して、紫外線照射及び加熱の少なくとも一方の処理を行う工程である。この紫外線照射は、例えば230nm以上300nmの波長領域を含む紫外線を照射することが好ましい。また、加熱温度の下限としては、例えば80℃が好ましく、90℃がより好ましい。加熱温度の上限としては、150℃が好ましく、120℃がより好ましい。加熱時間の下限としては、1分が好ましく、3分がより好ましい。また、加熱時間の上限としては、60分が好ましく、30分がより好ましく、20分又は10分がさらに好ましい。
金属めっき層形成工程S5は、表面処理剤が塗布され、化合物αが設けられた基材層(基材層となる材料)の両面に、めっき処理により金属めっき層を形成する工程である。
本発明は、上記した実施形態に限定されるものではなく、本発明の要旨を変更しない範囲において実施される各種の変形例も含むものとして理解されるべきである。
3-アジド安息香酸クロリド(N3C6H4COCl)をTHF(テトラヒドロフラン)に溶かした。窒素ガスの雰囲気下、3-アミノプロピルトリエトキシシランの加水分解縮合物である原料オリゴマー(米国Gelest)とTEA(トリエチルアミン)とをTHFに溶かし、撹拌しながら室温で滴下した。反応を完結させるためさらに撹拌を続けた。反応終了後、THFを含む溶液を留去し、得られた粗生成物を精製して目的物を得た。この目的物が、式(19)で表されるシルセスキオキサン化合物(IMB-4KP)であった。スペクトルから、生成物においては、式(19)におけるlとmとnとの比が、l:m:n=1:1:0であることを確認した。得られた化合物(IMB-4KP)を、濃度が2.5質量%となるようにイソプロパノールに溶解し、表面処理剤を得た。
基材層として、ポリイミド(PI)フィルム(平均厚さ5.0μm:東レ・デュポン「カプトン20EN」)を用いた。基材層をエタノールに浸漬して、5分間の超音波洗浄をすることで、脱脂洗浄を行い、その後エアブロー乾燥を行った。
次いで、この基材層に対して、前処理として、酸素プラズマ処理を行った。条件は、酸素流量200mL/分、処理時間10分、処理出力500Wとした。
次いで、この基材層を合成例1で得られた表面処理剤に約20秒浸漬させた。その後、表面処理剤が塗布された基材層に対して、100℃で10分間の加熱処理を行った。
次いで、以下の手順で金属めっき層(銅めっき層)を形成した。基材層をプレディップ液に1分浸漬させ、次いで、55℃のキャタリスト液に3分浸漬させた。その後、基材層の水洗、アクセラレータ液への浸漬及び水洗を行い、めっき触媒(Pd触媒)を基材層の表面に付着させた。
次いで、基材層を、無電解銅めっき液(奥野製薬(株)「ARGカッパー」、pH12.5)に浸漬し、銅めっき層(平均厚さ1μm)を設けた。
その後、100℃1時間のアニール処理を行い、実施例1-1の導電性基板を得た。
用いた基材層の種類及び形成した金属めっき層(銅めっき層)の平均厚さを表1に示す通りとしたこと以外は実施例1-1と同様にして、実施例1-2~1-8の各導電性基板を得た。
実施例1-1~1-8の各導電性基板についで、金属めっき層の外観を以下の基準で評価した。評価結果を表1に示す。
A:金属めっき層の剥離は全く生じなかった。
B:金属めっき層の端部のめくれが生じた。
C:金属めっき層が全面剥離した。
金属めっき層(銅めっき層)を以下の通り設けたこと以外は実施例1-1と同様にして、実施例2-1の導電性基板を得た。
めっき触媒を表面に付着させた基材層を、無電解銅めっき液に浸漬し、無電解銅めっき膜(平均厚さ0.1μm)を設けた。次いで、上記で得られた無電解銅めっき膜の表面をカソードに設置し、含リン銅をアノードに設置し、硫酸銅を含む電気めっき液を用いて電解めっきを行った。電気めっき液としては、硫酸銅70g/リットル、硫酸200g/リットル、塩素イオン50mg/リットル、トップルチナSF(奥野製薬工業(株)の光沢剤)5g/リットルの溶液を用いた。これにより、無電解銅めっき膜を含めた合計の平均厚さが3μmの金属めっき層(銅めっき層)を設けた。
用いた基材層の種類を表2に示す通りとしたこと以外は実施例2-1と同様にして、実施例2-2~2-8の各導電性基板を得た。
実施例2-1~2-8の各導電性基板についで、クロスカット試験を行った。クロスカット試験は、JIS-K5600-5-6に記載のクロスカット法に準拠し、1mm幅、5×5マスでカットを入れて行い、以下の基準で評価した。評価結果を表2に示す。
A:金属めっき層の剥離は全く生じなかった(100%密着)。
B:金属めっき層の一部が剥がれた(50%以上100%未満の密着)。
C:金属めっき層の半分以上が剥がれた(50%未満の密着)。
表面処理剤の塗布及びその後の加熱処理を行った後、再度表面処理剤の塗布及びその後の加熱処理を行ったこと、及び電解めっきの処理時間を調整して無電解銅めっき膜を含めた合計の平均厚さが20μmの金属めっき層(銅めっき層)を設けたこと以外は実施例2-1と同様にして、実施例3-1の導電性基板を得た。すなわち、実施例3-1においては、表面処理剤の処理を2回実施した。
用いた基材層の種類及び表面処理剤の処理回数を表3に示す通りとしたこと以外は実施例3-1と同様にして、実施例3-2~3-13及び比較例3-1~3-5の各導電性基板を得た。
実施例3-1~3-13及び比較例3-1~3-5の各導電性基板について、金属めっき層の剥離強度を測定した。縦型電動計測スタンドMX2-500N((株)イマダ)にフォースゲージZTA-50Nを取り付け、90°剥離のピール強度試験機を構成した。剥離速度は50mm/分とした。測定結果を表3に示す。
ポリイミド(PI)フィルム(平均厚さ25.0μm:東レ・デュポン「カプトン100EN」)に、直径60μmの多数の円形貫通孔を二次元格子状に形成した。この二次元多孔質構造を有する基材層を用いたこと以外は実施例2-1と同様にして、実施例4-1の導電性基板を得た。
ポリテトラフルオロエチレン(PTFE)フィルム(平均厚さ50μm)に、直径60μmの多数の円形貫通孔を二次元格子状に形成した。この二次元多孔質構造を有する基材層を用いたこと、及び前処理として、脱フッ化処理(Naナフタレン錯体溶液に5秒浸漬)を行ったこと以外は実施例2-1と同様にして、実施例4-2の導電性基板を得た。
実施例4-1~4-2の各導電性基板について、金属めっき層の剥離は全く生じておらず、金属めっき層が良好に密着していることを確認した。また、各導電性基板について、表面と裏面との間の抵抗値をテスターにより測定したところ、いずれも良好な導通が確認できた。
IR、NMR及びQCMSの各分析から、生成物が、N-(3-トリエトキシシリルプロピル)-4-アジドベンズアミドであることを確認した。
基材層としてのCOPシート(平均厚さ0.1mm)について、平均厚さ20μmの金属めっき層(銅めっき層)を形成し、密着性を試験した。まず、脱脂洗浄として、アセトンによる処理を行った。次いで、前処理として、酸素プラズマ処理(100mL/分、2分、200W)を施した。次いで、表面処理剤塗布として、IMB-4Kのエタノール溶液に30秒間浸漬した。次いで、UV照射・加熱として、試料にUV-LED照射器から被照射エネルギー200mJ/cm2で紫外線を照射し、次いで、125℃で15分の加熱を行った。表面処理剤塗布とUV照射・加熱とは、2回反復して行った。その後、無電解めっき及び電解めっきを行い、平均厚さ20μmの銅めっき層を形成した。めっき後においては、110℃で60分のアニール処理を行った。以上により、実施例5-1の導電性基板を得た。
表面処理剤塗布で用いる化合物αの種類、及びUV照射・加熱で加熱のみを行うのか(「H」と表す)、又は紫外線照射と加熱との両方を行うのか(「UV+H」と表す)、という点を表4に記載の通りとしたこと以外は実施例5-1と同様にして、実施例5-2~5-5の各導電性基板を得た。
実施例5-1~5-5の各導電性基板について、金属めっき層(銅めっき層)のピール強度(剥離強度)を実施例3-1等と同様の方法で測定した。各試料について3つのサンプルを作製してそれぞれについて計測を行い、ピール強度の平均値を求めた。測定結果を表4に示す。
基材層として、脱フッ素化PTFEフィルム(平均厚さ180μm:日東電工「900UL」)を用いた。基材層をエタノールに浸漬して、3分間の超音波洗浄をすることで、脱脂洗浄を行い、その後エアブロー乾燥を行った。
次いで、化合物αのエタノール溶液に30秒間浸漬させた。実施例6-1においては、化合物αとして、IMB-4Kを用いた。実施例6-2においては、化合物αとして、2,4-ジアジド-6-(3-トリエトキシシリルプロピル)アミノ-1,3,5-トリアジン(IMB-P)を用いた。その後、表面処理剤が塗布された基材層に対して、100℃で10分間の加熱処理を行った。
次いで、以下の手順で金属めっき層(銅めっき層)を形成した。基材層をプレディップ液に浸漬させ、次いで、キャタリスト液(ローム&ハース電子材料株式会社「キャタポジット44」)に浸漬させた。次いで、基材層を1v/v%濃度の塩酸に浸漬させた後、無電解めっきを施し、平均厚さ0.1μmの無電解銅めっき膜を設けた。その後、110℃1時間のアニール処理を施した。その後、電解めっきを施し、無電解銅めっき膜とあわせて平均厚さ20μmの銅めっき層を形成した。以上により、実施例6-1及び6-2の各導電性基板を得た。
化合物αのエタノール溶液への浸漬及びその後の加熱処理を行わなかったこと以外は実施例6-1と同様にして、比較例6-1の導電性基板を得た。
実施例6-1、6-2の各導電性基板においては、金属めっき層(銅めっき層)の剥離も膨れも無く良好であった。比較例6-1の導電性基板においては、部分的に金属めっき層が剥離する部分があり、不良であった。
実施例6-1~6-2の各導電性基板について、金属めっき層(銅めっき層)のピール強度(剥離強度)を実施例3-1等と同様の方法で測定した。各試料について3つのサンプルを作製して各々計測を行い、ピール強度の最大値及び平均値を求めた。評価結果を表5に示す。
11 基材層
12a、12b 金属めっき層
13a、13b 中間層
Claims (13)
- 基材層と、
上記基材層の両面に化合物αを介して積層される金属めっき層と
を備え、
上記基材層の密度が、上記金属めっき層の密度より低く、
上記化合物αが、上記基材層と反応して結合することが可能な第1官能基と、上記金属めっき層と反応して結合することが可能な第2官能基とを有する、電池電極用導電性基板。 - 上記基材層の平均厚さが3μm以上50μm以下である、請求項1に記載の電池電極用導電性基板。
- 上記基材層の平均厚さが3μm以上10μm以下である、請求項1又は請求項2に記載の電池電極用導電性基板。
- 上記基材層の表面粗さ(Ra)が1μm以下である、請求項1又は請求項2に記載の電池電極用導電性基板。
- 上記基材層が、厚さ方向に貫通する複数の孔が形成された二次元多孔質構造を有する、請求項1又は請求項2に記載の電池電極用導電性基板。
- 上記金属めっき層の各層の平均厚さが0.5μm以上20μm以下である、請求項1又は請求項2に記載の電池電極用導電性基板。
- 上記化合物αが芳香環を有し、
上記第1官能基が、上記芳香環に直接結合したアジド基、アジドスルホニル基又はジアゾメチル基である、請求項1又は請求項2に記載の電池電極用導電性基板。 - 上記芳香環がベンゼン環である、請求項7に記載の電池電極用導電性基板。
- 上記第2官能基が、シラノール基又はアルコキシシリル基である、請求項1又は請求項2に記載の電池電極用導電性基板。
- 上記化合物αが、
下記式(1)又は(2)で表される化合物α1、及び
上記化合物α1を含む加水分解性シラン化合物を加水分解縮合して得られる化合物α2
の少なくとも一方である、請求項1又は請求項2に記載の電池電極用導電性基板。
上記式(2)中、複数のR4、R5及びR6は、それぞれ独立して、水素原子、炭素数1から12のアルキル基、フェニル基、炭素数1から12のアルコキシ基、又はヒドロキシ基であり、複数のR4、R5及びR6のうちの少なくとも1つは、炭素数1から12のアルコキシ基である。複数のR7は、それぞれ独立して、水素原子、ハロゲン原子、又は1価の有機基である。X2は、アジド基、アジドスルホニル基、又はジアゾメチル基である。複数のZ2は、それぞれ独立して、単結合、炭素数1から12のアルカンジイル基、又は炭素数1から12のアルカンジイル基の末端若しくは炭素-炭素結合間に-NH-、-O-、-S-及び-S(O)-のうちの1つ以上の基を含む基である。
- 上記基材層を構成する物質が、樹脂、セラミック、ガラス繊維、紙、又はこれらの1種若しくは2種以上を含む複合材料である、請求項1又は請求項2に記載の電池電極用導電性基板。
- 基材層の両面に化合物αを含む表面処理剤を塗布する工程、及び
上記表面処理剤が塗布された基材層の両面に、めっき処理により金属めっき層を形成する工程
を備え、
上記基材層の密度が、上記金属めっき層の密度より低く、
上記化合物αが、上記基材層と反応して結合することが可能な第1官能基と、上記金属めっき層と反応して結合することが可能な第2官能基とを有する、電池電極用導電性基板の製造方法。 - 上記表面処理剤を塗布する工程の後に、上記化合物αに対する紫外線照射及び加熱の少なくとも一方の処理を行う工程をさらに備える、請求項12に記載の電池電極用導電性基板の製造方法。
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JP2022048068A (ja) * | 2020-09-13 | 2022-03-25 | 豊光社テクノロジーズ株式会社 | 表面処理方法、表面処理剤、結合体の製造方法、導体被覆を有する物質の製造方法、塗膜が形成された物質の製造方法、及び化合物 |
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US20110306722A1 (en) * | 2010-06-08 | 2011-12-15 | Bar-Ilan University | Surface-modified polymer films |
JP4936344B1 (ja) * | 2010-10-04 | 2012-05-23 | 邦夫 森 | 金属膜形成方法、及び金属膜を有する製品 |
JP2019102429A (ja) * | 2017-12-05 | 2019-06-24 | 寧徳時代新能源科技股▲分▼有限公司Contemporary Amperex Technology Co., Limited | 集電体、その極シート及び電気化学デバイス |
JP2022048068A (ja) * | 2020-09-13 | 2022-03-25 | 豊光社テクノロジーズ株式会社 | 表面処理方法、表面処理剤、結合体の製造方法、導体被覆を有する物質の製造方法、塗膜が形成された物質の製造方法、及び化合物 |
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