CN115211244A - Radio wave absorbing sheet - Google Patents
Radio wave absorbing sheet Download PDFInfo
- Publication number
- CN115211244A CN115211244A CN202180017971.5A CN202180017971A CN115211244A CN 115211244 A CN115211244 A CN 115211244A CN 202180017971 A CN202180017971 A CN 202180017971A CN 115211244 A CN115211244 A CN 115211244A
- Authority
- CN
- China
- Prior art keywords
- layer
- mass
- sheet
- flame retardant
- radio wave
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
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- GVALZJMUIHGIMD-UHFFFAOYSA-H magnesium phosphate Chemical compound [Mg+2].[Mg+2].[Mg+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O GVALZJMUIHGIMD-UHFFFAOYSA-H 0.000 description 1
- 239000004137 magnesium phosphate Substances 0.000 description 1
- 229910000157 magnesium phosphate Inorganic materials 0.000 description 1
- 229960002261 magnesium phosphate Drugs 0.000 description 1
- 235000010994 magnesium phosphates Nutrition 0.000 description 1
- 230000007257 malfunction Effects 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 229910001463 metal phosphate Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000010295 mobile communication Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000000025 natural resin Substances 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 239000010955 niobium Substances 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- ANISOHQJBAQUQP-UHFFFAOYSA-N octyl prop-2-enoate Chemical compound CCCCCCCCOC(=O)C=C ANISOHQJBAQUQP-UHFFFAOYSA-N 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- AQSJGOWTSHOLKH-UHFFFAOYSA-N phosphite(3-) Chemical class [O-]P([O-])[O-] AQSJGOWTSHOLKH-UHFFFAOYSA-N 0.000 description 1
- 150000003014 phosphoric acid esters Chemical class 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 description 1
- 229920002312 polyamide-imide Polymers 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 239000011116 polymethylpentene Substances 0.000 description 1
- 229920006324 polyoxymethylene Polymers 0.000 description 1
- 239000001205 polyphosphate Substances 0.000 description 1
- 235000011176 polyphosphates Nutrition 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 229920005990 polystyrene resin Polymers 0.000 description 1
- 229920005749 polyurethane resin Polymers 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 239000005033 polyvinylidene chloride Substances 0.000 description 1
- 229910000160 potassium phosphate Inorganic materials 0.000 description 1
- 235000011009 potassium phosphates Nutrition 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- SCUZVMOVTVSBLE-UHFFFAOYSA-N prop-2-enenitrile;styrene Chemical compound C=CC#N.C=CC1=CC=CC=C1 SCUZVMOVTVSBLE-UHFFFAOYSA-N 0.000 description 1
- 238000004549 pulsed laser deposition Methods 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000001488 sodium phosphate Substances 0.000 description 1
- 229910000162 sodium phosphate Inorganic materials 0.000 description 1
- 235000011008 sodium phosphates Nutrition 0.000 description 1
- 229920003048 styrene butadiene rubber Polymers 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
- 239000013077 target material Substances 0.000 description 1
- ISXSCDLOGDJUNJ-UHFFFAOYSA-N tert-butyl prop-2-enoate Chemical compound CC(C)(C)OC(=O)C=C ISXSCDLOGDJUNJ-UHFFFAOYSA-N 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- ILJSQTXMGCGYMG-UHFFFAOYSA-N triacetic acid Chemical compound CC(=O)CC(=O)CC(O)=O ILJSQTXMGCGYMG-UHFFFAOYSA-N 0.000 description 1
- VMFOHNMEJNFJAE-UHFFFAOYSA-N trimagnesium;diphosphite Chemical compound [Mg+2].[Mg+2].[Mg+2].[O-]P([O-])[O-].[O-]P([O-])[O-] VMFOHNMEJNFJAE-UHFFFAOYSA-N 0.000 description 1
- XZZNDPSIHUTMOC-UHFFFAOYSA-N triphenyl phosphate Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)(=O)OC1=CC=CC=C1 XZZNDPSIHUTMOC-UHFFFAOYSA-N 0.000 description 1
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 1
- NCPXQVVMIXIKTN-UHFFFAOYSA-N trisodium;phosphite Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])[O-] NCPXQVVMIXIKTN-UHFFFAOYSA-N 0.000 description 1
- BIKXLKXABVUSMH-UHFFFAOYSA-N trizinc;diborate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]B([O-])[O-].[O-]B([O-])[O-] BIKXLKXABVUSMH-UHFFFAOYSA-N 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 229920006337 unsaturated polyester resin Polymers 0.000 description 1
- 238000001771 vacuum deposition Methods 0.000 description 1
- 239000002759 woven fabric Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
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
- B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
- B32B5/02—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
- B32B7/02—Physical, chemical or physicochemical properties
- B32B7/025—Electric or magnetic properties
-
- 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
- H05K9/00—Screening of apparatus or components against electric or magnetic fields
Landscapes
- Engineering & Computer Science (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Laminated Bodies (AREA)
- Shielding Devices Or Components To Electric Or Magnetic Fields (AREA)
Abstract
The radio wave absorbing sheet comprises an outer layer 1, a conductive fiber sheet, and an outer layer 2, wherein the outer layer 1, the conductive fiber sheet, and the outer layer 2 are laminated in this order, the outer layer 1 contains a binder resin, a phosphorus flame retardant, and an inorganic flame retardant, and the outer layer 2 contains a binder resin, a phosphorus flame retardant, and an inorganic flame retardant.
Description
Technical Field
The present invention relates to a radio wave absorbing sheet and the like.
Background
Conventionally, in portable communication devices, electronic devices, and household electric appliances, members to which a radio wave absorbing material is applied have been used in order to prevent leakage and intrusion of radio waves. In recent years, particularly in electronic devices (information communication devices) using radio waves, radio wave absorbers that absorb unnecessary electromagnetic waves have been widely used from the viewpoints of preventing malfunction and signal degradation of other electronic devices and preventing adverse effects on human bodies. As the radio wave absorber, a product obtained by dispersing magnetic metal powder in various rubber or resin materials is used. Patent document 1 discloses a radio wave absorbing sheet in which a metal is adhered to the surface of a fabric (patent document 1). Such a radio wave absorbing sheet can be made flexible and thinner, and therefore can be disposed in a small space in a small electronic device or the like.
Documents of the prior art
Patent document
Patent document 1: japanese patent No. 5722608
Disclosure of Invention
Technical problem to be solved by the invention
Flame retardancy is required for parts used in electronic devices. Further, in addition to noise countermeasures, higher flame retardancy is required as countermeasures against heat generated from IC chips and the like, which are noise sources, in the development of high-capacity and high-speed communications such as 5G and IoT.
When flame retardancy is imparted to the radio wave absorbing sheet including the conductive fiber sheet, it is conceivable to include a flame retardant in a predetermined member. However, in this case, the durability of the radio wave absorption sheet is impaired, and the radio wave absorption characteristics may change.
The invention provides a radio wave absorption sheet having flame retardancy and excellent durability.
Means for solving the problems
The conductive fiber sheet has metal adhered to a fiber base material. The surface resistance of the radio wave absorption sheet is adjusted to a predetermined value by forming a conductive path by the fibers constituting the fiber base material and the metal attached to the fibers. When a radio wave enters the radio wave absorbing sheet from the outside, if the surface resistance is a predetermined value, reflection of the radio wave is suppressed. Further, the incident radio wave is converted into a current and absorbed in the process of passing through the conductive fiber sheet. That is, the surface resistance is adjusted to a range in which reflection of the radio wave entering from the outside is suppressed while having conductivity, whereby the radio wave absorbability can be exhibited. However, if a flame retardant is contained in the radio wave absorption sheet to impart flame retardancy, the metal may be deteriorated by the influence of the flame retardant, and the surface resistance value may be changed. As a result of intensive studies, the present inventors have found that the above-mentioned problems can be solved by a radio wave absorbing sheet comprising an outer layer 1, a conductive fiber sheet, and an outer layer 2, wherein the outer layer 1, the conductive fiber sheet, and the outer layer 2 are laminated in this order, the outer layer 1 contains a binder resin, a phosphorus flame retardant, and an inorganic flame retardant, and the outer layer 2 contains a binder resin, a phosphorus flame retardant, and an inorganic flame retardant. The present inventors have further studied based on this finding and, as a result, have completed the present invention. That is, the present invention includes the following aspects.
and an outer layer 1, a conductive fiber sheet, and an outer layer 2 are laminated in this order,
the outer layer 1 contains a binder resin, a phosphorus flame retardant and an inorganic flame retardant, and
the outer layer 2 contains a binder resin, a phosphorus flame retardant, and an inorganic flame retardant.
the outer layer 2 comprises an adhesive layer 2a and a sheet layer 2b,
the adhesive layer 2a and the sheet layer 2b are laminated in this order from the conductive fiber sheet side.
the total content of the flame retardant in the adhesive layer 2a is 0 to 40 mass% with respect to 100 mass% of the adhesive layer 2a.
the total content of the flame retardant in the sheet layer 2b is 40 to 90% by mass with respect to 100% by mass of the sheet layer 2b.
The radio wave absorbing sheet according to any one of the items 1 to 4, wherein,
the outer layer 1 is an adhesive layer.
The radio wave absorbing sheet according to any one of the items 2 to 4, wherein,
the outer layer 1 comprises an adhesive layer 1a and a sheet layer 1b,
the adhesive layer 1a and the sheet layer 1b are laminated in this order from the conductive fiber sheet side.
the total content of the flame retardant in the adhesive layer 1a is 0 to 50 mass% with respect to 100 mass% of the adhesive layer 1a.
the total content of the flame retardant in the sheet layer 1b is 50 to 90% by mass with respect to 100% by mass of the sheet layer 1b.
The radio wave absorbing sheet according to item 9 or any one of items 6 to 8, wherein,
the outer layer 1 comprises an adhesive layer 1a, a sheet layer 1b and an adhesive layer 1c,
the adhesive layer 1a, the sheet layer 1b, and the adhesive layer 1c are laminated in this order from the conductive fiber sheet side.
the total content of the flame retardant in the adhesive layer 1c is 10 to 90 mass% with respect to 100 mass% of the adhesive layer 1c.
The radio wave absorbing sheet according to item 11 or any one of items 1 to 10, wherein,
the inorganic flame retardant contained in at least one of the outer layer 1 or the outer layer 2 contains an aluminum component.
The radio wave absorbing sheet according to any one of items 6 to 11, wherein,
an integrated value of an endothermic quantity in a range of 200 to 400 ℃ of at least one of the adhesive layer 1a and the adhesive layer 1c is 9000 [ mu ] V · s/mg or more.
The radio wave absorbing sheet according to any one of items 1 to 12, wherein,
the conductive fiber sheet includes: the metal layer is configured on at least one surface of the fiber base material.
Item 14 the radio wave absorbing sheet according to item 13, wherein,
the metal layer includes: the conductive layer and the barrier layer are arranged on at least one surface of the conductive layer.
Item 15, the radio wave absorbing sheet according to item 13 or 14, wherein,
the surface resistance value of the metal layer is 40-500 omega/\9633.
The radio wave absorbing sheet according to item 16 or any one of items 13 to 15, wherein,
the metal layer includes: at least 1 metal element selected from the group consisting of nickel, molybdenum, chromium, titanium, copper, and aluminum.
Item 17, the radio wave absorption sheet according to any one of items 1 to 16, wherein the thickness is 100 to 500 μm.
Item 18, the radio wave absorption sheet according to any one of items 1 to 17, which has a flame retardancy of V-0 or V-1 in a test according to UL94 vertical burning test.
Effects of the invention
According to the present invention, a radio wave absorbing sheet having flame retardancy and excellent durability can be provided.
Drawings
FIG. 1 is a schematic cross-sectional view showing an example of a conductive fiber sheet including a metal layer and a fiber base material.
Fig. 2 is a schematic cross-sectional view showing an example of a conductive fiber sheet including a metal layer (conductive layer + barrier layer) and a fiber base material.
FIG. 3 is a schematic cross-sectional view showing an example of a radio wave absorbing sheet of the present invention.
Fig. 4 is a schematic cross-sectional view showing an example of the radio wave absorbing sheet of the present invention in which the outer layer 2 includes the adhesive layer 2a and the sheet layer 2 b.
Fig. 5 is a schematic cross-sectional view showing an example of the radio wave absorbing sheet of the present invention in which the outer layer 1 includes an adhesive layer 1a, a sheet layer 1b, and an adhesive layer 1c.
Detailed Description
In the present specification, the expressions "including" and "including" include concepts of "including", "consisting essentially of", and "consisting of only.
The present invention relates, in one aspect thereof, to a radio wave absorbing sheet (also referred to as "the radio wave absorbing sheet of the present invention" in the present specification) comprising an outer layer 1, a conductive fiber sheet, and an outer layer 2, wherein the outer layer 1, the conductive fiber sheet, and the outer layer 2 are laminated in this order, the outer layer 1 contains a binder resin, a phosphorus flame retardant, and an inorganic flame retardant, and the outer layer 2 contains a binder resin, a phosphorus flame retardant, and an inorganic flame retardant. Which will be explained below.
<1. Conductive fiber sheet >
The conductive fiber sheet is not particularly limited as long as it is a conductive fiber sheet. The conductive fiber sheet preferably includes a fiber base material and a metal layer disposed on at least one surface of the fiber base material.
<1-1. Fibrous base Material >
The fibrous base material is a base material containing fibers or fiber bundles as a raw material, and is not particularly limited as long as it is in a sheet form. The fiber base material may contain components other than the fibers and the fiber bundles as long as the effects of the present invention are not significantly impaired. In this case, the total amount of the fibers and the fiber bundles in the fiber base material is, for example, 80 mass% or more, preferably 90 mass% or more, more preferably 95 mass% or more, further preferably 99 mass% or more, and usually less than 100 mass%.
The material constituting the fibers is not particularly limited as long as it is fibrous or can be formed into a fibrous shape. Examples of the raw material of the fiber include: polyester resins such as polyethylene terephthalate (PET), polybutylene terephthalate (PBT), polyethylene naphthalate, modified polyesters, polyethylene (PE) resins, polyolefin resins such as polypropylene (PP) resins, polystyrene resins, and cyclic olefin resins, vinyl resins such as polyvinyl chloride and polyvinylidene chloride, polyvinyl acetal resins such as polyvinyl butyral (PVB), polyether ether ketone (PEEK) resins, polysulfone (PSF) resins, polyphenylene Sulfide (PPs) resins, polyether Sulfone (PEs) resins, polycarbonate (PC) resins, polyamide resins, aromatic polyamide (PPA) resins, polyimide resins, polyamide imide (PAI) resins, polyether imide (PEI) resins, polymethylpentene (PMP) resins, acrylic resins, cellulose Triacetate (TAC) resins, polyarylate (PAR), synthetic resins such as Liquid Crystal Polymers (LCP), natural resins, cellulose, glass, and the like. The fibers may be composed of 1 kind of single fiber raw material, or may be composed of 2 or more kinds of fiber raw materials.
The basis weight (weight in square meter) of the fiber base material is, for example, 1 to 500g/m 2 Preferably 3 to 300g/m 2 More preferably 5 to 150g/m 2 。
The thickness of the fibrous base material is, for example, 1 to 3000. Mu.m, preferably 5 to 1500. Mu.m, and more preferably 10 to 800. Mu.m. From the viewpoint of being suitable for placement in a minute space in a small electronic device or the like, the thickness of the fiber base material is preferably 300 μm or less, more preferably 200 μm or less, and still more preferably 100 μm or less.
The lower limit of the density of the fibrous base material is preferably 2.0X 10 4 g/m 3 More preferably 1.0X 10 5 g/m 3 More preferably 1.5X 10 5 g/m 3 . The upper limit of the density of the fiber base material is preferably 8.0X 10 5 g/m 3 More preferably 6.0X 10 5 g/m 3 . By setting the density of the fiber base material, the radio wave absorbability of the conductive fiber sheet can be improved. For this reason, although not bound by a particular theory, the following presumptions can be made: by using the fiber base material having a density in a specific range, the metal is not only attached to the surface of the fiber base material but also enters the interior of the fiber base material, and therefore the radio wave absorption property (particularly, the absorptivity) is improved.
Examples of the fiber base material include nonwoven fabric, net, woven fabric, and knitted fabric. Among these, a nonwoven fabric is preferable from the viewpoint of flexibility, followability, and the like.
The fiber base material preferably contains a resin having a melting point of 250 ℃ or higher, from the viewpoint of heat resistance of the radio wave absorbing sheet of the present invention. The resin may be a material of the fibers constituting the fiber base material, or may be a component other than the fibers. Examples of such a resin include various LCP resins, PET resins, and polyamide resins (nylon 66).
The layer structure of the fiber base material is not particularly limited. The fiber base material may be composed of 1 kind of single fiber base material, or may be composed of 2 or more kinds of fiber base materials in combination (laminated).
In the present specification, the melting point refers to a main absorption peak temperature measured by a differential scanning calorimeter (DSC; for example, "TA3000" by Mettler) in accordance with JIS K7121. Specifically, in the measurement by the DSC apparatus, 10 to 20mg of a measurement sample was taken, sealed in an aluminum pan, and then nitrogen as a carrier gas was flowed at a flow rate of 100mL/min, and the absorption peak in the 1st run in the case of raising the temperature at 20 ℃/min was measured. When no clear absorption peak was observed in the 1st run (1 st run) depending on the type of the polymer, the temperature was raised at a temperature rise rate of 50 ℃/min to a temperature 50 ℃ higher than the expected melting temperature, the temperature was maintained at that temperature for 3 minutes or more, the polymer was completely dissolved, the polymer was cooled at a rate of 80 ℃/min to 50 ℃, and then the endothermic peak in the 2nd run (2 nd run) was measured at a temperature rise rate of 20 ℃/min.
<1-2. Metal layer >
The metal layer is disposed on the fiber base material directly or via another layer, in other words, on at least one surface of the 2 main surfaces of the fiber base material. The metal layer is not particularly limited as long as it includes a conductive layer containing a conductive metal as a raw material.
The surface resistance of the metal layer is not particularly limited as long as the radio wave absorption sheet of the present invention can exhibit radio wave absorption characteristics. The surface resistance value is, for example, 10. Omega./9633a, 1000. Omega./9633a, or less. From the viewpoint of further suppressing the variation in surface resistance value, the surface resistance value is preferably 40 Ω/\9633, more preferably 500 Ω/\33, or less, more preferably 50 Ω/\9633, or more preferably 300 Ω/\9633, or less.
<1-2-1. Conductive layer >
The conductive layer is not particularly limited as long as it is a layer containing a conductive metal as a raw material. The conductive layer may contain a component other than a metal as long as the effect of the present invention is not significantly impaired. In this case, the amount of the metal in the conductive layer is, for example, 80 mass% or more, preferably 90 mass% or more, more preferably 95 mass% or more, further preferably 99 mass% or more, and usually less than 100 mass%.
The conductive layer preferably comprises a volume resistivity of 140 x 10 -8 Metal elements of not more than Ω · m. This makes it easy to adjust the surface resistance value of the metal layer to the above range.
The metal constituting the conductive layer is not particularly limited as long as it can exhibit radio wave absorption properties. Examples of the metal include nickel, molybdenum, chromium, titanium, copper, aluminum, gold, silver, zinc, tin, platinum, iron, indium, alloys containing these metals, and metal compounds of these metals or alloys containing these metals. From the viewpoint of suppressing the change over time (durability) of the radio wave absorption characteristics of the conductive fiber sheet, the conductive layer preferably contains at least 1 metal element selected from nickel, molybdenum, chromium, titanium, copper, and aluminum.
When the at least 1 metal element selected from the group consisting of nickel, molybdenum, chromium, titanium, copper, and aluminum is contained, the content thereof is, for example, 10% by mass or more, preferably 20% by mass or more, more preferably 40% by mass or more, further preferably 60% by mass or more, and usually less than 100% by mass. .
As the conductive layer, a conductive layer containing molybdenum is preferably used from the viewpoint of easiness in adjustment of durability and sheet resistance. The lower limit of the content of molybdenum is not particularly limited, but from the viewpoint of further improving the durability, it is preferably 5% by weight, more preferably 7% by weight, still more preferably 9% by weight, still more preferably 11% by weight, particularly preferably 13% by weight, very particularly preferably 15% by weight, and most preferably 16% by weight. The upper limit of the content of molybdenum is preferably 70 wt%, more preferably 30 wt%, even more preferably 25 wt%, and even more preferably 20 wt%, from the viewpoint of facilitating adjustment of the surface resistance value.
When the conductive layer contains molybdenum, it more preferably further contains nickel and chromium. By further containing nickel and chromium in addition to molybdenum, a conductive fiber sheet having more excellent durability can be produced. Examples of the alloy containing nickel, chromium and molybdenum include Hastelloy alloys B-2, B-3, C-4, C-2000, C-22, C-276, G-30, N, W and X.
When the conductive layer contains molybdenum, nickel, and chromium, the content of molybdenum is preferably 5 wt% or more, the content of nickel is preferably 40 wt% or more, and the content of chromium is preferably 1 wt% or more. When the contents of molybdenum, nickel and chromium are in the above ranges, a conductive fiber sheet having more excellent durability can be produced. More preferably, the molybdenum, nickel and chromium are contained in an amount of 7 wt% or more in terms of molybdenum content, 45 wt% or more in terms of nickel content and 3 wt% or more in terms of chromium content. Further preferably, the molybdenum, nickel and chromium are contained in an amount of 9 wt% or more in terms of molybdenum content, 47 wt% or more in terms of nickel content and 5 wt% or more in terms of chromium content.
The conductive layer may contain a metal other than molybdenum, nickel, and chromium. Examples of such metals include iron, cobalt, tungsten, manganese, and titanium. When the conductive layer contains molybdenum, nickel, and chromium, the upper limit of the total content of the metals other than molybdenum, nickel, and chromium is preferably 45% by weight, more preferably 40% by weight, even more preferably 35% by weight, even more preferably 30% by weight, particularly preferably 25% by weight, and very preferably 23% by weight, from the viewpoint of the durability of the conductive layer. The lower limit of the total content of the metals other than molybdenum, nickel and chromium is, for example, 1 wt% or more.
The conductive layer may contain silicon and/or carbon. In the case where the conductive layer contains silicon and/or carbon, the content of silicon and/or carbon is preferably 1 wt% or less, and more preferably 0.5 wt% or less, respectively and independently. In addition, when the conductive layer contains silicon and/or carbon, the content of silicon and/or carbon is preferably 0.01 wt% or more.
The amount of the metal element and/or metalloid element attached to the conductive layer is not particularly limited as long as the radio wave absorption sheet of the present invention can exhibit radio wave absorption properties. The amount of the metal element and/or metalloid element adhered to the conductive layer is, for example, 5 to 200. Mu.g/cm 2 Preferably 7 to 100. Mu.g/cm 2 More preferably 10 to 80. Mu.g/cm 2 . If it is 5. Mu.g/cm 2 As described above, the fiber base material is imparted with conductivity, and radio wave absorbability is easily exhibited. Further, if it is 200. Mu.g/cm 2 Hereinafter, reflection of the radio wave at the surface is suppressed, and the radio wave absorbability is easily exhibited.
The thickness of the conductive layer is not particularly limited as long as the radio wave absorption sheet of the present invention can exhibit radio wave absorption characteristics. The thickness of the conductive layer is, for example, 10nm to 100nm, preferably 20nm to 60nm, and more preferably 30nm to 40nm. If the thickness is 10nm or more, the fiber base material is imparted with conductivity, and the radio wave absorbability is easily exhibited. Further, if it is 100nm or less, reflection of the radio wave at the surface is suppressed, and the radio wave absorbability is easily exhibited.
The amount of the metal element and/or metalloid element attached derived from the conductive layer can be determined by fluorescent X-ray analysis. Specifically, analysis was performed using a scanning fluorescent X-ray analyzer (for example, ZSPrimusIII +, manufactured by RIGAKU corporation, or the equivalent) so that the acceleration voltage was 50kV, the acceleration current was 50mA, and the integration time was 60 seconds. The X-ray intensity of the K α ray of the component of the measurement object is measured, and the intensity at the background position is also measured in addition to the peak position, so that the net intensity can be calculated. The measured intensity value can be converted into the amount of adhesion based on a calibration curve prepared in advance. The same samples were analyzed 5 times, and the average value was used as the average adhesion amount.
The layer structure of the conductive layer is not particularly limited. The conductive layer may be composed of 1 kind of single conductive layer, or may be composed of a combination of 2 or more kinds of conductive layers.
<1-2-2. Barrier layer >
The metal layer preferably includes a barrier layer disposed on the conductive layer and at least one surface (preferably both surfaces) of the conductive layer.
The barrier layer is not particularly limited as long as it is a layer capable of protecting the conductive layer and suppressing the deterioration thereof, and preferably has a composition different from that of the conductive layer. Examples of the material of the barrier layer include metals, metalloids, alloys, metal compounds, and metalloid compounds. The barrier layer may contain components other than the raw materials as long as the effects of the present invention are not significantly impaired. In this case, the amount of the raw material in the barrier layer is, for example, 80% by mass or more, preferably 90% by mass or more, more preferably 95% by mass or more, further preferably 99% by mass or more, and usually less than 100% by mass.
Examples of the metal that can be suitably used for the barrier layer include nickel, titanium, aluminum, niobium, and cobalt. Examples of the metalloid which can be suitably used in the barrier layer include silicon, germanium, antimony, bismuth, and the like.
Specific examples of the metal compound and metalloid compound used in the barrier layer include SiO 2 SiOx (X represents an oxidation number, 0)<X<2)、Al 2 O 3 、MgAl 2 O 4 、CuO、CuN、TiO 2 TiN, AZO (aluminum-doped zinc oxide), and the like.
The barrier layer preferably contains at least 1 element selected from the group consisting of nickel, silicon, titanium and aluminum. Among them, silicon is preferably used.
The amount of the metal element and/or metalloid element attached to the barrier layer is not particularly limited as long as the radio wave absorption sheet of the present invention can exhibit the radio wave absorption property. The amount of the metal element and/or metalloid element adhered to the barrier layer is, for example, 0.5 to 50. Mu.g/cm 2 Preferably 1 to 30. Mu.g/cm 2 More preferably 2 to 20. Mu.g/cm 2 。
The layer structure of the barrier layer is not particularly limited. The barrier layer may be composed of 1 kind of single barrier layer, or may be composed of a combination of 2 or more kinds of barrier layers.
<2. Outer layer >
In the present specification, the outer layer 1 and the outer layer 2 are collectively referred to as "outer layer". When the conductive fiber sheet includes a fiber base material and a metal layer disposed on one surface of the fiber base material, it is preferable that the outer layer 1 is disposed on the fiber base material side of the conductive fiber sheet and the outer layer 2 is disposed on the metal layer side of the conductive fiber sheet from the viewpoint of durability.
The binder resin contained in the outer layer is not particularly limited as long as it is a resin capable of dispersing the flame retardant. Examples of the binder resin include vinyl resins, thermoplastic resins, curable resins, thermoplastic block copolymers, and elastomers. Examples of the vinyl resin include vinyl acetate resins, acrylic resins, and styrene resins. Examples of the thermoplastic resin include polyester resins such as polyethylene terephthalate (PET), polybutylene terephthalate (PBT), polyethylene naphthalate and modified polyester, polyethylene (PE) resins, polypropylene (PP) resins, polyolefin resins, polyvinyl butyral, ethylene-vinyl acetate copolymers, and polyamide resins. Examples of the curable resin include epoxy resins, polyurethane resins, polyimide resins, and unsaturated polyester resins. The curable resin may be a room temperature curable resin, a thermosetting resin, a photocurable resin, or a moisture curable resin. The curable resin may be used in combination with a curing agent. Examples of the thermoplastic block copolymer include a styrene-butadiene-styrene block copolymer, a styrene-isoprene-styrene block copolymer, a hydrogenated product of a styrene-butadiene-styrene block copolymer, and a hydrogenated product of a styrene-isoprene-styrene block copolymer. Examples of the elastomer include styrene-butadiene copolymer rubber, acrylonitrile-styrene block copolymer rubber, and the like. Among them, from the viewpoint of ease of lamination of the outer layer, the outer layer preferably contains a resin having adhesiveness as a binder resin or a layer containing a resin having adhesiveness as a binder resin. As the resin having adhesiveness, an acrylic resin is particularly preferable. The binder resin may be 1 kind alone or a combination of 2 or more kinds.
As the acrylic ester used for the acrylic resin, various acrylic esters used for adhesives can be used, and an alkyl acrylate having an alkyl group of 1 to 12 carbon atoms is preferred. Examples of the alkyl acrylate having 1 to 12 carbon atoms include monomers such as methyl acrylate, ethyl acrylate, n-butyl acrylate, isobutyl acrylate, tert-butyl acrylate, n-octyl acrylate, isooctyl acrylate, isononyl acrylate, cyclohexyl acrylate, and 2-ethylhexyl acrylate. Among them, from the viewpoint of adhesiveness, an alkyl acrylate in which the alkyl group has 4 to 8 carbon atoms is preferable, and n-butyl acrylate and 2-ethylhexyl acrylate are particularly preferable. The acrylic resin may be 1 type alone or 2 or more types in combination.
As the binder resin, a tackifier may also be contained. The adhesion is improved by the tackifier. Examples of the tackifier include petroleum resins such as aliphatic petroleum resins, aromatic petroleum resins, and alicyclic petroleum resins, rosin ester resins, disproportionated rosin resins, polymerized rosin ester resins, rosin resins such as rosin phenols, terpene resins, and terpene phenol resins. The tackifier may be 1 kind alone or a combination of 2 or more kinds.
The content of the binder resin in the outer layer 1 is, for example, 20 to 95 mass% with respect to 100 mass% of the outer layer 1. From the viewpoint of dispersibility and flame retardancy of the flame retardant, the content is preferably 30 to 80% by mass, more preferably 35 to 75% by mass, and still more preferably 40 to 70% by mass.
The content of the binder resin in the outer layer 2 is, for example, 10 to 98 mass% with respect to 100 mass% of the outer layer 2. From the viewpoint of dispersibility and flame retardancy of the flame retardant, the content is preferably 15 to 95% by mass, more preferably 20 to 90% by mass, still more preferably 25 to 85% by mass, and particularly preferably 30 to 75% by mass.
The content of the binder resin was determined as follows. Specifically, TG-DTA (for example, thermo plus EVO2 manufactured by RIGA KU Co., ltd., or the equivalent) was used, and the measurement was carried out under the following conditions, and the mass reduction rate up to a temperature of 450 ℃ was obtained.
(measurement conditions of the differential Heat balance)
Measurement of atmosphere: air 100mL/min
Sample size: 10mg of
Measurement temperature: 30 ℃→ 800 ℃
Temperature rise conditions: 10 ℃/min
In the radio wave absorbing sheet of the present invention, the outer layer contains a phosphorus flame retardant and an inorganic flame retardant. By combining the phosphorus flame retardant and the inorganic flame retardant, the flame retardancy can be improved, and the flame retardancy can be exhibited to a certain degree or more while suppressing the change in the electric resistance value. The reason why the flame retardancy can be improved by combining the phosphorus-based flame retardant with the inorganic flame retardant is not limited to a specific reason, but it is presumed that: the flame retardancy can be improved by using an inorganic flame retardant in combination with a phosphorus flame retardant which blocks oxygen and heat by the formation of carbon (char) and has an oxygen radical trapping effect. Further, since the flame retardancy is exhibited while the amount of the phosphorus-based flame retardant used is reduced, it is considered that the flame retardancy of a certain degree or more can be exhibited while the change in the electric resistance value due to the phosphorus-based flame retardant is suppressed.
The phosphorus-based flame retardant is not particularly limited as long as it contains phosphorus, and examples thereof include red phosphorus, triphenyl phosphate, tricresyl phosphate, cresyldiphenyl phosphate, tris (2-ethylhexyl) phosphate, bisphenol a diphosphate, and phosphate esters such as 1, 3-phenylene bisxylyl phosphate, metal phosphates such as sodium phosphate, potassium phosphate, and magnesium phosphate, metal phosphites such as sodium phosphite, potassium phosphite, magnesium phosphite, and aluminum phosphite, ammonium polyphosphate, urethane polyphosphate, and biguanide phosphate. The phosphorus-based flame retardant may be 1 kind alone or a combination of 2 or more kinds.
The content of the phosphorus-based flame retardant in the outer layer 1 is, for example, 5 to 80 mass% with respect to 100 mass% of the outer layer 1. The content is preferably 10 to 70% by mass, more preferably 15 to 65% by mass, still more preferably 17.5 to 60% by mass, and particularly preferably 20 to 40% by mass. The lower limit or more improves the flame retardancy, and the upper limit or less suppresses the change in the resistance value.
The content of the phosphorus-based flame retardant in the outer layer 2 is, for example, 3 to 90% by mass with respect to 100% by mass of the outer layer 2. The content is preferably 5 to 85% by mass, more preferably 10 to 85% by mass, still more preferably 20 to 82.5% by mass, and particularly preferably 30 to 80% by mass. The lower limit or more improves the flame retardancy, and the upper limit or less suppresses the change in the resistance value.
The content of the phosphorus-based flame retardant can be measured, for example, as follows. Specifically, the residual ash content can be determined from the elemental ratio of the ash content by measuring the residual ash content using an energy dispersive fluorescent X-ray spectrometer (for example, EDX-800HS manufactured by Shimadzu corporation or equivalent) after the temperature of TG-DTA reaches 800 ℃.
(measurement conditions of energy dispersive fluorescent X-ray analysis device)
X-ray target (target): rhodium
Measurement time 300 seconds
Collimator: phi 1mm
Voltage: na-Sc 15kV Na-U50 kV
Atmosphere: and (4) carrying out vacuum.
The inorganic flame retardant is not particularly limited as long as it can exhibit flame retardancy. Examples of the inorganic flame retardant include metal hydroxides, metal oxides, and ceramics. Examples of the metal hydroxide include aluminum hydroxide, magnesium hydroxide, calcium hydroxide, zirconium hydroxide, barium hydroxide, and hydrotalcite. The inorganic flame retardant preferably contains an aluminum component and a magnesium component. Aluminum hydroxide or magnesium hydroxide is more preferable from the viewpoint of exhibiting an endothermic effect by dehydration reaction and improving flame retardancy by using it in combination with a phosphorus flame retardant. From the viewpoint of thermal decomposition temperature, aluminum hydroxide is particularly preferable. The inorganic flame retardant may be 1 kind alone or a combination of 2 or more kinds. In the present specification, the aluminum component refers to an aluminum element, and the magnesium component refers to a magnesium element. In the present specification, aluminum phosphite is a phosphorus-based flame retardant, and is an inorganic-based flame retardant.
The content of the inorganic flame retardant in the outer layer 1 is, for example, 3 to 70% by mass with respect to 100% by mass of the outer layer 1. The content is preferably 5 to 60% by mass, more preferably 8 to 55% by mass, and still more preferably 10 to 50% by mass. The lower limit or more improves the flame retardancy, and the upper limit or less suppresses the change in the resistance value.
The content of the inorganic flame retardant in the outer layer 2 is, for example, 5 to 95% by mass with respect to 100% by mass of the outer layer 2. The content is preferably 8 to 90% by mass, more preferably 10 to 85% by mass, still more preferably 20 to 82.5% by mass, and particularly preferably 30 to 80% by mass. The lower limit or more improves the flame retardancy, and the upper limit or less suppresses the change in the resistance value.
The content of the inorganic flame retardant was measured as follows. Specifically, the temperature of the residual ash was measured using an energy dispersive fluorescent X-ray analyzer after the temperature was reached to 800 ℃ using TG-DTA, and the measurement was obtained from the elemental ratio of the ash.
(measurement conditions of energy dispersive fluorescent X-ray analysis device)
X-ray target material: rhodium
Measurement time 300 seconds
Collimator: phi 1mm
Voltage: na-Sc 15kV Na-U50 kV
Atmosphere: and (4) carrying out vacuum.
The outer layer may contain other flame retardants than those mentioned above. Examples of the other flame retardant include a silicone flame retardant, a halogen flame retardant (halogenated aromatic compound), a nitrogen flame retardant (guanidine, triazine, melamine, and derivatives thereof), a boron flame retardant (e.g., zinc borate), and the like. Among them, from the viewpoint of environmental conservation and safety, the outer layer preferably does not contain a halogen-based flame retardant.
In the case where the outer layer contains other flame retardant, the content thereof is preferably small. The content is, for example, 15 mass% or less, preferably 10 mass% or less, more preferably 5 mass% or less, and still more preferably 0 mass% with respect to 100 mass% of the outer layer. When the outer layer contains a halogen flame retardant, the content thereof is preferably small. The content is, for example, 3% by mass or less, preferably 2% by mass or less, more preferably 1% by mass or less, and further preferably 0% by mass, relative to 100% by mass of the outer layer.
Hereinafter, the phosphorus-based flame retardant, the inorganic flame retardant, and the other flame retardants are also collectively referred to as "flame retardants".
The total content of the flame retardant or the total content of the phosphorus-based flame retardant and the inorganic flame retardant in the outer layer 1 is, for example, 15 to 85 mass% with respect to 100 mass% of the outer layer 1. The content is preferably 20 to 75% by mass, more preferably 25 to 65% by mass. The lower limit or more improves the flame retardancy, and the upper limit or less suppresses the change in the resistance value.
The total content of the flame retardant or the total content of the phosphorus-based flame retardant and the inorganic flame retardant in the outer layer 2 is, for example, 3 to 90% by mass with respect to 100% by mass of the outer layer 2. The content is preferably 5 to 85 mass%, more preferably 10 to 80 mass%. The lower limit or more improves the flame retardancy, and the upper limit or less suppresses the change in the resistance value.
The thickness of the outer layer 1 is not particularly limited, and is, for example, 10 to 300. Mu.m. The thickness of the outer layer 1 is preferably 15 to 200 μm, and more preferably 20 to 150 μm, from the viewpoint of improving flame retardancy and flexibility and being suitable for arrangement in a minute space.
The thickness of the outer layer 2 is not particularly limited, and is, for example, 10 to 300. Mu.m. The thickness of the outer layer 1 is preferably 15 to 200 μm, and more preferably 20 to 150 μm from the viewpoints of flame retardancy and suitability for arrangement in a minute space.
In one embodiment of the present invention, the integral value of the endothermic amount of the adhesive layer 1a or the adhesive layer 1c in the range of 200 to 400 ℃ is preferably 9000 μ V · s/mg or more from the viewpoint of improving flame retardancy. In particular, in the structure including the adhesive layer 1a and the adhesive layer 1c, the integrated value of the endothermic amounts of the adhesive layer 1a and the adhesive layer 1c in the range of 200 to 400 ℃ is more preferably 9000 μ V · s/mg or more from the viewpoint of improving flame retardancy. The integral value is preferably 9500. Mu.V.s/mg or more, more preferably 10000. Mu.V.s/mg or more. The upper limit is, for example, 20000. Mu.V.s/mg, 18000. Mu.V.s/mg or 15000. Mu.V.s/mg. The integrated value is measured as follows. Specifically, the integral value of the endothermic peak at a temperature of 200 ℃ to 400 ℃ can be calculated by using TG-DTA.
The layer constitution of the outer layer is not particularly limited. The outer layer may be composed of 1 kind of single outer layer, or may be composed of 2 or more kinds of layers.
In one embodiment of the present invention, the outer layer 2 preferably includes an adhesive layer 2a and a sheet layer 2b, and the adhesive layer 2a and the sheet layer 2b are laminated in this order from the conductive fiber sheet side. In this configuration, while the sheet layer 2b exhibits flame retardancy, the transfer of the flame retardant in the sheet layer 2b to the conductive fiber sheet is suppressed through the adhesive layer 2a, and the change in resistance value can be suppressed.
The adhesive layer 2a is not particularly limited as long as it contains a binder resin. From the viewpoint of suppressing the change in the resistance value, the content of the flame retardant or the total content of the phosphorus-based flame retardant and the inorganic flame retardant in the adhesive layer 2a is, for example, 0 to 40% by mass, preferably 0 to 20% by mass, more preferably 0 to 10% by mass, and particularly preferably no flame retardant is contained in the adhesive layer 2a, relative to 100% by mass of the adhesive layer 2 a.
The sheet layer 2b is not particularly limited as long as it contains a binder resin and a phosphorus-based flame retardant. The content of the flame retardant in the sheet layer 2b or the total content of the phosphorus-based flame retardant and the inorganic flame retardant is, for example, 15 to 95 mass%, preferably 40 to 90 mass%, and more preferably 65 to 85 mass% with respect to 100 mass% of the sheet layer 2b. The lower limit or more improves the flame retardancy, and the upper limit or less suppresses the change in the resistance value.
In this configuration, the outer layer 1 is preferably an adhesive layer. That is, the outer layer 1 (adhesive layer), the conductive fiber sheet, the adhesive layer 2a, and the sheet layer 2b are preferably laminated in this order from the outer layer 1 side.
In this configuration, when the outer layer 1 is an adhesive layer, the content of the phosphorus-based flame retardant in the adhesive layer is, for example, 5 to 80% by mass with respect to 100% by mass of the adhesive layer. The content is preferably 10 to 70% by mass, more preferably 15 to 65% by mass, still more preferably 17.5 to 60% by mass, and particularly preferably 20 to 40% by mass. The lower limit or more improves the flame retardancy, and the upper limit or less suppresses the change in the resistance value.
In one embodiment of the present invention, the outer layer 1 preferably further includes an adhesive layer 1a and a sheet layer 1b. That is, it is preferable to laminate the sheet layer 1b, the adhesive layer 1a, the conductive fiber sheet, the adhesive layer 2a, and the sheet layer 2b in this order from the outer layer 1 side. In this configuration, the sheet layer 1b can further exhibit flame retardancy.
In this structure, the adhesive layer 1a is not particularly limited as long as it contains a binder resin. From the viewpoint of suppressing the change in the resistance value, the content of the flame retardant or the total content of the phosphorus flame retardant and the inorganic flame retardant in the adhesive layer 1a is, for example, 0 to 60 mass%, preferably 0 to 50 mass%, more preferably 0 to 40 mass%, and particularly preferably no flame retardant is contained, with respect to 100 mass% of the adhesive layer 1a.
In this structure, the sheet layer 1b is not particularly limited as long as it contains a binder resin. The content of the flame retardant in the sheet layer 1b or the total content of the phosphorus flame retardant and the inorganic flame retardant is, for example, 0 to 95 mass%, preferably 5 to 90 mass%, and more preferably 25 to 85 mass% with respect to 100 mass% of the sheet layer 1b. The lower limit or more improves the flame retardancy, and the upper limit or less suppresses the change in the resistance value.
In one embodiment of the present invention, the outer layer 1 preferably further includes an adhesive layer 1a, a sheet layer 1b, and an adhesive layer 1c. That is, it is preferable to laminate the adhesive image 1c, the sheet layer 1b, the adhesive layer 1a, the conductive fiber sheet, the adhesive layer 2a, and the sheet layer 2b in this order from the outer layer 1 side. In this configuration, while further exhibiting flame retardancy by at least one of the sheet layer 1b and the adhesive layer 1c, the adhesive layer 1c can be attached to a component such as an electronic device while suppressing a change in resistance value due to a flame retardant through the adhesive layer 1 a.
In this structure, the adhesive layer 1a is not particularly limited as long as it contains a binder resin. From the viewpoint of suppressing the change in the resistance value, the content of the flame retardant or the total content of the phosphorus-based flame retardant and the inorganic flame retardant in the adhesive layer 1a is, for example, 0 to 60 mass%, preferably 0 to 50 mass%, more preferably 0 to 40 mass%, further preferably 0 to 35 mass%, and particularly preferably no flame retardant is contained, with respect to 100 mass% of the adhesive layer 1a.
In this structure, the sheet layer 1b is not particularly limited as long as it contains a binder resin. The content of the flame retardant in the sheet layer 1b or the total content of the phosphorus-based flame retardant and the inorganic flame retardant is, for example, 0 to 95 mass%, preferably 5 to 90 mass%, and more preferably 25 to 85 mass% with respect to 100 mass% of the sheet layer 1b. The lower limit or more improves the flame retardancy, and the upper limit or less suppresses the change in the resistance value.
The adhesive layer 1c is not particularly limited as long as it contains an adhesive binder resin, a phosphorus flame retardant and an inorganic flame retardant. The content of the flame retardant or the total content of the phosphorus flame retardant and the inorganic flame retardant in the adhesive layer 1c is, for example, 5 to 95% by mass, preferably 10 to 90% by mass, more preferably 15 to 85% by mass, and still more preferably 20 to 80% by mass, relative to 100% by mass of the adhesive layer 1c. The lower limit or more improves the flame retardancy, and the upper limit or less suppresses the change in the resistance value.
The thickness of the adhesive layer 2a is not particularly limited. From the viewpoint of adhesion, it is preferably 3 μm or more, more preferably 5 μm or more, still more preferably 10 μm or more, and still more preferably 15 μm or more. The thickness of the adhesive layer 2a is, for example, 150 μm or less, 100 μm or less, or 50 μm or less from the viewpoint of flame retardancy and suitability for arrangement in a minute space.
The thickness of the sheet layer 2b is not particularly limited. From the viewpoint of flame retardancy, it is preferably 10 μm or more, more preferably 15 μm or more, still more preferably 20 μm or more, and still more preferably 25 μm or more. The sheet layer 2b has a thickness of, for example, 100 μm or less, 80 μm or less, or 50 μm or less, from the viewpoint of being suitable for arrangement in a minute space.
The thickness of the adhesive layer 1a is not particularly limited. From the viewpoint of adhesion, it is preferably 5 μm or more, more preferably 10 μm or more, and still more preferably 20 μm or more. From the viewpoint of being suitable for being disposed in a small space, the thickness of the adhesive layer 1a is, for example, 150 μm or less, 100 μm or less, or 50 μm or less.
<3. Layer constitution >
The radio wave absorbing sheet of the present invention is not particularly limited as long as it includes the outer layer 1, the conductive fiber sheet, and the outer layer 2, and the outer layer 1, the conductive fiber sheet, and the outer layer 2 are laminated in this order. These 3 layers may be disposed adjacent to each other or with other layers interposed therebetween, and are preferably disposed adjacent to each other (without interposing other layers therebetween).
The thickness of the radio wave absorption sheet of the present invention is, for example, 50 to 1000. Mu.m. The thickness is preferably 80 to 800. Mu.m, more preferably 100 to 500. Mu.m. The lower limit or more improves the flame retardancy, and the upper limit or less is suitable for arrangement in a small space.
<4. Characteristics >
The radio wave absorbing sheet of the present invention has flame retardancy and can suppress the change in surface resistance.
Regarding flame retardancy, in a preferred embodiment of the present invention, the radio wave absorption sheet of the present invention is preferably V-2, V-1 or V-0, more preferably V-1 or V-0, and still more preferably V-0 in a test according to the UL94 vertical burning test.
In a preferred embodiment of the present invention, the surface resistance value (R11) after exposing the electric wave absorption sheet of the present invention to an atmosphere of 85 ℃ and 85% rh for 200 hours and the surface resistance value (R10) before the endurance test are measured in accordance with the above "(2-1) measurement of the surface resistance", and the rate of change in the surface resistance value (R1) is calculated by the following formula (1).
R1= (R11-R10)/R10X 100. Formula (1)
The rate of change in the surface resistance value after the durability test is preferably 50% or less, more preferably 30% or less, and still more preferably less than 15%.
<5 > production method
The radio wave absorbing sheet of the present invention can be obtained, for example, by a method including the steps of: a step of obtaining a conductive fiber sheet by adhering a metal, a barrier layer component, and the like to the surface of a fiber base material; and a step of laminating the layers including the conductive fiber sheet and the outer layer.
The adhesion is not particularly limited, and may be performed by, for example, a sputtering method, a vacuum evaporation method, an ion plating method, a chemical evaporation method, a pulsed laser deposition method, or the like. Among these, sputtering is preferred from the viewpoint of film thickness controllability, radio wave absorption characteristics, and the like.
The sputtering method is not particularly limited, and examples thereof include dc magnetron sputtering, high-frequency magnetron sputtering, and ion beam sputtering. The sputtering apparatus may be of a batch type or a Roll-to-Roll (Roll-to-Roll) type.
In the case of deposition by sputtering, the gradient of the amount of metal deposited on the surface and inside thereof can be adjusted by the gas pressure during sputtering. By reducing the gas pressure during sputtering, the metal can be attached to a deeper part inside the fiber base material, and can be distributed with a gentle gradient. This further improves the radio wave absorbability.
The method for forming the outer layer in the present invention is not particularly limited. Examples thereof include press molding, injection molding, extrusion molding, calender molding, roll molding, doctor blade molding, printing, coating, impregnation, and transfer.
The method of laminating the layers including the conductive fiber sheet and the outer layer is not particularly limited. For example, a method of laminating layers by utilizing the bondability of the outer layer or the bonding layer in the outer layer can be given.
<6 > use
The radio wave absorption sheet of the present invention has a performance of absorbing unnecessary electromagnetic waves in one aspect thereof, and therefore can be suitably used as a radio wave countermeasure component in, for example, an optical transceiver and a next-generation mobile communication system (5G). In addition, as another application, the present invention may be applied to a millimeter wave radar used in an advanced road traffic system (ITS) or a vehicle collision prevention system for performing information communication between vehicles, roads, and people for the purpose of radio interference suppression and noise reduction. The frequency of the radio wave to be targeted by the radio wave absorbing sheet of the present invention is, for example, 0.1GHz to 150GHz, preferably 0.5GHz to 85GHz, and more preferably 1GHz to 40 GHz.
The object to be radio wave-absorbed is not particularly limited. Examples of the object to be radio wave-absorbed include electronic components such as LSIs, circuit surfaces such as glass epoxy boards and FPCs, inner surfaces thereof, connection cables and connector portions between components, inner surfaces or outer surfaces of cases and holders in which electronic components and devices are mounted, and cables such as power supply lines and transmission lines.
In one embodiment of the radio wave absorbing sheet of the present invention, the radio wave absorbing sheet can be used by covering the periphery of a radio wave absorbing object. Therefore, the molding can be appropriately performed according to the shape of the object. In the present specification, the "radio wave absorbing compact" also means a formed product.
The radio wave absorbing sheet of the present invention is used to cover the periphery of the radio wave absorbing object by being disposed at a position away from the generation source of the radio wave noise, and can more effectively exhibit the performance of absorbing unnecessary radio wave noise. Further, by being disposed at a position distant from the source of generation of radio wave noise, heat dissipation from heat generated from the LSI or the like is not easily hindered. The radio wave absorbing sheet of the present invention is preferably disposed at a position λ/2 π or more away from the source of radio wave noise from the viewpoint of radio wave absorption. λ represents the wavelength of the radio wave to be detected. Further, in the case where radio wave noise is generated inside the case, the case itself may be referred to as a radio wave noise source due to the cavity resonance phenomenon. By disposing the radio wave absorbing sheet of the present invention on the inner wall of the case, the cavity resonance phenomenon can be suppressed, and the generation of noise from the case can be suppressed. A case having the radio wave absorbing sheet of the present invention on the inner surface thereof and an electronic device having the case are also one embodiment of the present invention.
In one embodiment of the radio wave absorbing sheet of the present invention, when a case housing an electronic device or the like has an opening, the radio wave absorbing sheet is attached to the opening, whereby a case having excellent radio wave absorption properties can be obtained. When a case in which an electronic device or the like is built has an opening, radio noise generated from the electronic device inside leaks from the opening, or the opening functions as an antenna and the radio noise is re-radiated. In such a case, by disposing the radio wave absorbing sheet of the present invention in the opening of the case, noise emitted from the case can be reduced. A case having the radio wave absorbing sheet of the present invention in an opening of the case and an electronic device having the case are also one embodiment of the present invention.
Examples
The present invention will be described in detail below based on examples, but the present invention is not limited to these examples.
(1) Production of radio wave absorbing sheet
(example 1)
A nonwoven fabric (melt blown, thickness 25 μm, basis weight 6 g/m) composed of PAR as a fiber base material was used 2 ) Is arranged in a vacuum device, and is vacuum-exhausted to be less than 5.0 x 10 < -4 > Pa. Next, argon gas was introduced to a gas pressure of 0.5Pa, and a metal layer was formed by sequentially laminating a barrier layer 1 (base layer) made of silicon, a conductive layer made of hastelloy (C-276, manufactured by yohimoto corporation), and a barrier layer 2 (surface layer) made of silicon on one surface of the fiber base material by a DC magnetron sputtering method, thereby obtaining a conductive fiber sheet.
The fiber base side of the obtained conductive fiber sheet was bonded to the outer layer 1 (3 sheets having a thickness of 50 μm manufactured by 808080nr. The outer layer 2 was formed of an adhesive layer 2a (double-sided adhesive tape: acrylic 100%, thickness 50 μm) and a sheet layer 2b (binder resin: PVB15%, flame retardant: aluminum phosphite 85%, thickness 50 μm) as shown in Table 1.
(examples 2 and 10)
A radio wave absorbing sheet was obtained in the same manner as in example 1, except that the thickness of the barrier layer in the conductive fiber sheet was changed.
(examples 3 and 4)
A radio wave absorbing sheet was obtained in the same manner as in example 1, except that the thickness of the sheet layer 2b in the outer layer 2 was changed.
(examples 5 to 7)
A radio wave absorbing sheet was obtained in the same manner as in example 1, except that the thickness of the adhesive layer 2a in the outer layer 2 was changed.
(example 8)
A radio wave absorbing sheet was obtained in the same manner as in example 1, except that the configuration of the outer layer 2 was changed to that of the adhesive layer 2a (double-sided adhesive tape: 8810NR-TD, produced by DIC corporation, thickness 150 μm).
(example 9)
A radio wave absorbing sheet was obtained in the same manner as in example 1, except that the conductive layer in the conductive fiber sheet was changed.
(example 11)
An electric wave absorbing sheet was obtained in the same manner as in example 1, except that the flame retardant content and the thickness of the sheet layer 2b in the outer layer 2 were changed.
(examples 12 to 18)
An electric wave absorption sheet was obtained in the same manner as in example 1, except that the amount of adhesion of the conductive layer in the conductive fiber sheet was changed.
(example 19)
A radio wave absorbing sheet was obtained in the same manner as in example 1, except that the structure of the outer layer 1 was changed to an adhesive layer 1a (double-sided adhesive tape: 8080NR manufactured by DIC having a thickness of 50 μm), a sheet layer 1b (nonwoven fabric: PET100% and a thickness of 50 μm), and an adhesive layer 1c (double-sided adhesive tape: 8080NR manufactured by DIC having a thickness of 50 μm).
(example 20)
A radio wave absorbing sheet was obtained in the same manner as in example 1, except that the structure of the outer layer 1 was changed to an adhesive layer 1a (double-sided adhesive tape: acrylic 100% with a thickness of 10 μm), a sheet layer 1b (adhesive resin: PVB15%, flame retardant: aluminum phosphite 85%, thickness 50 μm), and an adhesive layer 1c (double-sided adhesive tape: 8080NR manufactured by DIC corporation, thickness 50 μm).
(example 21)
A radio wave absorbing sheet was obtained in the same manner as in example 1 except that the configuration of the outer layer 1 was changed to an adhesive layer 1a (double-sided adhesive tape: 8080NR manufactured by DIC corporation, thickness 50 μm), a sheet layer 1b (adhesive resin: 15% PVB, flame retardant: aluminum phosphite 85%, thickness 50 μm), and an adhesive layer 1c (double-sided adhesive tape: 8080NR manufactured by DIC corporation, thickness 50 μm).
(example 22)
A radio wave absorbing sheet was obtained in the same manner as in example 1, except that the structure of the outer layer 1 was changed to the adhesive layer 1a (double-sided adhesive tape: 8080NR manufactured by DIC corporation, thickness 50 μm) and the sheet layer 1b (binder resin: PVB15%, flame retardant: aluminum phosphite 85%, thickness 50 μm).
Comparative examples 1 and 2
A radio wave absorbing sheet was obtained in the same manner as in example 1, except that the flame retardant and the thickness in the outer layer 1 were changed.
Comparative example 3
A radio wave absorbing sheet was obtained in the same manner as in example 1, except that the sheet layer 2b in the outer layer 2 was changed to a film (Torrelina, toray corporation, binder resin: PPS, thickness 125 μm).
Comparative example 4
A radio wave absorbing sheet was obtained in the same manner as in example 1, except that the sheet layer 2b in the outer layer 2 was changed to a nonwoven fabric (FBBK 6F, manufactured by Coli, binder resin: PAR, thickness 25 μm).
(2) Evaluation of
Various performances of the obtained radio wave absorbing sheet were evaluated.
(2-1) measurement of endothermic integral value
The measurement was carried out using TG-DTA (Thermo plus EVO2, manufactured by RIGAKU Co., ltd.) under the following conditions, and an integrated value (. Mu.V.s/mg) was calculated from an endothermic peak at a temperature of 200 to 400 ℃ on the basis of 0. Mu.V.s/mg.
(measurement conditions of the differential Heat balance)
Measurement of atmosphere: air 100mL/min
Sample size: 10mg of
Measurement temperature: 30 ℃→ 800 ℃
Temperature rise conditions: 10 ℃/min.
(2-2) measurement of surface resistance
The surface resistance values of the conductive fiber sheet and the radio wave absorption sheet were measured at room temperature by the eddy current method using a non-contact resistance measuring instrument (EC-80P manufactured by NAPSON corporation) (Ω/\9633;). The conductive fiber sheet is measured from the metal layer side, and the radio wave absorbing sheet is measured from the outer layer 2 side.
(2-3) evaluation of durability
The wet heat resistance test was performed as follows, and the durability was evaluated.
In accordance with the above "(2-1) measurement of surface resistance", the surface resistance value (R11) after exposing the radio wave absorption sheet to an atmosphere of 85 ℃ and 85% rh for 200 hours and the surface resistance value (R10) before the durability test were measured, and the surface resistance value change rate (R1) was calculated by the following formula (1).
R1= (R11-R10)/R10X 100. The formula (1)
Evaluation was evaluated based on the value of R1 by the following criteria.
Very good: r1 is less than 15 percent.
O: r1 is more than 15% and less than 50%.
X: r1 is greater than 50%.
(2-4) evaluation of flame retardance
The flame retardance was evaluated by conducting a flame test in accordance with UL standards (UL 94:20mm flame vertical burning test).
(2-5) comprehensive evaluation
The flame retardancy and durability were evaluated by the following criteria.
O: the flame retardance was V-1 or V-0, and the durability was evaluated as O or X.
X: the flame retardance was not V-2 and/or the durability was evaluated as X.
(3) Results
The overall structure of the radio wave absorbing sheet including the respective layers and the laminate, and the evaluation results are shown in tables 1 to 12.
[ Table 7]
[ Table 8]
[ Table 9]
[ Table 10]
[ Table 11]
[ Table 12]
1. Metal layer
2. Fibrous substrate
3. Conductive layer
4. Barrier layer
5. Conductive fiber sheet
6. Outer layer 1
7. Outer layer 2
8. Adhesive layer 2a
9. Sheet layer 2b
10. Adhesive layer 1a
11. Sheet layer 1b
12. Adhesive layer 1c
Claims (18)
1. An electric wave absorption sheet comprises an outer layer 1, a conductive fiber sheet, and an outer layer 2,
and an outer layer 1, a conductive fiber sheet, and an outer layer 2 are laminated in this order,
the outer layer 1 contains a binder resin, a phosphorus flame retardant and an inorganic flame retardant, and
the outer layer 2 contains a binder resin, a phosphorus flame retardant, and an inorganic flame retardant.
2. The electric wave absorption sheet according to claim 1, wherein,
the outer layer 2 comprises an adhesive layer 2a and a sheet layer 2b,
the adhesive layer 2a and the sheet layer 2b are laminated in this order from the conductive fiber sheet side.
3. The electric wave absorption sheet according to claim 2, wherein,
the total content of the flame retardant in the adhesive layer 2a is 0 to 40 mass% with respect to 100 mass% of the adhesive layer 2a.
4. The electric wave absorption sheet according to claim 2 or 3, wherein,
the total content of the flame retardant in the sheet layer 2b is 40 to 90% by mass with respect to 100% by mass of the sheet layer 2b.
5. The electric wave absorption sheet according to any one of claims 1 to 4,
the outer layer 1 is an adhesive layer.
6. The radio wave absorption sheet according to any one of claims 2 to 4,
the outer layer 1 comprises an adhesive layer 1a and a sheet layer 1b,
the adhesive layer 1a and the sheet layer 1b are laminated in this order from the conductive fiber sheet side.
7. The electric wave absorption sheet according to claim 6, wherein,
the total content of the flame retardant in the adhesive layer 1a is 0 to 50 mass% with respect to 100 mass% of the adhesive layer 1a.
8. The electric wave absorption sheet according to claim 6 or 7, wherein,
the total content of the flame retardant in the sheet layer 1b is 50 to 90% by mass with respect to 100% by mass of the sheet layer 1b.
9. The radio wave absorption sheet according to any one of claims 6 to 8,
the outer layer 1 comprises an adhesive layer 1a, a sheet layer 1b and an adhesive layer 1c,
the adhesive layer 1a, the sheet layer 1b, and the adhesive layer 1c are laminated in this order from the conductive fiber sheet side.
10. The electric wave absorption sheet according to claim 9, wherein,
the total content of the flame retardant in the adhesive layer 1c is 10 to 90 mass% with respect to 100 mass% of the adhesive layer 1c.
11. The radio wave absorption sheet according to any one of claims 1 to 10,
the inorganic flame retardant contained in at least one of the outer layer 1 or the outer layer 2 contains an aluminum component.
12. The electric wave absorption sheet according to any one of claims 6 to 11, wherein,
an integrated value of an endothermic quantity in a range of 200 to 400 ℃ of at least one of the adhesive layer 1a and the adhesive layer 1c is 9000 μ V · s/mg or more.
13. The radio wave absorption sheet according to any one of claims 1 to 12, wherein,
the conductive fiber sheet comprises: the metal layer is configured on at least one surface of the fiber base material.
14. The electric wave absorption sheet according to claim 13, wherein,
the metal layer includes: the conductive layer and the barrier layer are arranged on at least one surface of the conductive layer.
15. The electric wave absorption sheet according to claim 13 or 14, wherein,
the surface resistance value of the metal layer is 40-500 omega/\9633;.
16. The electric wave absorption sheet according to any one of claims 13 to 15, wherein,
the metal layer includes: at least 1 metal element selected from the group consisting of nickel, molybdenum, chromium, titanium, copper, and aluminum.
17. The electric wave absorption sheet according to any one of claims 1 to 16, which has a thickness of 100 to 500 μm.
18. The electric wave absorbing sheet according to any one of claims 1 to 17, which has a flame retardancy of V-0 or V-1 in a test according to UL94 vertical burning test.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2020-137479 | 2020-08-17 | ||
| JP2020137479 | 2020-08-17 | ||
| PCT/JP2021/029946 WO2022039132A1 (en) | 2020-08-17 | 2021-08-16 | Radio wave absorbing sheet |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN115211244A true CN115211244A (en) | 2022-10-18 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202180017971.5A Pending CN115211244A (en) | 2020-08-17 | 2021-08-16 | Radio wave absorbing sheet |
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| Country | Link |
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| JP (1) | JPWO2022039132A1 (en) |
| CN (1) | CN115211244A (en) |
| WO (1) | WO2022039132A1 (en) |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4638217B2 (en) * | 2004-01-16 | 2011-02-23 | 大京化学株式会社 | Flame retardant metal coated fabric |
| JP2007203726A (en) * | 2006-02-01 | 2007-08-16 | Nippon Jitsupaa Chiyuubingu Kk | Flame retardant metal-clad fabric and metal-clad sheet |
| JP2008100479A (en) * | 2006-10-20 | 2008-05-01 | Seiren Co Ltd | Flame-retardant metal-coated cloth |
| CN113165339A (en) * | 2018-11-30 | 2021-07-23 | 积水化学工业株式会社 | Conductive nonwoven fabric |
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- 2021-08-16 WO PCT/JP2021/029946 patent/WO2022039132A1/en active Application Filing
- 2021-08-16 CN CN202180017971.5A patent/CN115211244A/en active Pending
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| JPWO2022039132A1 (en) | 2022-02-24 |
| WO2022039132A1 (en) | 2022-02-24 |
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Application publication date: 20221018 |