WO2022176697A1 - 積層板及び発熱体の製造方法並びにデフロスタ - Google Patents
積層板及び発熱体の製造方法並びにデフロスタ Download PDFInfo
- Publication number
- WO2022176697A1 WO2022176697A1 PCT/JP2022/004841 JP2022004841W WO2022176697A1 WO 2022176697 A1 WO2022176697 A1 WO 2022176697A1 JP 2022004841 W JP2022004841 W JP 2022004841W WO 2022176697 A1 WO2022176697 A1 WO 2022176697A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- copper foil
- less
- resin film
- polyvinyl acetal
- treated surface
- Prior art date
Links
- 238000000034 method Methods 0.000 title claims abstract description 42
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 13
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 108
- 239000011889 copper foil Substances 0.000 claims abstract description 102
- 229920005989 resin Polymers 0.000 claims abstract description 55
- 239000011347 resin Substances 0.000 claims abstract description 55
- DHKHKXVYLBGOIT-UHFFFAOYSA-N 1,1-Diethoxyethane Chemical compound CCOC(C)OCC DHKHKXVYLBGOIT-UHFFFAOYSA-N 0.000 claims abstract description 37
- 239000011354 acetal resin Substances 0.000 claims abstract description 37
- 229920006324 polyoxymethylene Polymers 0.000 claims abstract description 37
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 37
- 238000010438 heat treatment Methods 0.000 claims description 44
- 238000012545 processing Methods 0.000 claims description 8
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims description 6
- 238000007788 roughening Methods 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 2
- 238000005304 joining Methods 0.000 abstract description 5
- 230000009257 reactivity Effects 0.000 abstract description 4
- 239000011521 glass Substances 0.000 description 9
- 238000005530 etching Methods 0.000 description 7
- 239000000654 additive Substances 0.000 description 6
- 229910052802 copper Inorganic materials 0.000 description 6
- 239000010949 copper Substances 0.000 description 6
- 239000005357 flat glass Substances 0.000 description 5
- 238000005259 measurement Methods 0.000 description 5
- 238000004381 surface treatment Methods 0.000 description 5
- 238000011282 treatment Methods 0.000 description 5
- 238000001125 extrusion Methods 0.000 description 3
- 238000003475 lamination Methods 0.000 description 3
- 238000002834 transmittance Methods 0.000 description 3
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 3
- 238000000576 coating method Methods 0.000 description 2
- 239000000155 melt Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 230000035515 penetration Effects 0.000 description 2
- 239000004014 plasticizer Substances 0.000 description 2
- 238000007747 plating Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 229920005992 thermoplastic resin Polymers 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- 239000010937 tungsten Substances 0.000 description 2
- MSYQXPANIUQLKY-UHFFFAOYSA-N 2,2-dihexylhexanedioic acid Chemical compound CCCCCCC(C(O)=O)(CCCC(O)=O)CCCCCC MSYQXPANIUQLKY-UHFFFAOYSA-N 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 238000010952 in-situ formation Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000005340 laminated glass Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000011342 resin composition Substances 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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
- B32B15/20—Layered products comprising a layer of metal comprising aluminium or copper
-
- 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
- B32B15/082—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 comprising vinyl resins; comprising acrylic resins
-
- 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
- B32B27/30—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/06—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the heating method
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/10—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the pressing technique, e.g. using action of vacuum or fluid pressure
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/10—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor
- H05B3/12—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/20—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater
- H05B3/34—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater flexible, e.g. heating nets or webs
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/84—Heating arrangements specially adapted for transparent or reflecting areas, e.g. for demisting or de-icing windows, mirrors or vehicle windshields
-
- 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
- B32B2250/00—Layers arrangement
- B32B2250/02—2 layers
-
- 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
- B32B2307/50—Properties of the layers or laminate having particular mechanical properties
- B32B2307/538—Roughness
-
- 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
- B32B2307/737—Dimensions, e.g. volume or area
- B32B2307/7375—Linear, e.g. length, distance or width
- B32B2307/7376—Thickness
-
- 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
- B32B2311/00—Metals, their alloys or their compounds
- B32B2311/12—Copper
-
- 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
- B32B2329/00—Polyvinylalcohols, polyvinylethers, polyvinylaldehydes, polyvinylketones or polyvinylketals
- B32B2329/06—PVB, i.e. polyinylbutyral
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B2203/00—Aspects relating to Ohmic resistive heating covered by group H05B3/00
- H05B2203/017—Manufacturing methods or apparatus for heaters
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B2214/00—Aspects relating to resistive heating, induction heating and heating using microwaves, covered by groups H05B3/00, H05B6/00
- H05B2214/02—Heaters specially designed for de-icing or protection against icing
-
- 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
- Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
- Y02B30/00—Energy efficient heating, ventilation or air conditioning [HVAC]
Definitions
- the present invention relates to a laminated plate, a method for manufacturing a heating element, and a defroster.
- a defroster is widely used as a device for preventing or removing frost, icing, fogging, etc. on window glass in vehicles such as automobiles.
- the defroster for example, by blowing warm air containing no water vapor intensively to a portion to be dehumidified, fogging is removed and visibility is ensured.
- defrosters that use heating wires (electric heating wires) for the purpose of improving heating efficiency and saving power in electric vehicles.
- heating wires electric heating wires
- fogging can be removed by heating the glass with a heating wire interposed between the glass plates, for example.
- Patent Document 1 Japanese Patent Application Laid-Open No. 2018-35036 describes a vehicle glass device comprising a pair of glass substrates and a transparent resin intermediate film and a heating electrode sheet interposed between the glass substrates. The use of polyvinyl butyral resin as the membrane is disclosed.
- tungsten wires are generally used as heating wires for defrosters.
- the tungsten wire has a large wire diameter of about 30 ⁇ m, and it is difficult to thin the wire, resulting in poor visibility.
- Patent Document 2 Japanese Patent Application Laid-Open No. 2018-161889 describes a polyvinyl acetal resin having a polyvinyl acetal resin layer and a conductive structure based on a metal foil disposed on or inside the polyvinyl acetal resin layer. Concerning the film, it is disclosed that the conductive structure is composed of copper or the like. Further, in Patent Document 3 (Japanese Patent Application Laid-Open No.
- a polyvinyl acetal resin film in which a copper foil is bonded is obtained by thermocompression bonding a laminate obtained by stacking a polyvinyl acetal resin film and a copper foil. Later, it is disclosed that a copper foil bonded to a resin film is processed to form a conductive layer. Furthermore, in Patent Document 4 (International Publication No. 2017/090386), in a laminate having a resin layer containing polyvinyl acetal resin and a copper layer, a method such as a subtractive method, a semi-additive method, a modified semi-additive method, etc. It is disclosed that a wiring pattern is formed by processing the layers.
- polyvinyl acetal resin is a thermoplastic resin, and lamination of copper foil and resin film can be performed in a short time (for example, several tens of seconds or less) at low temperature and low pressure (for example, 180° C. or less and 0.6 MPa or less). need to do. For this reason, the polyvinyl acetal resin has low reactivity with the copper foil, and it is difficult to ensure the adhesion between the copper foil and the resin film.
- the present inventors have recently joined or formed a polyvinyl acetal resin film on a copper foil having a treated surface in which the interfacial developed area ratio Sdr and the root mean square height Sq defined in ISO 25178 are controlled within predetermined ranges.
- the inventors have found that a laminate having excellent adhesion between the copper foil and the resin film can be produced by doing so.
- an object of the present invention is to produce a laminate having excellent adhesion between the copper foil and the resin film while using a polyvinyl acetal resin with low reactivity with the copper foil.
- a copper foil having, on at least one side, a treated surface having an interfacial developed area ratio Sdr of 0.50% or more and 9.00% or less and a root mean square height Sq of 0.010 ⁇ m or more and 0.200 ⁇ m or less a step of preparing bonding or forming a polyvinyl acetal resin film on the treated surface of the copper foil to form a laminate; wherein the Sdr and Sq are values measured under the conditions of an S filter cutoff wavelength of 0.55 ⁇ m and an L filter cutoff wavelength of 10 ⁇ m in accordance with ISO 25178. .
- a heating element by bonding or forming an additional polyvinyl acetal resin film to the laminate on which the heating wire is formed, so as to sandwich the heating wire;
- a defroster comprising a heating element manufactured by the above method.
- the term “developed area ratio Sdr of the interface” or “Sdr” refers to how much the developed area (surface area) of the defined region increases with respect to the area of the defined region, which is measured in accordance with ISO25178. It is a parameter that indicates whether or not In this specification, the developed area ratio Sdr of the interface is expressed as an increase (%) of the surface area. The smaller this value, the more nearly flat the surface shape is, and the Sdr of a completely flat surface is 0%. On the other hand, the larger this value, the more uneven the surface shape. For example, if a surface has an Sdr of 4.00%, it indicates a 4.00% increase in surface area from a perfectly flat surface.
- the "root mean square height Sq" or “Sq” is a parameter that corresponds to the standard deviation of the distance from the average plane, measured according to ISO25178.
- the root-mean-square height Sq is a concept close to the average roughness, but it is easy to handle statistically and is not easily affected by disturbances such as dust, scratches, and noise existing on the measurement surface, so it is stable. You can get results.
- mountain peak density Spd or “Spd” is a parameter representing the number of peak points per unit area, measured according to ISO25178.
- the peak vertex density Spd can be obtained by counting only the peak points larger than 5% of the maximum amplitude on the contour curved surface and dividing the number of peaks included in the contour curved surface by the projected area of the contour curved surface. A large value suggests a large number of contact points with other objects.
- the developed area ratio Sdr of the interface, the root-mean-square height Sq, and the peak density Spd are obtained by measuring the surface profile of a predetermined measurement area (for example, a two-dimensional area of 16384 ⁇ m 2 ) on the treated surface with a commercially available laser microscope. Each can be calculated.
- the numerical values of the developed area ratio Sdr and the root-mean-square height Sq of the interface are values measured under the conditions of a cutoff wavelength of 0.55 ⁇ m by the S filter and a cutoff wavelength of 10 ⁇ m by the L filter.
- the value of the peak density Spd is a value measured under the condition that the cutoff wavelength by the S filter is 2 ⁇ m and the cutoff by the L filter is not performed.
- the present invention relates to a method of manufacturing a laminate.
- the method of the present invention includes the steps of (1) preparing a copper foil having a predetermined treated surface on at least one side; a step of bonding or forming a
- the treated surface of the copper foil has an interface developed area ratio Sdr of 0.50% or more and 9.00% or less and a root mean square height Sq of 0.010 ⁇ m or more and 0.200 ⁇ m or less.
- copper foil and prepreg composite material in which the base material is impregnated with a thermosetting resin
- high temperature and high pressure for example, 220 ° C. and 4 MPa
- a long time for example, 90 minutes
- the adhesion between the copper foil and the resin film can be improved by using a copper foil having a treated surface that is controlled to have fine irregularities.
- polyvinyl acetal resin is a thermoplastic resin with high light transmittance used as a glass intermediate film, and lamination with copper foil is performed at low temperature and low pressure (e.g., 180 ° C. or less and 0 .6 MPa or less) for a short period of time (for example, several tens of seconds or less).
- low temperature and low pressure e.g. 180 ° C. or less and 0 .6 MPa or less
- the polyvinyl acetal resin has low reactivity with the copper foil, making it difficult to ensure the adhesion between the copper foil and the polyvinyl acetal resin film.
- the copper foil used in the method of the present invention has a treated surface on at least one side.
- This treated surface has an interface developed area ratio Sdr of 0.50% or more and 9.00% or less, preferably 2.50% or more and 9.00% or less, more preferably 5.00% or more and 9.00%. It is below. Within such a range, the surface area of the treated surface that contributes to adhesion to the resin film can be increased while the treated surface has small bumps suitable for the penetration of the polyvinyl acetal resin. - The adhesion between resin films can be improved.
- the treated surface of the copper foil has a root mean square height Sq of 0.010 ⁇ m or more and 0.200 ⁇ m or less, preferably 0.050 ⁇ m or more and 0.180 ⁇ m or less, more preferably 0.100 ⁇ m or more and 0.140 ⁇ m or less. Within such a range, the treated surface of the copper foil has small bumps suitable for permeation of the polyvinyl acetal resin, and the adhesion between the copper foil and the resin film can be improved.
- the treated surface of the copper foil preferably has a vertex density Spd of 100 mm ⁇ 2 or more and 26000 mm ⁇ 2 or less, more preferably 10000 mm ⁇ 2 or more and 20000 mm ⁇ 2 or less, still more preferably 10000 mm ⁇ 2 or more and 15000 mm ⁇ 2 or less. is. Within such a range, the polyvinyl acetal resin can more easily penetrate the copper foil surface, and the contact points between the copper foil and the resin film can be increased, so the adhesion between the copper foil and the resin film It is possible to further improve the property.
- the treated surface having the above surface parameters can be formed by subjecting the copper foil surface to surface treatment under known or desired conditions.
- a commercially available copper foil having a treated surface that satisfies the above conditions may be selectively obtained.
- Various surface treatments are performed to improve or impart certain properties (e.g., rust resistance, moisture resistance, chemical resistance, acid resistance, heat resistance, and adhesion to resin films) on the surface of copper foil.
- the surface treatment applied to the copper foil include antirust treatment, silane treatment, roughening treatment, and the like.
- the treated surface of the copper foil preferably has a plurality of roughening particles.
- the surface treatment preferably includes roughening treatment.
- Surface treatment may be performed on at least one side of the copper foil, or may be performed on both sides of the copper foil.
- the copper foil may have a treated surface (eg, a roughened surface) on both sides, or may have a treated surface on only one side.
- the thickness of the copper foil is not particularly limited, it is preferably 0.1 ⁇ m or more and 35 ⁇ m or less, more preferably 0.3 ⁇ m or more and 18 ⁇ m or less, and still more preferably 1.0 ⁇ m or more and 12 ⁇ m or less.
- the copper foil may be prepared in the form of a copper foil with a carrier in order to improve handleability.
- a carrier-attached copper foil typically comprises a carrier, a release layer provided on the carrier, and a copper foil provided on the release layer with the treated surface facing outward.
- the carrier-attached copper foil can employ a known layer structure.
- a laminate is formed by joining or forming a polyvinyl acetal resin film on the treated surface of the copper foil prepared in (1) above.
- Bonding of the resin film to the copper foil is preferably carried out by thermocompression bonding or adhesion of a resin film prepared in advance to the copper foil.
- the bonding of the resin film to the copper foil is performed by thermocompression bonding the resin film and the copper foil at a temperature of 180° C. or less and a pressure of 0.6 MPa or less, more preferably 100° C. or more and 150° C. or less. It is carried out at a temperature and a pressure of 0.2 MPa or more and 0.6 MPa or less.
- thermocompression bonding is preferably performed for 60 seconds or less, more preferably 10 seconds or more and 30 seconds or less. As described above, according to the method of the present invention, even under such lamination conditions of low temperature and low pressure, a laminate having excellent adhesion between the copper foil and the resin film can be produced.
- the formation of the resin film on the copper foil is carried out by coating or applying the resin composition constituting the resin film to the copper foil using a known method such as a melt extrusion method, a casting method, a coating method, or the like. is preferred.
- a resin film can be directly formed on the copper foil (in situ formation).
- the resin temperature during extrusion is preferably 250° C. or less from the viewpoint of efficiently removing volatile substances in the resin film. ° C. or higher and 230 ° C. or lower.
- the thickness of the resin film is not particularly limited, it is preferably 1 ⁇ m or more and 1000 ⁇ m or less, more preferably 10 ⁇ m or more and 900 ⁇ m or less, and still more preferably 80 ⁇ m or more and 900 ⁇ m or less. Within such a range, both good light transmittance and transportability (that is, supportability of the circuit (heating wire) obtained by processing the copper layer) can be achieved.
- the resin film only needs to contain polyvinyl acetal resin, and may further contain known additives.
- Preferred examples of the polyvinyl acetal resin contained in the resin film include polyvinyl butyral resin from the viewpoint of penetration impact resistance and transparency as a glass intermediate film.
- additives that can be contained in the resin film include plasticizers, antioxidants, ultraviolet absorbers, adhesion modifiers, and the like.
- a commercially available polyvinyl acetal resin film may be used as it is, or a known method for producing a polyvinyl acetal resin film (see, for example, Patent Documents 2 and 3) may be adopted as it is or appropriately modified. It may be produced by
- the peel strength between the copper foil and the resin film in the laminate is preferably 0.60 kgf/cm or more, more preferably 1.00 kgf/cm or more, still more preferably 1.00 kgf/cm or more when the circuit height is 12 ⁇ m and the circuit width is 3 mm. It is 1.20 kgf/cm or more.
- the measurement of peel strength can be preferably carried out according to the procedure shown in the examples described later in accordance with JIS C 5016-1994 A method (90° peeling).
- the peel strength may be measured after metal plating (for example, copper plating) is applied until the copper foil has a thickness of 12 ⁇ m.
- the peel strength may be measured after etching until the thickness of the copper foil reaches 12 ⁇ m.
- the laminate manufactured by the method of the present invention is preferably used to form a heating element. That is, according to a preferred aspect of the present invention, a method for manufacturing a heating element is provided. This method comprises the steps of: preparing a laminate produced by the above method; processing the copper foil of the laminate to form a heating wire in a predetermined pattern; forming a heating element by joining or forming additional polyvinyl acetal resin films so as to sandwich the heating element.
- the processing of the copper foil is not particularly limited as long as it is performed based on a known method.
- a method such as a subtractive method, a semi-additive method, a modified semi-additive method as disclosed in Patent Document 4 can be used to form a heating wire with a predetermined pattern.
- the pattern of the heating wire preferably includes at least one pattern selected from the group consisting of linear, wavy, lattice and net.
- the line width of the heating wire (wiring) is preferably 1 ⁇ m or more and 25 ⁇ m or less, and more preferably.
- the heating wire is 1 ⁇ m or more and 15 ⁇ m or less, more preferably 1 ⁇ m or more and 5 ⁇ m or less.
- the height (thickness) of the heating wire is preferably 1 ⁇ m or more and 25 ⁇ m or less, more preferably 1 ⁇ m or more and 15 ⁇ m or less, and still more preferably 1 ⁇ m or more and 5 ⁇ m or less.
- the ratio of the area where the polyvinyl acetal resin film and the heating wire are not in contact on the surface of the polyvinyl acetal resin film on the heating wire side is preferably 70% or more and 98% or less. By doing so, it is possible to ensure even better visibility in the heating element.
- the bonding or forming of the additional polyvinyl acetal resin film to the laminate on which the heating wire is formed may be in accordance with the bonding or forming of the resin film to the copper foil described above. That is, the preferred aspects described above for bonding or forming the resin film to the copper foil also apply to bonding or forming the additional polyvinyl acetal resin film.
- the laminate or heating element produced by the method of the present invention is preferably used in the production of a defroster. That is, according to a preferred aspect of the present invention, there is provided a defroster having a heating element manufactured by the method described above.
- the configuration of the defroster is not particularly limited, and a known configuration can be adopted except for the provision of the heating element described above.
- the defroster of the present invention can be used in the form of laminated glass in which the above-described heating element is bonded to the surface or inside of the window glass of a vehicle such as an automobile.
- the heating wire forming the heating element may be stretched over the entire surface of the window glass, or may be provided only in a specific region of the window glass.
- the window glass can be efficiently warmed by the heating element, and frost, icing, fogging, etc. can be prevented or removed.
- Examples 1-7 Seven kinds of copper foils were prepared, and resin films were bonded to these copper foils to obtain laminates. Peel strength was measured using the obtained laminate. Specifically, it is as follows.
- Each parameter on the treated surface (roughened surface) of the prepared copper foil was measured according to ISO25178 using a laser microscope (OLS5000 manufactured by Olympus Corporation). Specifically, the surface profile of a region having an area of 16384 ⁇ m 2 on the treated surface of the copper foil was measured with the above laser microscope using a 100-fold lens with a numerical aperture (NA) of 0.95. After performing noise removal and first-order linear surface inclination correction on the surface profile of the obtained treated surface, the developed surface area ratio Sdr of the interface, the root mean square height Sq and the crest density Spd are measured by the surface property analysis. carried out.
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- Physics & Mathematics (AREA)
- Fluid Mechanics (AREA)
- Laminated Bodies (AREA)
- Engineering & Computer Science (AREA)
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- Lining Or Joining Of Plastics Or The Like (AREA)
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Abstract
Description
界面の展開面積比Sdrが0.50%以上9.00%以下であり、かつ、二乗平均平方根高さSqが0.010μm以上0.200μm以下である処理表面を少なくとも一方の側に有する銅箔を用意する工程と、
前記銅箔の前記処理表面にポリビニルアセタール樹脂フィルムを接合又は形成して積層板を形成する工程と、
を含み、前記Sdr及びSqは、ISO25178に準拠してSフィルターによるカットオフ波長0.55μm及びLフィルターによるカットオフ波長10μmの条件で測定される値である、積層板の製造方法が提供される。
前記方法により製造された積層板を用意する工程と、
前記積層板の前記銅箔を加工して所定パターンの発熱線を形成する工程と、
前記発熱線が形成された前記積層板に、前記発熱線を挟み込むように、追加のポリビニルアセタール樹脂フィルムを接合又は形成して発熱体を形成する工程と、
を含む、発熱体の製造方法が提供される。
本発明を特定するために用いられるパラメータの定義を以下に示す。
本発明は積層板の製造方法に関する。本発明の方法は、(1)所定の処理表面を少なくとも一方の側に有する銅箔を用意する工程と、(2)銅箔の処理表面にポリビニルアセタール樹脂フィルム(以下、単に「樹脂フィルム」と称することがある)を接合又は形成する工程とを含む。そして、銅箔の処理表面は、界面の展開面積比Sdrが0.50%以上9.00%以下であり、かつ、二乗平均平方根高さSqが0.010μm以上0.200μm以下である。このように、Sdr及びSqがそれぞれ所定の範囲に制御された処理表面を有する銅箔にポリビニルアセタール樹脂フィルムを接合又は形成することにより、銅箔-樹脂フィルム間の密着性に優れた積層板を製造することができる。
本発明の方法に用いる銅箔は少なくとも一方の側に処理表面を有する。この処理表面は、界面の展開面積比Sdrが0.50%以上9.00%以下であり、好ましくは2.50%以上9.00%以下、より好ましくは5.00%以上9.00%以下である。このような範囲内であると、処理表面がポリビニルアセタール樹脂の浸透に適した小さなコブを有しつつ、樹脂フィルムとの密着に寄与する処理表面の表面積をも大きくすることができるため、銅箔-樹脂フィルム間の密着性を向上することができる。
上記(1)で用意した銅箔の処理表面にポリビニルアセタール樹脂フィルムを接合又は形成して積層板を形成する。樹脂フィルムの銅箔への接合は、予め用意した樹脂フィルムを銅箔に熱圧着ないし接着することにより行うのが好ましい。好ましくは、樹脂フィルムの銅箔への接合は、180℃以下の温度及び0.6MPa以下の圧力で樹脂フィルム及び銅箔を熱圧着することにより行われ、より好ましくは100℃以上150℃以下の温度及び0.2MPa以上0.6MPa以下の圧力で行われる。また、この熱圧着は60秒以下で行うのが好ましく、より好ましくは10秒以上30秒以下である。前述のとおり、本発明の方法によれば、このような低温度かつ低圧力のラミネート条件であっても、銅箔-樹脂フィルム間の密着性に優れた積層板を製造することができる。
本発明の方法により製造される積層板は、発熱体の形成に用いられるのが好ましい。すなわち、本発明の好ましい態様によれば、発熱体の製造方法が提供される。この方法は、上記方法により製造された積層板を用意する工程と、積層板の銅箔を加工して所定パターンの発熱線を形成する工程と、発熱線が形成された積層板に、発熱線を挟み込むように、追加のポリビニルアセタール樹脂フィルムを接合又は形成して発熱体を形成する工程とを含む。
本発明の方法により製造される積層板ないし発熱体は、デフロスタの製造に用いられるのが好ましい。すなわち、本発明の好ましい態様によれば、上記方法により製造された発熱体を備えたデフロスタが提供される。デフロスタの構成は特に限定されるものではなく、前述の発熱体を備えること以外は公知の構成が採用可能である。例えば、本発明のデフロスタは、自動車等の乗物における窓ガラスの表面ないし内部に前述の発熱体が接合された、合わせガラスの形態で用いることができる。この場合、発熱体を構成する発熱線は窓ガラスの全面にわたって張り巡らされるものであってもよく、窓ガラスの特定の領域のみに設けられるものであってもよい。いずれにせよ、本発明のデフロスタによれば、発熱体によって効率的に窓ガラスを温めることができ、着霜や着氷、曇り等を防止ないし除去することができる。
銅箔を7種類用意し、これらの銅箔に樹脂フィルムを接合して積層板を得た。得られた積層板を用いてピール強度の測定を行った。具体的には以下のとおりである。
表1に示される各パラメータを有する処理表面(粗化処理面)を少なくとも一方の側に備えた銅箔(粗化処理銅箔)を7種類用意した。これらの銅箔は市販品、又は特許文献5等に開示されるような公知の製造方法で製造されたものである。なお、用意した銅箔の厚さは、例1~3及び5~7が12μmであり、例4が18μmであった。
可塑剤としてジヘキシルアジピン酸が配合された市販のポリビニルブチラール樹脂フィルム(厚さ:760μm)を用意した。後述するピール測定時の土台としての厚さ0.2mmの銅張積層板上に、上記ポリビニルブチラール樹脂フィルム及び上記(1)で用意した銅箔を、銅箔の処理表面が樹脂フィルムと当接するように積層した。このとき、温度110℃、圧力0.4MPa、時間20秒以下の条件で銅箔及び樹脂フィルムを熱圧着することにより、銅箔及び樹脂フィルムが接合された積層板を得た。
上記得られた積層板について、ピール強度の測定を以下のとおり行った。まず、積層板の銅箔側の表面にドライフィルムを張り合わせて、エッチングレジスト層を形成した。そして、このエッチングレジスト層に露光及び現像を行い、所定のエッチングパターンを形成した。その後、銅エッチング液で回路エッチングを行い、エッチングレジストを剥離して高さ12μm及び幅3mmの回路を得た。なお、例4については、エッチングレジスト層の形成前に、銅箔の厚さが12μmとなるまで積層体の銅箔側表面に対してエッチングを行った。こうして得られた回路を、JIS C 5016-1994のA法(90°剥離)に準拠して樹脂フィルムから引き剥がして、ピール強度(kgf/cm)を測定した。結果は表1に示されるとおりであった。
Claims (13)
- 界面の展開面積比Sdrが0.50%以上9.00%以下であり、かつ、二乗平均平方根高さSqが0.010μm以上0.200μm以下である処理表面を少なくとも一方の側に有する銅箔を用意する工程と、
前記銅箔の前記処理表面にポリビニルアセタール樹脂フィルムを接合又は形成して積層板を形成する工程と、
を含み、前記Sdr及びSqは、ISO25178に準拠してSフィルターによるカットオフ波長0.55μm及びLフィルターによるカットオフ波長10μmの条件で測定される値である、積層板の製造方法。 - 前記Sdrが2.50%以上9.00%以下であり、かつ、前記Sqが0.050μm以上0.180μm以下である、請求項1に記載の方法。
- 前記Sdrが5.00%以上9.00%以下であり、かつ、前記Sqが0.100μm以上0.140μm以下である、請求項1に記載の方法。
- 前記処理表面は、山の頂点密度Spdが100mm-2以上26000mm-2以下であり、前記SpdはISO25178に準拠してSフィルターによるカットオフ波長2μm及びLフィルターによるカットオフを行わない条件で測定される値である、請求項1~3のいずれか一項に記載の方法。
- 前記Spdが10000mm-2以上20000mm-2以下である、請求項4に記載の方法。
- 前記Spdが10000mm-2以上15000mm-2以下である、請求項4に記載の方法。
- 前記処理表面が複数の粗化粒子を備える、請求項1~6のいずれか一項に記載の方法。
- 前記樹脂フィルムの前記銅箔への接合が、180℃以下の温度及び0.6MPa以下の圧力で前記樹脂フィルム及び前記銅箔を熱圧着することにより行われる、請求項1~7のいずれか一項に記載の方法。
- 前記樹脂フィルムの厚さが1μm以上1000μm以下である、請求項1~8のいずれか一項に記載の方法。
- 前記ポリビニルアセタール樹脂がポリビニルブチラール樹脂である、請求項1~9のいずれか一項に記載の方法。
- 請求項1~10のいずれか一項に記載の方法により製造された積層板を用意する工程と、
前記積層板の前記銅箔を加工して所定パターンの発熱線を形成する工程と、
前記発熱線が形成された前記積層板に、前記発熱線を挟み込むように、追加のポリビニルアセタール樹脂フィルムを接合又は形成して発熱体を形成する工程と、
を含む、発熱体の製造方法。 - 前記所定パターンが、線状、波線状、格子状及び網状からなる群から選択される少なくとも1種のパターンを含む、請求項11に記載の方法。
- 請求項11又は12に記載の方法により製造された発熱体を備えた、デフロスタ。
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