WO2014007277A1 - 積層体 - Google Patents
積層体 Download PDFInfo
- Publication number
- WO2014007277A1 WO2014007277A1 PCT/JP2013/068222 JP2013068222W WO2014007277A1 WO 2014007277 A1 WO2014007277 A1 WO 2014007277A1 JP 2013068222 W JP2013068222 W JP 2013068222W WO 2014007277 A1 WO2014007277 A1 WO 2014007277A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- silicon
- group
- metal salt
- nitrogen
- atoms
- Prior art date
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 91
- 229910052751 metal Inorganic materials 0.000 claims abstract description 85
- 239000002184 metal Substances 0.000 claims abstract description 85
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 78
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 75
- 239000010703 silicon Substances 0.000 claims abstract description 71
- 229920001709 polysilazane Polymers 0.000 claims abstract description 69
- 150000003839 salts Chemical class 0.000 claims abstract description 63
- 229920000642 polymer Polymers 0.000 claims abstract description 59
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 54
- 150000007524 organic acids Chemical class 0.000 claims abstract description 48
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 41
- 239000001301 oxygen Substances 0.000 claims abstract description 41
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 41
- 125000004433 nitrogen atom Chemical group N* 0.000 claims abstract description 36
- 125000004430 oxygen atom Chemical group O* 0.000 claims abstract description 20
- 125000004432 carbon atom Chemical group C* 0.000 claims abstract description 7
- -1 carboxylic acid compound Chemical class 0.000 claims description 77
- 239000007789 gas Substances 0.000 claims description 62
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 49
- 238000000034 method Methods 0.000 claims description 46
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- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 34
- 238000000576 coating method Methods 0.000 claims description 27
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 22
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 claims description 17
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 16
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- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 4
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- 229910052725 zinc Inorganic materials 0.000 claims description 4
- JAHNSTQSQJOJLO-UHFFFAOYSA-N 2-(3-fluorophenyl)-1h-imidazole Chemical compound FC1=CC=CC(C=2NC=CN=2)=C1 JAHNSTQSQJOJLO-UHFFFAOYSA-N 0.000 claims description 3
- XEEYSDHEOQHCDA-UHFFFAOYSA-N 2-methylprop-2-ene-1-sulfonic acid Chemical compound CC(=C)CS(O)(=O)=O XEEYSDHEOQHCDA-UHFFFAOYSA-N 0.000 claims description 3
- 125000003504 2-oxazolinyl group Chemical group O1C(=NCC1)* 0.000 claims description 3
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- PXQLVRUNWNTZOS-UHFFFAOYSA-N sulfanyl Chemical class [SH] PXQLVRUNWNTZOS-UHFFFAOYSA-N 0.000 claims 1
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- RPACBEVZENYWOL-XFULWGLBSA-M sodium;(2r)-2-[6-(4-chlorophenoxy)hexyl]oxirane-2-carboxylate Chemical compound [Na+].C=1C=C(Cl)C=CC=1OCCCCCC[C@]1(C(=O)[O-])CO1 RPACBEVZENYWOL-XFULWGLBSA-M 0.000 description 1
- FWFUWXVFYKCSQA-UHFFFAOYSA-M sodium;2-methyl-2-(prop-2-enoylamino)propane-1-sulfonate Chemical compound [Na+].[O-]S(=O)(=O)CC(C)(C)NC(=O)C=C FWFUWXVFYKCSQA-UHFFFAOYSA-M 0.000 description 1
- PNGLEYLFMHGIQO-UHFFFAOYSA-M sodium;3-(n-ethyl-3-methoxyanilino)-2-hydroxypropane-1-sulfonate;dihydrate Chemical compound O.O.[Na+].[O-]S(=O)(=O)CC(O)CN(CC)C1=CC=CC(OC)=C1 PNGLEYLFMHGIQO-UHFFFAOYSA-M 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- JBQYATWDVHIOAR-UHFFFAOYSA-N tellanylidenegermanium Chemical compound [Te]=[Ge] JBQYATWDVHIOAR-UHFFFAOYSA-N 0.000 description 1
- KKEYFWRCBNTPAC-UHFFFAOYSA-L terephthalate(2-) Chemical compound [O-]C(=O)C1=CC=C(C([O-])=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-L 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
- 239000010409 thin film Substances 0.000 description 1
- RYYWUUFWQRZTIU-UHFFFAOYSA-K thiophosphate Chemical compound [O-]P([O-])([O-])=S RYYWUUFWQRZTIU-UHFFFAOYSA-K 0.000 description 1
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical class Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 description 1
- ODHXBMXNKOYIBV-UHFFFAOYSA-N triphenylamine Chemical compound C1=CC=CC=C1N(C=1C=CC=CC=1)C1=CC=CC=C1 ODHXBMXNKOYIBV-UHFFFAOYSA-N 0.000 description 1
- YFTHZRPMJXBUME-UHFFFAOYSA-N tripropylamine Chemical compound CCCN(CCC)CCC YFTHZRPMJXBUME-UHFFFAOYSA-N 0.000 description 1
- LENZDBCJOHFCAS-UHFFFAOYSA-N tris Chemical compound OCC(N)(CO)CO LENZDBCJOHFCAS-UHFFFAOYSA-N 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 239000011882 ultra-fine particle Substances 0.000 description 1
- 239000006097 ultraviolet radiation absorber Substances 0.000 description 1
- 229920006305 unsaturated polyester Polymers 0.000 description 1
- 229940005605 valeric acid Drugs 0.000 description 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 1
- 238000001947 vapour-phase growth Methods 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
- UGZADUVQMDAIAO-UHFFFAOYSA-L zinc hydroxide Chemical compound [OH-].[OH-].[Zn+2] UGZADUVQMDAIAO-UHFFFAOYSA-L 0.000 description 1
- 229940007718 zinc hydroxide Drugs 0.000 description 1
- 229910021511 zinc hydroxide Inorganic materials 0.000 description 1
- XKMZOFXGLBYJLS-UHFFFAOYSA-L zinc;prop-2-enoate Chemical compound [Zn+2].[O-]C(=O)C=C.[O-]C(=O)C=C XKMZOFXGLBYJLS-UHFFFAOYSA-L 0.000 description 1
Images
Classifications
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Definitions
- transparent gas barrier materials that block gases such as oxygen and water vapor have been used not only for packaging materials such as food and pharmaceuticals, which are the main applications of the past, but also for flat panel displays (FPD) such as liquid crystal displays and solar cells. It has come to be used also for electronic members, such as a member (a board
- transparent gas barrier materials employed in some applications include silicon and aluminum oxides that exhibit gas barrier properties by dry processes such as vapor deposition, plasma CVD, sputtering, ion plating, and catalytic CVD, There are techniques for depositing nitrides, and mixtures thereof, on plastic substrates. However, in the dry process, a minute defect called a part (pinhole) that is not partially deposited is formed, and the gas barrier property may be impaired.
- a water-soluble polymer and (a) one or more alkoxides and / or hydrolysates thereof are formed on a silicon or aluminum oxide, nitride, or mixture layer produced by a dry process.
- Lamination with an organic layer such as coating has been proposed, and an improvement in barrier properties of about an order of magnitude has been reported.
- the barrier performance is still insufficient for electronic member applications that require high gas barrier performance.
- An object of the present invention is to provide a laminate having sufficient gas barrier performance that can be used for an electronic member.
- the present inventors laminated a polysilazane film with a silicon-containing layer obtained by irradiating energy rays such as plasma under a predetermined condition and a polymer layer obtained from an organic acid metal salt. It has been found that a laminate having sufficient oxygen gas barrier performance and water vapor barrier performance with few defects such as pinholes and excellent in bending resistance can be obtained.
- the silicon-containing layer (B) has a high-concentration nitrogen region composed of silicon atoms and nitrogen atoms, or silicon atoms, nitrogen atoms, and oxygen atoms, or silicon atoms, nitrogen atoms, oxygen atoms, and carbon atoms, In the high nitrogen concentration region, the polysilazane film formed on the substrate (A) is irradiated with energy rays at an oxygen concentration of 5% or less and / or a relative humidity of 30% or less at a room temperature of 23 ° C.
- composition ratio of nitrogen atoms represented by the following formula (1) measured by X-ray photoelectron spectroscopy is in a range of 0.01 or more and 1 or less.
- Formula (1) Composition ratio of nitrogen atom / (composition ratio of oxygen atom + composition ratio of nitrogen atom)
- the polysilazane film is obtained by applying the polysilazane-containing solution to the base material by a method selected from a bar coating method, a roll coating method, a gravure coating method, a spray coating method, an air knife coating method, a spin coating method, and a dip coating method.
- the polymer layer (C) is an organic acid metal salt having the polymerizable group on the silicon-containing layer (B) having a high nitrogen concentration region formed on the substrate (A).
- polymerizable group is selected from vinyl group, epoxy group, mercapto group, ureido group, sulfide group, isocyanate group, amino group, hydroxyl group, halogen atom, oxazoline group, carbodiimide group or derivatives thereof
- the sulfonic acid compound is selected from vinyl sulfonic acid, allyl sulfonic acid, methallyl sulfonic acid, sulfonic acid acrylate, sulfonic acid acrylamide, sulfonic acid methacrylate, styrene sulfonic acid, and isoprene sulfonic acid.
- the laminated body of description [16] The laminate according to any one of [1] to [15], wherein the polymer layer (C) further includes a silane coupling agent.
- a member including an element selected from an organic electroluminescence element, an electronic paper display element, and a liquid crystal display element, and the polymer layer (C) are disposed so as to be on the member side [1] to [16]
- An electronic member comprising the laminate according to any one of the above.
- the polysilazane film is irradiated with energy rays at an oxygen concentration of 5% or less and / or a relative humidity of 30% or less at a room temperature of 23 ° C. to modify at least a part of the film, so that silicon atoms and nitrogen atoms, or silicon atoms and nitrogen atoms
- the manufacturing method of the laminated body containing this.
- a composition ratio of nitrogen atoms represented by the following formula (1) measured by X-ray photoelectron spectroscopy is in a range of 0.01 or more and 1 or less.
- Body manufacturing method [21] The method for manufacturing a laminate according to [20], wherein the plasma irradiation is performed in an atmospheric gas selected from an inert gas, a rare gas, and a reducing gas.
- a silicon-containing layer (B) modified by energy ray irradiation and a polymer layer (C) obtained from an organic acid metal salt having a polymerizable group are sequentially laminated on the substrate (A).
- a dense silicon-containing layer having excellent bending resistance and no pinholes can be obtained as compared with the conventional laminate of inorganic layer / organic layer, and has a high oxygen gas barrier property and water vapor sufficient for use in electronic members. Barrier properties can be provided.
- FIG. 1 is a schematic cross-sectional view of an electronic member using the laminate of the present invention.
- FIG. 2 is a diagram showing the XPS measurement result of the silicon-containing layer (B) obtained by performing the low-pressure plasma treatment in Example 1.
- the substrate (A) in the present invention is not particularly limited as long as it is a resin.
- polyolefins such as polyethylene, polypropylene, poly-4-methyl-1-pentene, and polybutene; cyclic olefin polymers; polyimide; polyethylene terephthalate, polybutylene
- polyesters such as terephthalate and polyethylene naphthalate
- polyamides such as nylon-6, nylon-66, polymetaxylene adipamide, polyphenylene sulfide, and mixtures thereof.
- the base material (A) in the present invention includes an ultraviolet absorber, an antioxidant, an antistatic agent, a surfactant, a pigment, a fluorescent brightening agent, and the like as long as the effects of the present invention are not impaired.
- the silicon-containing layer (B) has a high nitrogen concentration region obtained by irradiating the polysilazane film with energy rays and modifying at least a part of the polysilazane.
- the polysilazane film other than the region modified by the energy ray irradiation can react with the water vapor transmitted from the substrate (A) side after the energy ray irradiation, and can be changed to silicon oxide (SiO 2 ).
- the silicon-containing layer (B) is composed of a high nitrogen concentration region and a silicon oxide region. Due to the configuration of this high nitrogen concentration region / silicon oxide / resin base material, the silicon-containing layer (B) has a gas barrier property such as an oxygen barrier property and a water vapor barrier property in a single layer film such as SiO 2 or Si 3 N 4. It is superior compared.
- the silicon-containing layer (B) preferably has a thickness of 0.01 ⁇ m or more and 4.0 ⁇ m or less, more preferably 0.02 ⁇ m or more and 2.0 ⁇ m or less, and more preferably 0.05 ⁇ m or more and 1.0 ⁇ m or less.
- “atmosphere of low oxygen and / or low water vapor” means that oxygen and / or water vapor is not present at all, or the oxygen concentration is 5% or less, preferably 0.5% (5000 ppm) or less.
- the oxygen concentration is 0.05% (500 ppm) or less, more preferably, the oxygen concentration is 0.005% (50 ppm) or less, more preferably, the oxygen concentration is 0.002% (20 ppm) or less, and the relative humidity at a room temperature of 23 ° C. 30% or less, preferably 10% or less relative humidity, more preferably 0.5% or less, preferably 0.2% or less relative humidity, and more preferably 0.1% or less relative humidity.
- Energy irradiation can be performed in a pressure range of low pressure to atmospheric pressure of 0.1 Pa or more.
- the layer thickness of the silicon-containing layer (B) is 0.1 to 0.2 ⁇ m, and the high nitrogen concentration region is formed over the entire upper surface of the silicon-containing layer (B).
- the high nitrogen concentration region may be formed in a part near the upper surface of the silicon-containing layer (B).
- region may be formed over the whole layer of a silicon containing layer (B).
- the composition of the silicon-containing layer (B) is the same as that in the high nitrogen concentration region.
- the silicon-containing layer (B) formed by energy irradiation of the polysilazane film having a nitrogen high concentration region having such a composition is particularly excellent in mechanical properties such as oxygen barrier properties, gas barrier properties such as water vapor barrier properties, and scratch resistance. Excellent. That is, by having a nitrogen high concentration region having such a composition, the laminate has an excellent balance between improving barrier properties and improving mechanical properties.
- the high-concentration nitrogen region has a thickness of 0.001 ⁇ m or more and 0.2 ⁇ m or less, preferably 0.005 ⁇ m or more and 0.1 ⁇ m or less, and more preferably 0.01 ⁇ m or more and 0.1 ⁇ m or less. And preferred from the viewpoint of mechanical properties.
- the nitrogen high-concentration region may have a thickness in the above range in a part of the upper surface of the silicon-containing layer (B). It preferably has a thickness in the range.
- polysilazane one or a combination of two or more selected from perhydropolysilazane, organopolysilazane, and derivatives thereof can be used.
- the derivative include perhydropolysilazane or organopolysilazane in which part or all of hydrogen is substituted with an organic group such as an alkyl group or an oxygen atom.
- perhydropolysilazane represented by H 3 Si (NHSiH 2 ) n NHSiH 3 but organopolysilazane in which part or all of hydrogen is substituted with an organic group such as an alkyl group may be used. . Moreover, you may use by a single composition and may mix and use two or more components.
- the polysilazane-containing liquid may contain a metal carboxylate as a catalyst for converting polysilazane into a ceramic.
- the metal carboxylate is a compound represented by the following general formula. (RCOO) nM
- R represents an aliphatic group or alicyclic group having 1 to 22 carbon atoms
- M represents at least one metal selected from the following metal group
- n represents the valence of the metal M. .
- M is selected from the group of nickel, titanium, platinum, rhodium, cobalt, iron, ruthenium, osmium, palladium, iridium, and aluminum, and is particularly preferably palladium (Pd).
- the metal carboxylate may be an anhydride or a hydrate.
- the metal carboxylate / polysilazane weight ratio is preferably 0.001 to 1.0, more preferably 0.01 to 0.5.
- M is selected from the group of nickel, titanium, platinum, rhodium, cobalt, iron, ruthenium, osmium, palladium, iridium, and aluminum, and is particularly preferably palladium (Pd).
- the weight ratio of acetylacetonato complex / polysilazane is preferably 0.001 to 1.0, more preferably 0.01 to 0.5.
- amine compounds pyridines, DBU, DBN and the like and / or acid compounds such as organic acids and inorganic acids can be mentioned.
- R 4 R 5 R 6 N represents a hydrogen atom, an alkyl group, an alkenyl group, a cycloalkyl group, an aryl group, an alkylsilyl group, an alkylamino group, or an alkoxy group.
- amine compound examples include methylamine, dimethylamine, trimethylamine, ethylamine, diethylamine, triethylamine, propylamine, dipropylamine, tripropylamine, butylamine, dibutylamine, tributylamine, pentylamine, dipentylamine, tripentylamine, Examples include hexylamine, dihexylamine, trihexylamine, heptylamine, diheptylamine, triheptylamine, octylamine, dioctylamine, trioctylamine, phenylamine, diphenylamine, and triphenylamine.
- the hydrocarbon chain contained in these amine compounds may be a straight chain or a branched chain.
- Particularly preferred amine compounds are triethylamine, tripentylamine, tributylamine, trihexylamine, triheptylamine and trioctylamine.
- pyridines include pyridine, ⁇ -picoline, ⁇ -picoline, ⁇ -picoline, piperidine, lutidine, pyrimidine, pyridazine, DBU (1,8-diazabicyclo [5.4.0] -7-undecene), DBN (1,5-diazabicyclo [4.3.0] -5-nonene) and the like.
- the acid compound examples include organic acids such as acetic acid, propionic acid, butyric acid, valeric acid, maleic acid and stearic acid, and inorganic acids such as hydrochloric acid, nitric acid, sulfuric acid and hydrogen peroxide.
- organic acids such as acetic acid, propionic acid, butyric acid, valeric acid, maleic acid and stearic acid
- inorganic acids such as hydrochloric acid, nitric acid, sulfuric acid and hydrogen peroxide.
- Particularly preferred acid compounds are propionic acid, hydrochloric acid and hydrogen peroxide.
- a transition metal compound may be added to facilitate the reaction of polysilazane by irradiation with energy rays by acting on the Si—H bond of polysilazane and activating the bond state. As a result, by adding the transition metal compound, a high effect can be expected with a short irradiation.
- transition metal species of the above transition metal compounds platinum (Pt), ruthenium (Ru), rhodium (Rh), iridium (Ir), iron (Fe), osmium (Os), cobalt (Co), palladium (Pd ), Nickel (Ni), titanium (Ti), vanadium (V), chromium (Cr), manganese (Mn), molybdenum (Mo), tungsten (W), niobium (Nb), tantalum (Ta), zirconium (Zr) ), Hafnium (Hf), scandium (Sc), yttrium (Y), lanthanum (La), rhenium (Re), or a mixture thereof.
- transition metal compound a transition metal halide or complex, a transition metal salt or a transition metal oxide is used.
- the halide is a compound in which the transition metal is combined with chlorine (Cl), bromine (Br), iodine (I), or fluorine (F). All of the above transition metal halides can be used effectively, but more preferably, chloroplatinic acid (H 2 PtCl 6 .nH 2 O), PtCl 2 , PtCl 4 , PtCl 2 (NH 3 ) 2 , Na 2 (PtCl 4 ).
- the complex examples include an olefin complex, a cyclic olefin complex, a vinyl siloxane complex, a phosphine complex, a phosphite complex, a carbon monoxide complex (CO), an amine complex, and a nitrile complex.
- it is used mainly as a catalyst for the reaction between SiH groups and organic substances having a vinyl group and the like, and is known to facilitate the dissociation of Si—H bonds.
- the addition can facilitate the reaction of polysilazane by irradiation with energy rays.
- the transition metal salts include tetrafluoroboric acid (BF 4 ) salt, hexafluorophosphoric acid (PF 6 ) salt, hexafluoroantimonate, tetrakis (perfluorophenyl) borate, perchlorate and trifluoro It is a methyl sulfonic acid (CF 3 SO 3 ) salt.
- transition metal salt like above, more preferably, Rh (cyclooctadiene) 2 BF 4 , Pentametylcyclopentadienyltris (acetonitrile) RuPF 6, (Pentametylcyclopentadiene) 2 CoPF 6, La (CF 3 SO 3) 3, Sc (CF 3 SO 3 ) 3 , a mixture thereof, and the like can be given.
- the transition metal oxide is a compound in which one or more oxygen atoms are bonded to the transition metal.
- the weight ratio of transition metal compound / polysilazane is preferably 0.0001 to 1.0, more preferably 0.001 to 0.5, and still more preferably 0.01 to 0.2.
- the polysilazane-containing liquid can contain metal fine particles.
- a preferred metal is Ag.
- the particle size of the metal fine particles is preferably 0.5 ⁇ m or less, more preferably 0.1 ⁇ m or less, and even more preferably 0.05 ⁇ m or less.
- a polysilazane-containing liquid in which independently dispersed ultrafine particles having a particle size of 0.005 to 0.01 ⁇ m are dispersed in a high boiling alcohol is preferable.
- the addition amount of the metal fine particles is 0.01 to 10 parts by weight, preferably 0.05 to 5 parts by weight with respect to 100 parts by weight of polysilazane.
- polysilazane-containing liquid polysilazane, a catalyst used as necessary, metal fine particles, and the like are dissolved or dispersed in a solvent.
- the solvent examples include aromatic compounds such as benzene, toluene, xylene, ethylbenzene, diethylbenzene, trimethylbenzene, and triethylbenzene; n-pentane, i-pentane, n-hexane, i-hexane, n-heptane, and i-heptane.
- a known application method can be applied, and is not particularly limited.
- a bar coating method, a roll coating method, a gravure coating method, a spray coating method can be used.
- Air knife coating method, spin coating method, dip coating method and the like can be used.
- the polysilazane film is irradiated with energy rays in an atmosphere of low oxygen and / or low water vapor to modify at least part of the polysilazane film to form a silicon-containing layer (B) including a high nitrogen concentration region.
- the energy beam irradiation include plasma treatment, and a combination of these treatments can also be performed.
- a high nitrogen concentration region can be uniformly formed as compared with other energy beam irradiations, which is preferable in that the barrier property of the silicon-containing layer (B), in particular, the water vapor barrier property is excellent.
- Plasma treatment includes low pressure and near atmospheric pressure plasma. More preferably, low-pressure plasma is a preferred processing method.
- nitrogen gas that is an inert gas, argon gas that is a rare gas, helium gas, neon gas, krypton gas, xenon gas, and the like are reduced.
- the gas include hydrogen gas and ammonia gas. More preferable gas includes argon gas, helium gas, nitrogen gas, hydrogen gas, or a mixed gas thereof.
- Low pressure plasma treatment For low-pressure plasma, a known electrode or waveguide is placed in a vacuum closed system, and power such as direct current, alternating current, radio wave, or microwave is applied via the electrode or waveguide. Plasma can be generated. Power applied to the plasma treatment (W), the unit area of the electrode (cm 2) per preferably 0.0001W / cm 2 ⁇ 100W / cm 2, more preferably 0.001W / cm 2 ⁇ 50W / cm 2 is there.
- the plasma treatment can be performed under a low pressure corresponding to a low oxygen and / or low water vapor atmosphere.
- Low pressure means a pressure of 100 Pa or less, preferably a pressure of 10 Pa or less.
- the low-pressure state in the apparatus is that the pressure in the apparatus is reduced from atmospheric pressure (101325 Pa) to a pressure of 100 Pa or less, preferably 10 Pa or less using a vacuum pump such as a hydraulic rotary pump or a turbo molecular pump, and then the plasma gas Is introduced to a pressure of 100 Pa or less.
- the oxygen concentration and water vapor concentration under low pressure are generally evaluated by the oxygen partial pressure and the water vapor partial pressure.
- the nitrogen high-concentration region of this embodiment is not formed, and silanol groups (Si—OH) are generated, so that a sufficient water vapor barrier property may not be obtained. is there.
- the above-described plasma gas species are introduced and performed at a low gas pressure of 500 Pa to 0.1 Pa. More preferably, the plasma generation efficiency is good when performed at 100 Pa to 0.1 Pa.
- the opposed plate electrodes are a typical electrode structure.
- the electrode on the side to which the high-frequency power is applied is not limited to a flat plate shape, and may have an uneven shape.
- ICP Inductively coupled plasma
- a gas is passed between two electrodes, and this gas is turned into a plasma before irradiating the substrate (A), or a substrate with a polysilazane film irradiated between the two electrodes is arranged.
- the plasma gas flow rate is preferably as high as possible in order to obtain the low oxygen / low water vapor concentration atmosphere, preferably 0.01 to 1000 L / min, more preferably 0.1 to 500 L / min.
- the applied power (W), the unit area of the electrode (cm 2) per preferably 0.0001W / cm 2 ⁇ 100W / cm 2, more preferably 0.001W / cm 2 ⁇ 50W / Cm 2 .
- the moving speed of the substrate with a polysilazane film is preferably 0.001 to 1000 m / min, more preferably 0.001 to 500 m / min.
- the silicon-containing layer (B) in the present invention can be produced.
- An undercoat layer may be provided between the substrate (A) and the silicon-containing layer (B) in order to suppress oligomer and additive precipitation in the substrate (A).
- a layer in which a polymerizable monomer or oligomer having at least one vinyl group in the molecule is coated and a coat layer is formed by a crosslinking reaction by heating, ultraviolet rays, electron beams or the like is preferable. In particular, it is preferable to use ultraviolet rays or electron beams because of good reactivity.
- Epoxy (meth) acrylate compounds include bisphenol A type epoxy compounds, bisphenol F type epoxy compounds, bisphenol S type epoxy compounds, phenol novolac type epoxy compounds, cresol novolac type epoxy compounds, aliphatic epoxy compounds, and acrylic compounds and acrylics. Examples include compounds obtained by reacting acid or methacrylic acid, and acid-modified epoxy (meth) acrylates obtained by reacting these compounds with carboxylic acids or anhydrides thereof. These epoxy (meth) acrylate compounds are applied to the surface of the substrate (A) together with a photopolymerization initiator and, if necessary, a diluent made of other photopolymerization or heat-reactive monomers, and then ultraviolet rays, etc. And an undercoat layer is formed by a crosslinking reaction.
- Specific polyisocyanates include adducts of methylene bis (p-phenylene diisocyanate), hexamethylene diisocyanate / hexane triol, hexamethylene diisocyanate, tolylene diisocyanate, tolylene diisocyanate trimethylolpropane, 1,5- Examples include naphthylene diisocyanate, thiopropyl diisocyanate, ethylbenzene-2,4-diisocyanate, 2,4-tolylene diisocyanate dimer, hydrogenated xylylene diisocyanate, and tris (4-phenyl isocyanate) thiophosphate.
- Typical polyols include polyether polyols such as polyoxytetramethylene glycol, polyadipate polyols, and polycarbonate polyols. What polyester polyols, and the like copolymers of acrylic acid esters and hydroxyethyl methacrylate.
- monomers constituting the acrylate methyl (meth) acrylate, ethyl (meth) acrylate, butyl (meth) acrylate, 2 ethylhexyl (meth) acrylate, methoxyethyl (meth) acrylate, butoxyethyl (meth) acrylate, phenyl (Meth) acrylate and the like.
- epoxy (meth) acrylate compounds and urethane (meth) acrylate compounds are used in combination as necessary.
- Examples of a method for polymerizing these include various known methods, specifically, a method using irradiation with ionizing radiation or heating. When these are used after being cured with ultraviolet rays, acetophenones, benzophenones, mifilabenzoylbenzoate, ⁇ -amyloxime esters, thioxanthones, etc. are used as photopolymerization initiators, and n-butylamine, triethylamine, tri-n- It is preferable to use butyl phosphine or the like as a photosensitizer. In the present invention, the epoxy (meth) acrylate compound and the urethane (meth) acrylate compound are also used in combination.
- epoxy (meth) acrylate compounds and urethane (meth) acrylate compounds are diluted with (meth) acrylic monomers.
- acrylic monomers include methyl (meth) acrylate, ethyl (meth) acrylate, butyl (meth) acrylate, 2-ethylhexyl (meth) acrylate, methoxyethyl (meth) acrylate, and butoxyethyl (meth).
- undercoat layer when a urethane (meth) acrylate compound is used as the undercoat layer, it contributes to the improvement of the oxygen gas barrier property of the obtained gas barrier film.
- These undercoat layers are usually 0.05 to 5.0 g / m 2 , and 0.1 to 3.0 g / m 2 is particularly preferable.
- the surface of the silicon-containing layer (B) is preferably subjected to pretreatment such as corona treatment, glow discharge treatment, atmospheric pressure plasma treatment, and vacuum plasma discharge treatment before providing the metal salt polymer layer (C). . Of these, corona treatment is preferred.
- the conditions for the corona treatment are not particularly limited, but for example, the discharge frequency may be 5 to 40 kHz, especially about 10 to 30 kHz, and the waveform is, for example, an AC sine wave.
- the gap clearance between the electrode and the dielectric roll is set to 0.1 to 10 millimeters, particularly about 1.0 to 2.0 millimeters, and the processing amount is set to about 0.3 to 0.4 KV ⁇ A ⁇ minute / m 2 . You can also It is preferable in that it can be processed at normal pressure in air.
- the heat treatment temperature is preferably as high as possible, but considering the characteristics of the substrate, it is preferably in the range of 25 ° C. to 1000 ° C., more preferably 30 ° C. to 500 ° C., and even more preferably 60 ° C. to 300 ° C. .
- Additional processing By subjecting the silicon-containing layer (B) modified by the plasma treatment to irradiation of active energy rays or heat treatment, the high nitrogen concentration region in the silicon-containing layer (B) can be increased.
- active energy rays include microwaves, infrared rays, ultraviolet rays, and electron beams, and infrared rays, ultraviolet rays, and electron beams are preferable.
- Examples of the method for generating ultraviolet rays include, as described above, methods using a metal halide lamp, a high-pressure mercury lamp, a low-pressure mercury lamp, a xenon arc lamp, a carbon arc lamp, an excimer lamp, a UV light laser such as an Ar—F laser, and the like. It is done.
- a method for generating infrared rays for example, a method using an infrared radiator or an infrared ceramic heater can be mentioned. Also, when using an infrared radiator, depending on the wavelength used for infrared rays, a near-infrared radiator having an intensity peak at a wavelength of 1.3 ⁇ m, a mid-infrared radiator having an intensity peak at a wavelength of 2.5 ⁇ m, and a wavelength of 4.5 ⁇ m A far-infrared radiator having an intensity peak can be used.
- infrared laser having a single spectrum.
- infrared lasers include gas chemical lasers such as HF, DF, HCl, DCl, HBr, and DBr, CO 2 gas lasers, N 2 O gas lasers, CO 2 gas laser excited far infrared lasers (NH 3 , CF 4 , etc.), Pb (Cd) S, PbS (Se), Pb (Sn) Te, Pb (Sn) Se, and other compound semiconductor lasers (irradiation wavelength: 2.5 to 20 ⁇ m).
- gas chemical lasers such as HF, DF, HCl, DCl, HBr, and DBr
- CO 2 gas lasers such as HF, DF, HCl, DCl, HBr, and DBr
- CO 2 gas lasers such as HF, DF, HCl, DCl, HBr, and DBr
- CO 2 gas lasers such as HF, DF, HCl, DCl, HBr, and
- the organic acid metal salt having a polymerizable group constituting the polymer layer (C) has a polymerizable group and an acidic functional group in the molecule.
- the polymerizable group is a functional group that polymerizes by a chain reaction such as vinyl group, epoxy group, mercapto group, ureido group, sulfide group, isocyanate group, amino group, hydroxyl group, halogen atom, oxazoline group, carbodiimide group, or derivatives thereof. Particularly preferred are vinyl groups or derivatives thereof.
- the acidic functional group that becomes a counter anion with the metal salt in the organic acid metal salt is an acidic hydroxyl group such as carboxylic acid, sulfonic acid, or phenol, or mercapto acid, preferably carboxylic acid, sulfonic acid, or mercapto acid, and more preferably Are carboxylic acid and sulfonic acid.
- the organic acid metal salt having a polymerizable group can be polymerized by ultraviolet rays, electron beams or heat after forming a film as a monomer to obtain a polymer layer (C).
- the organic acid metal salt having a polymerizable group may be formed into a polymer layer (C) by forming a film as a low polymer, that is, a polymer having a low polymerization degree, and then polymerizing it with ultraviolet rays, electron beams or heat.
- the degree of polymerization of such a low molecular weight polymer is preferably a degree of polymerization of less than 20, more preferably a monomer or a polymer of 10 or less.
- the organic acid metal salt having a polymerizable group is not particularly limited, but examples of polymerizable carboxylic acid compounds that can be preferably used include acrylic acid, methacrylic acid, maleic acid, itaconic acid, and derivatives thereof. It is a carboxylic acid compound having a polymerizable vinyl group. These carboxylic acid compounds may be one kind or a mixture of two or more kinds.
- examples of polymerizable sulfonic acid compounds that can be preferably used include vinyl sulfonic acid, allyl sulfonic acid, methallyl sulfonic acid, sulfonic acid acrylate, It is a sulfonic acid compound having a polymerizable vinyl group such as sulfonic acid acrylamide, sulfonic acid methacrylate, styrene sulfonic acid, isoprene sulfonic acid and derivatives thereof. These sulfonic acid compounds may be one kind or a mixture of two or more kinds.
- the organic acid metal salt having a polymerizable group may be a mixture of two or more of a carboxylic acid compound having a polymerizable group and a sulfonic acid compound.
- the metal compound forming the metal salt used in the present invention is composed of a divalent or higher valent metal compound, a monovalent metal compound, or a mixture thereof.
- divalent metal compounds are preferable, and magnesium oxide, calcium oxide, barium oxide, zinc oxide, magnesium hydroxide, calcium hydroxide, barium hydroxide, zinc hydroxide, and the like are particularly preferable.
- the gas barrier property under high humidity of the film obtained by polymerizing the salt with the unsaturated carboxylic acid compound is particularly excellent.
- At least one kind of these divalent or higher-valent metal compounds is used, and only one kind may be used or two or more kinds may be used in combination.
- Mg, Ca, Zn and Ba are preferable, and among them, Zn is particularly preferable.
- the monovalent metal compound is a group 1A of the periodic table, that is, an alkali metal and a metal compound thereof, specifically, monovalent metals such as lithium (Li), sodium (Na), potassium (K), and the like.
- Metal oxides, hydroxides, halides, carbonates, phosphates, phosphites, hypophosphites, sulfates or sulfites, specifically lithium oxide, sodium oxide, oxidation Examples include potassium, lithium hydroxide, sodium hydroxide, and potassium hydroxide.
- the film obtained by polymerization as a metal salt of the unsaturated carboxylic acid compound has good gas barrier properties under low humidity.
- the gas barrier properties under high humidity are particularly excellent.
- At least one kind of these monovalent metal compounds is used, and only one kind may be used, or two or more kinds may be used in combination.
- lithium (Li) or sodium (Na) is particularly preferable.
- the polymer layer (C) formed from the compound composed of the above-described polymer group and organic acid metal salt includes methyl (meth) acrylate, (meth) within a range not impairing the object of the present invention.
- Monomers or low molecular weight compounds such as unsaturated carboxylic acid ester compounds such as ethyl acrylate, vinyl ester compounds such as vinyl acetate, polyvinyl alcohol, ethylene / vinyl alcohol copolymers, polyvinyl pyrrolidone, polyvinyl ethyl ether, polyacrylamide , Polyethyleneimine, starch, gum arabic, methylcellulose and other water-soluble polymers, acrylic ester polymers, ethylene / acrylic acid copolymers, polyvinyl acetate, ethylene / vinyl acetate copolymers, polyester, polyurethane, epoxy resins, etc. Or a high molecular weight compound may be contained.
- the surface of the silicon-containing layer (B) is subjected to corona treatment, glow discharge treatment, near-atmospheric pressure plasma treatment, low-pressure plasma treatment, mercury lamp or excimer lamp before the metal salt polymer layer (C) is provided.
- Pretreatment such as ultraviolet ozone treatment may be performed.
- corona treatment and ultraviolet ozone treatment are preferred.
- the conditions for the corona treatment are not particularly limited, but for example, the discharge frequency may be 5 to 40 kHz, especially about 10 to 30 kHz, and the waveform is, for example, an AC sine wave.
- the gap clearance between the electrode and the dielectric roll is set to 0.1 to 10 millimeters, particularly about 1.0 to 2.0 millimeters, and the processing amount is set to about 0.3 to 0.4 KV ⁇ A ⁇ minute / m 2 .
- You can also Corona treatment and ultraviolet ozone treatment are suitable in that they can be treated at atmospheric pressure.
- the polymer layer (C) obtained from an organic acid metal salt having a polymerizable group or a polymer containing the same is prepared by, for example, dissolving a compound composed of a polymer group and an organic acid metal salt in a solvent, and then mixing the mixture.
- a monovalent metal salt and a divalent or higher metal salt are formed by adding the above metal compound to a method of applying a solution of the above or a solution in which a compound composed of a polymerization group and an organic acid is dissolved in a solvent. Examples thereof include a method of preparing a polymer layer (C) by coating with a prepared solution and polymerizing it with ultraviolet rays, electron beams or heat, but is not limited thereto.
- a method for applying a polymer layer (C) obtained from a compound comprising a polymer group and an organic acid metal salt or a polymer containing the same on the silicon-containing layer (B) of the laminate for example, an air knife Reverse roll coaters such as coaters, direct gravure coaters, gravure offsets, arc gravure coaters, gravure reverse and jet nozzle types, top feed reverse coaters, bottom feed reverse coaters and nozzle feed reverse coaters, 5-roll coaters, lips
- an air knife Reverse roll coaters such as coaters, direct gravure coaters, gravure offsets, arc gravure coaters, gravure reverse and jet nozzle types, top feed reverse coaters, bottom feed reverse coaters and nozzle feed reverse coaters, 5-roll coaters, lips
- the method include coating using various known coating machines such as a coater, a bar coater, a bar reverse coater, and a die coater.
- unsaturated carboxylic acid ester compounds such as methyl (meth) acrylate and ethyl (meth) acrylate, as long as the object of the present invention is not impaired.
- Monomers such as vinyl ester compounds such as vinyl acetate or low molecular weight compounds, polyvinyl alcohol, ethylene / vinyl alcohol copolymers, polyvinyl pyrrolidone, polyvinyl ethyl ether, polyacrylamide, polyethylene imine, starch, gum arabic, methyl cellulose, etc.
- Water-soluble polymers acrylic acid ester polymers, ethylene / acrylic acid copolymers, polyvinyl acetate, ethylene / vinyl acetate copolymers, polyesters, polyurethanes and other high molecular weight compounds may be added.
- a lubricant when dissolving the organic acid metal salt having a polymerizable group, a lubricant, a slip agent, an anti-blocking agent, an antistatic agent, an antifogging agent, and a pigment within the range not impairing the object of the present invention.
- Various additives such as dyes, inorganic or organic fillers may be added, and various surfactants may be added to improve the wettability with the silicon-containing layer (B). May be.
- a silane coupling agent may be added in order to improve the adhesion with the polysilazane film.
- the silane coupling agent is preferably a (meth) acrylic silane coupling agent.
- Specific examples of the (meth) acrylic silane coupling agent include 3-methacryloxypropylmethyldimethoxysilane, 3-methacryloxypropyltrimethoxysilane, 3-methacryloxypropylmethyldiethoxysilane, and 3-methacryloxypropyltriethoxy. Examples thereof include silane and 3-acryloxypropyltrimethoxysilane.
- the (meth) acrylic silane coupling agent may be used as a solution obtained by hydrolyzing the coupling agent. Hydrolysis may be promoted under acidic conditions during the hydrolysis. Moreover, you may dilute and use the solution which hydrolyzed the (meth) acrylic-type silane coupling agent.
- the diluent solvent include water, alcohols such as methanol, ethanol and 2-propanol. The addition amount is preferably 0.1 to 20% by mass relative to the organic acid metal salt having a polymerizable group.
- the organic acid metal salt having a polymerizable group In order to polymerize the organic acid metal salt having a polymerizable group, various known methods, specifically, for example, a method by irradiation of energy rays such as ionizing radiation or heating are used.
- energy rays When energy rays are used, the energy region is not particularly limited as long as the wavelength region is in the range of 0.0001 to 800 nm. Examples of such energy rays include ⁇ rays, ⁇ rays, ⁇ rays, X rays, visible rays, Examples include ultraviolet rays and electron beams.
- a polymerization accelerator can be added to improve the polymerization degree or polymerization rate, for example, N, N-dimethylamino-ethyl- (meth) acrylate, N- (meth) acryloyl-morpholine, 2,2 -Bis (2-chlorophenyl) -4,4 ', 5,5'-tetraphenyl-1,2'-biimidazole, tris (4-dimethylaminophenyl) methane, 4,4'-bis (dimethylamino) benzophenone 2-ethylanthraquinone, camphorquinone and the like.
- a thermal polymerization initiator may be used when heat treatment is performed in order to advance polymerization by heat.
- the thermal polymerization initiator include persulfate, azo polymerization initiator, peroxide, and hydrogen peroxide solution.
- a thermal polymerization initiator is usually added in a proportion of 0.001 to 10% by weight, preferably 0.01 to 5% by weight, in the polymerizable composition.
- Heat treatment to promote polymerization by heat includes convection heat transfer (eg, dryer, oven), conduction heat transfer (eg, heating roll), and radiant heat transfer (eg, infrared, far infrared, near infrared heaters) And the like due to internal heat generation (for example, microwaves).
- convection heat transfer eg, dryer, oven
- conduction heat transfer eg, heating roll
- radiant heat transfer eg, infrared, far infrared, near infrared heaters
- internal heat generation for example, microwaves.
- heat treatment in an oven although it depends on the type of film substrate, it is usually about 60 ° C. to 350 ° C., usually about 1 minute to 5 hours, particularly preferably 100 ° C. to 200 ° C., 5 minutes to 2 hours. .
- continuous heating treatment with a heating roll and a far-infrared furnace is effective at a high treatment speed.
- the laminate of the present invention has a thermosetting resin layer, an ultraviolet curable resin layer, a hard coat resin layer, an easy-sliding layer, a conductive layer, a heat-sealing layer, a function such as the following on at least one surface according to the intended application.
- the element sealing resin layer may be further laminated, or a single layer or a combination of layers may be laminated.
- Thermosetting resin layer, UV curable resin layer, hard coat resin layer It can be formed by coating a general thermosetting resin layer, an ultraviolet curable resin, or a hard coat resin, and crosslinking by heating, ultraviolet rays, an electron beam or the like. Specifically, it is a (meth) acrylic resin or an epoxy resin. In addition, these resins may be used alone or in combination as necessary. When used after being cured with ultraviolet rays, it is preferable to use a photo radical initiator, a photo cation initiator, a photo acid generator, and a photo sensitizer in combination.
- a laminated film suitable as an electronic member can be obtained by laminating conductive metals, ceramics, and carbon materials. Although it does not specifically limit as a metal, Metals, such as gold
- the conductive layer is coated with a paste-like coating liquid in which fine particles of the metal, ceramics, or carbon material are dispersed in water or an organic solvent, or by using a vapor phase deposition method such as vapor deposition or sputtering. A thin film can be produced.
- Heat-fusion layer By laminating the heat-fusible layer, a laminated film suitable as a packaging film that can be heat-heat sealed can be obtained.
- a heat-sealing layer an ⁇ -olefin such as ethylene, propylene, butene-1, hexene-1, 4-methylpentene-1, octene-1, etc., which are generally known as heat-sealing layers, are used alone or in combination.
- Polymer high pressure low density polyethylene, linear low density polyethylene (so-called LLDPE), high density polyethylene, polypropylene, polypropylene random copolymer, polybutene, poly-4-methyl pentene-1, low crystalline or amorphous Polyethylene such as ethylene / propylene random copolymer, ethylene / butene-1 random copolymer, propylene / butene-1 random copolymer, or a composition of two or more kinds, ethylene / vinyl acetate copolymer (EVA) , Ethylene / (meth) acrylic acid copolymer or metal salt thereof, EVA and polyolefin A layer obtained from the composition or the like.
- LLDPE linear low density polyethylene
- EVA ethylene / vinyl acetate copolymer
- EVA Ethylene / (meth) acrylic acid copolymer or metal salt thereof
- EVA polyolefin A layer obtained from the composition or the like.
- a heat-sealing layer obtained from an ethylene-based polymer such as high-pressure method low-density polyethylene, linear low-density polyethylene (so-called LLDPE), or high-density polyethylene is preferable because it has excellent low-temperature heat sealability and heat seal strength.
- the thickness of such a heat-sealing layer is usually about 1 to 50 ⁇ m.
- Examples of the element 14 include liquid crystal display elements, elements such as organic EL, organic functional elements such as planar light emitters and optical devices, and inorganic functional elements such as inorganic EL.
- the laminate of the present invention can be effectively used particularly for organic ELs that require a high moisture / oxygen barrier.
- the laminated body of this invention can be used effectively with respect to organic EL.
- the functional element sealing resin layer 16 can be used as an organic EL sealing resin layer.
- As the organic EL sealing resin layer a known thermosetting resin, ultraviolet curable resin, or heat sealable thermoplastic resin such as acrylate or epoxy resin is used.
- the thermoplastic resin used in the heat-sealable thermoplastic resin layer is not particularly limited, but among them, low density polyethylene, LLDPE, which is a random copolymer of ethylene and an ⁇ -olefin having 4 to 8 carbon atoms, and ethylene / propylene copolymer.
- thermoplastic resins include a method of laminating and a method of forming a coat layer by coating.
- examples of the coating agent include ionomers such as ethylene-vinyl acetate copolymer, ethylene-vinyl acetate copolymer, ethylene-acrylic acid copolymer, and ethylene-methacrylic acid sodium salt copolymer. Is done.
- the heat-sealable thermoplastic resin layer can be used without particular limitation as long as it is melt-fixed to other materials by heat melting.
- polyolefins such as acrylic acid, maleic anhydride, polyethylene grafted with these derivatives, and polypropylene are preferable.
- the polymer layer (C) 18 and the sealing resin layer 16 can be further bonded to the organic EL sealing resin layer using a cured resin as an adhesive layer as necessary. That is, the structure of base material (A) / silicon-containing layer (B) / polymer layer (C) / (adhesive layer) / organic EL sealing resin is obtained. Such a configuration is preferable because high moisture / oxygen barrier properties and EL element protection performance can be obtained.
- the outline of the plasma processing apparatus used in the production of the silicon-containing layers (B) in Examples 1 to 10 and Comparative Examples 3, 5 and 6 is as follows.
- Low-pressure capacitively coupled plasma processing equipment manufactured by U-Tech Co., Ltd.
- a parallel plate electrode type low pressure capacitively coupled plasma processing apparatus using a SUS vacuum vessel One is connected to a high frequency power source through a matching unit, and the other is grounded.
- the electrode interval was 70 mm.
- the polysilazane film was placed on the grounded electrode side for processing.
- the input power density was determined with the area of the opposing electrode surface on the high frequency power supply side as the area of the plasma source.
- the temperature of the electrode can be controlled by flowing a liquid, and the substrate of the polysilazane film can be heated.
- II Low pressure inductively coupled plasma processing equipment ICP method
- An external antenna type low pressure inductively coupled plasma processing apparatus in which a single loop antenna coil is installed in a cylindrical stainless steel vessel made of SUS through a quartz dielectric window. The entire upper surface of the vacuum vessel is an inductively coupled plasma source. Therefore, the area of the plasma source was calculated from the inner diameter of the vacuum vessel, and the input power density was obtained.
- One of the antenna coils is connected to a high frequency power source through a matching unit, and the other is grounded.
- the polysilazane film was placed on a sample stage 200 mm away from the dielectric window.
- Dielectric barrier discharge type plasma processing apparatus A parallel plate electrode type dielectric barrier discharge type plasma processing apparatus in which a glass vacuum vessel is covered with glass. One is connected to an impulse type high-voltage power supply, and the other is grounded. The electrode interval was 5 mm. The polysilazane film was placed on the grounded electrode side for processing. In addition, the input power density was determined with the area of the opposing electrode surface on the high-voltage power supply side as the area of the plasma source.
- Initiator [1- [4- (2-hydroxyethoxy) -phenyl] -2-hydroxy-2-methyl-1-propan-1-one (trade name; Irgacure 2959 manufactured by Ciba Specialty Chemicals)] and Surfactant (trade name; Emulgen 120, manufactured by Kao Corporation) was added at 2% and 0.4%, respectively, in a solid content ratio with respect to acrylic acid to prepare an unsaturated carboxylic acid compound Zn salt solution (W).
- Propan-1-one (trade name; Irgacure 2959, manufactured by Ciba Specialty Chemicals) and surfactant (trade name; Emulgen 120, manufactured by Kao Corporation) were 2% and 0% in terms of solid content with respect to acrylic acid, respectively. .4% was added to prepare a solution (X) of a lithium salt of an unsaturated carboxylic acid compound.
- Propan-1-one (trade name; Irgacure 2959, manufactured by Ciba Specialty Chemicals) and surfactant (trade name; Emulgen 120, manufactured by Kao Corporation) were 2% and 0% in terms of solid content with respect to acrylic acid, respectively. .4% was added to prepare a sodium salt solution (Y) of an unsaturated carboxylic acid compound.
- Example 1 4.5 wt% xylene (dehydration) of polysilazane (NL110A, manufactured by AZ Electronic Materials) on a polyethylene terephthalate (PET) film (thickness 50 ⁇ m, “A4100”, manufactured by Toyobo Co., Ltd.) as a base material (A) )
- the solution was bar coated and dried at 150 ° C. for 90 seconds to produce a polysilazane film having a thickness of 0.15 ⁇ m.
- the polysilazane film was subjected to low-pressure plasma treatment under the following conditions to produce a silicon-containing layer (B).
- Vacuum plasma processing equipment Low-pressure capacitively coupled plasma processing equipment (manufactured by UTEC Co., Ltd.) Gas: He Gas flow rate: 50 mL / min Pressure: 19Pa Applied power per electrode unit area: 1.3 W / cm 2 Frequency: 13.56MHz Treatment time: 30 seconds Oxygen concentration: 1 ppm or less Water vapor concentration: 1 ppm or less
- the solution (A) is applied to the produced silicon-containing layer (B) so as to be 2.8 g / m 2 , and the temperature is 60%, the time is 30 seconds using a hot air dryer. Dried.
- the coated surface is fastened and fixed to a stainless steel plate, and using a UV irradiation device (EYE GRANDAGE model ECS 301G1 manufactured by Eye Graphic Co., Ltd.) under the conditions of UV intensity 190 mW / cm 2 and integrated light quantity 250 mJ / cm 2 .
- the obtained gas barrier laminate film was placed on a hot plate and subjected to heat treatment to obtain a laminate.
- the conditions for the heat treatment are a hot plate temperature of 200 ° C. and a holding time of 60 minutes.
- FIG. 2 shows the XPS measurement result of the silicon-containing layer (B) obtained by performing the low-pressure plasma treatment
- Table 1 shows the physical property measurement result of the obtained laminate.
- N / (N + O) at the depth at which the nitrogen content was highest was calculated.
- results similar to the measured values in FIG. 2 were obtained at any location, so that nitrogen was spread over the entire surface of the silicon-containing layer (B). It was confirmed that a high concentration region was formed.
- Example 2 On a polyethylene terephthalate (PET) film (thickness 50 ⁇ m, “A4100”, manufactured by Toyobo Co., Ltd.) as a base material (A), urethane acrylate (urethane acrylate UV curable coating material (made by Shin-Nakamura Chemical Co., Ltd., trade name UA-) 100) was diluted with ethyl acetate, applied to 1.2 g / m 2 (solid content) using a Mayer bar, and dried for 15 seconds at 100 ° C. Subsequently, a UV irradiation device (eye) was applied to the coated surface. EYE GRANDAGE Model ECS 301G1) manufactured by Graphic Co., Ltd.
- EYE GRANDAGE Model ECS 301G1 manufactured by Graphic Co., Ltd.
- Example 3> The solution A used in Example 2 was changed to Solution B, and other operations similar to those in Example 2 were performed to obtain a laminate.
- Table 1 shows the physical property measurement results of the obtained laminate.
- Example 4> The solution A used in Example 2 was changed to Solution C, and other operations similar to those in Example 2 were performed to obtain a laminate.
- Table 1 shows the physical property measurement results of the obtained laminate.
- Example 5 Solution A used in Example 2 was changed to Solution D, and other operations similar to Example 2 were performed to obtain a laminate.
- Table 1 shows the physical property measurement results of the obtained laminate.
- Example 6 Coating and drying were performed in the same manner as in Example 2 to prepare a polysilazane film, and the plasma treatment in Example 2 was changed to the following conditions to perform low-pressure plasma treatment.
- Vacuum plasma processing equipment Low-pressure capacitively coupled plasma processing equipment (manufactured by UTEC Co., Ltd.) Gas: Ar Gas flow rate: 50 mL / min Pressure: 19Pa Applied power per electrode unit area: 1.3 W / cm 2 Frequency: 13.56MHz Treatment time: 5 minutes Oxygen concentration: 1 ppm or less Water vapor concentration: 1 ppm or less Thereafter, a polymer layer (C) was produced on the silicon-containing layer (B) in the same manner as in Example 2 to obtain a laminate. Table 1 shows the physical property measurement results of the obtained laminate.
- Example 7 Coating and drying were performed in the same manner as in Example 2 to prepare a polysilazane film, and the plasma treatment in Example 2 was changed to the following conditions to perform low-pressure plasma treatment.
- Plasma processing equipment Low-pressure capacitively coupled plasma processing equipment (manufactured by UTEC Co., Ltd.) Gas: He + H 2 (H 2 concentration: 6 vol%) Total pressure: 19Pa Input power density: 1.3 W / cm 2 Frequency: 13.56MHz
- Water vapor concentration: 1 ppm or less Thereafter, a polymer layer (C) was produced on the silicon-containing layer (B) in the same manner as in Example 2 to obtain a laminate. Table 1 shows the physical property measurement results of the obtained laminate.
- Example 9 Coating and drying were performed in the same manner as in Example 2 to prepare a polysilazane film, and the plasma treatment in Example 2 was changed to the following conditions to perform low-pressure plasma treatment.
- Plasma processing apparatus Low-pressure inductively coupled plasma processing apparatus (self-made): ICP gas: He + H 2 (H 2 concentration: 6 vol%) Pressure: 20Pa Input power density: 2 W / cm 2 (4000 W, plasma source area ⁇ 250 mm) Frequency: 13.56MHz Treatment time: 20 seconds Oxygen concentration: 1 ppm or less Water vapor concentration: 1 ppm or less Thereafter, a polymer layer (C) was produced on the silicon-containing layer (B) in the same manner as in Example 2 to obtain a laminate. Table 1 shows the physical property measurement results of the obtained laminate.
- Example 10 Coating and drying were performed in the same manner as in Example 2 to prepare a polysilazane film, and the plasma treatment in Example 2 was changed to the following conditions to perform near atmospheric pressure plasma treatment.
- Plasma processing equipment Dielectric barrier discharge type plasma processing equipment (self-made) Gas: Ar Pressure: 50kPa Substrate heating temperature: Room temperature Input power density: 0.4 W / cm 2 Frequency: 10kHz Treatment time: 600 seconds Oxygen concentration: 1 ppm or less Water vapor concentration: 1 ppm or less Thereafter, a polymer layer (C) was produced on the silicon-containing layer (B) in the same manner as in Example 2 to obtain a laminate. Table 1 shows the physical property measurement results of the obtained laminate.
- the coated surface is fastened and fixed to a stainless steel plate, and using a UV irradiation device (EYE GRANDAGE model ECS 301G1 manufactured by Eye Graphic Co., Ltd.) under the conditions of UV intensity 190 mW / cm 2 and integrated light quantity 250 mJ / cm 2 .
- a UV irradiation device EYE GRANDAGE model ECS 301G1 manufactured by Eye Graphic Co., Ltd.
- the obtained gas barrier laminate film was placed on a hot plate and subjected to heat treatment to obtain a laminate.
- the conditions for the heat treatment are a hot plate temperature of 200 ° C. and a holding time of 60 minutes. Table 1 shows the physical property measurement results of the obtained laminate.
- urethane acrylate urethane acrylate UV curable coating material (manufactured by Shin-Nakamura Chemical Co., Ltd., trade name) UA ⁇ 100)
- urethane acrylate UV curable coating material manufactured by Shin-Nakamura Chemical Co., Ltd., trade name
- the coating is photocured under the conditions of UV intensity: 250 mW / cm 2 and integrated light quantity: 117 mJ / cm 2 , and the undercoat layer is formed. Provided. Thereafter, the same operation as in Comparative Example 1 was performed to obtain a laminate. Table 1 shows the physical property measurement results of the obtained laminate.
- urethane acrylate urethane acrylate UV curable coating material (manufactured by Shin-Nakamura Chemical Co., Ltd., trade name) UA ⁇ 100)
- urethane acrylate UV curable coating material manufactured by Shin-Nakamura Chemical Co., Ltd., trade name
- urethane acrylate urethane acrylate UV curable coating material (manufactured by Shin-Nakamura Chemical Co., Ltd., trade name) UA ⁇ 100)
- urethane acrylate UV curable coating material manufactured by Shin-Nakamura Chemical Co., Ltd., trade name
- the above solution (A) was applied at 2.8 g / m 2 without passing through the silicon-containing layer (B), and dried using a hot air drier at a temperature of 60 ° C. for a time of 30 seconds. did.
- the coated surface is fastened and fixed to a stainless steel plate, and UV light is applied under the conditions of UV intensity of 190 mW / cm 2 and integrated light quantity of 250 mJ / cm 2 using a UV irradiation device (EYE GRANDAGE model ECS 301G1 manufactured by Eye Graphic).
- EYE GRANDAGE model ECS 301G1 manufactured by Eye Graphic a UV irradiation device
- the resulting gas barrier laminate film was placed on a hot plate and heat-treated to obtain a polymer layer (C).
- the conditions for the heat treatment are a hot plate temperature of 200 ° C. and a holding time of 60 minutes.
- the physical property measurement results are shown in Table 1.
- urethane acrylate urethane acrylate UV curable coating material (manufactured by Shin-Nakamura Chemical Co., Ltd., trade name) UA ⁇ 100) was diluted with ethyl acetate, applied to 1.2 g / m 2 (solid content) using a Mayer bar, and dried at 100 ° C. for 15 seconds.
- Example 6 Coating and drying were performed in the same manner as in Example 2 to prepare a polysilazane film, and the plasma treatment in Example 2 was changed to the following conditions to perform near atmospheric pressure plasma treatment.
- Plasma processing equipment Atmospheric pressure plasma processing equipment (APT-02, manufactured by Sekisui Chemical Co., Ltd.)
- Gas Ar Pressure: Atmospheric pressure substrate heating temperature: Room temperature (23 ° C)
- Treatment time 600 seconds
- Table 1 shows the physical property measurement results of the obtained laminate.
- the laminate of the present invention was particularly excellent in water vapor gas barrier properties compared to the case where the dry method inorganic film in Comparative Examples 1 and 2 was used as the underlayer. Moreover, when Example 1 and Comparative Example 1 were compared, in the Example, high gas barrier property was expressed even if it did not use an undercoat layer on a base material (A). Further, from comparison between Example 2 and Comparative Examples 3, 4 and 5, as in Example 2, three of the substrate (A), the silicon-containing layer (B), and the polymer layer (C) were obtained. Only by laminating in order, it was found that a very high oxygen or water vapor barrier property that cannot be manifested in each single layer is synergistically exhibited and exhibits good bending resistance.
- the laminate of the present invention is excellent not only in oxygen gas barrier properties but also in water vapor permeation resistance, and can be used for various applications such as various packaging materials, medical applications, and industrial applications, particularly electronic paper and liquid crystal displays. It can be used for electrical and electronic materials such as organic EL panel / sealing material and substrate sealing material.
- the organic EL to be applied is not particularly limited, and can be used for any organic EL of a passive type or an active type made of a low molecular material or a high molecular material. It can be used for flexible displays, lighting, advertisement displays, sideboards, and other uses.
- the laminate of the present invention has an excellent oxygen gas barrier property and water vapor permeability resistance even when the base material is a plastic material, and can maintain the barrier property even when bent into a curved surface. Can be suitably used.
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Abstract
Description
[1]基材(A)と、前記基材(A)の少なくとも一方の面に順に積層された、シリコン含有層(B)と、重合性基を有する有機酸金属塩から得られる重合体層(C)と、からなり、
前記シリコン含有層(B)は、珪素原子と窒素原子、または珪素原子と窒素原子と酸素原子、または珪素原子と窒素原子と酸素原子と炭素原子とからなる窒素高濃度領域を有し、
前記窒素高濃度領域は、前記基材(A)上に形成されたポリシラザン膜に酸素濃度5%以下および/または室温23℃における相対湿度30%以下でエネルギー線照射を行い、当該膜の少なくとも一部を変性することにより形成される、積層体。
式(1):窒素原子の組成比/(酸素原子の組成比+窒素原子の組成比)
[4]前記重合体層(C)は、前記基材(A)上に形成された、窒素高濃度領域を有する前記シリコン含有層(B)上に、前記重合性基を有する有機酸金属塩膜を形成し、前記有機酸金属塩膜を紫外線、電子線または熱により重合して得られる、[1]乃至[3]のいずれかに記載の積層体。
[5]前記エネルギー線照射は、プラズマ照射により行われる、[1]乃至[4]のいずれかに記載の積層体。
[7]前記プラズマ照射は、酸素濃度5000ppm以下、かつ水蒸気濃度8400ppm以下で行われる、[5]または[6]に記載の積層体。
[9]前記有機酸金属塩は、カルボン酸、スルホン酸、メルカプト酸から選択される1種以上の有機酸の金属塩である、[1]乃至[8]のいずれかに記載の積層体。
[10]前記重合性基が、ビニル基、エポキシ基、メルカプト基、ウレイド基、スルフィド基、イソシアネート基、アミノ基、水酸基、ハロゲン原子、オキサゾリン基、カルボジイミド基またはそれらの誘導体から選択される1種以上の重合性基である、[1]乃至[9]のいずれかに記載の積層体。
[12] 前記有機酸金属塩は、重合性基としてビニル基を有するカルボン酸化合物の金属塩である、[1]乃至[11]のいずれかに記載の積層体。
[14]前記有機酸金属塩は、重合性基としてビニル基を有するスルホン酸化合物の金属塩である、[1]乃至[11]のいずれかに記載の積層体。
[16]前記重合体層(C)は、更にシランカップリング剤を含んでなる、[1]乃至[15]のいずれかに記載の積層体。
[17]有機エレクトロルミネッセンス素子、電子ペーパー表示素子、液晶表示素子から選ばれる素子を含む部材と、重合体層(C)が該部材側となるように配設された[1]乃至[16]のいずれかに記載の積層体とからなる、電子部材。
前記ポリシラザン膜に酸素濃度5%以下および/または室温23℃における相対湿度30%以下でエネルギー線照射を行い当該膜の少なくとも一部を変性し、珪素原子と窒素原子、または珪素原子と窒素原子と酸素原子とからなる窒素高濃度領域を含むシリコン含有層(B)を形成する工程と、
前記シリコン含有層(B)上に重合性基を有する有機酸金属塩から得られる重合体層(C)を形成する工程と、
を含む積層体の製造方法。
式(1):窒素原子の組成比/(酸素原子の組成比+窒素原子の組成比)[20]前記エネルギー線照射は、プラズマ照射により行われる、[18]または[19]に記載の積層体の製造方法。
[21]前記プラズマ照射は、不活性ガス、希ガスまたは還元ガスから選ばれる雰囲気ガス中にて行われる[20]に記載の積層体の製造方法。
以下、基材(A)、シリコン含有層(B)、重合体層(C)、および任意に用いられるその他の層について順番に詳説する。
本発明における基材(A)は、樹脂であれば特に限定されないが、例えば、ポリエチレン、ポリプロピレン、ポリ4-メチル-1-ペンテン、ポリブテン等のポリオレフィン;環状オレフィンポリマー;ポリイミド;ポリエチレンテレフタレート、ポリブチレンテレフタレート、ポリエチレンナフタレート等のポリエステル;ナイロン-6、ナイロン-66、ポリメタキシレンアジパミド等のポリアミド、ポリフェニレンスルフィド、あるいはこれらの混合物等を例示することができる。これらのうちでは、ポリプロピレン、ポリエチレンテレフタレート、ポリアミド等が延伸性、透明性、剛性が良好なフィルムが得られるので好ましい。
なお、本発明における基材(A)には、本発明の効果を損ねない範囲で紫外線吸収剤、酸化防止剤、帯電防止剤、界面活性剤、顔料、蛍光増白剤等、さらにシリカ、炭酸カルシウム、酸化チタン等の無機粒子、アクリル、スチレン等を構成成分とする有機粒子を必要に応じて適宜含有してもよい。
シリコン含有層(B)は、ポリシラザン膜にエネルギー線照射を行い、このポリシラザンの少なくとも一部を変性することにより得られる窒素高濃度領域を有する。エネルギー線照射で変性された領域以外のポリシラザン膜は、エネルギー線照射後、前記基材(A)側から透過してきた水蒸気と反応し、酸化珪素(SiO2)に変化し得る。
エネルギー照射は、0.1Pa以上の低圧~大気圧の圧力範囲で行うことができる。
また、シリコン含有層(B)の層全体に亘って窒素高濃度領域が形成されていてもよい。この場合、シリコン含有層(B)の組成は窒素高濃度領域と同様なものとなる。
式(1):窒素原子の組成比/(酸素原子の組成比+窒素原子の組成比)
窒素高濃度領域は、シリコン含有層(B)の上面の一部において上記範囲の厚みを有していればよいが、上記効果の観点から、シリコン含有層(B)の上面全体に亘って上記範囲の厚みを有していることが好ましい。
(RCOO)nM
式中、Rは炭素原子数1~22個の脂肪族基又は脂環式基であり、Mは下記金属群から選択される少なくとも1種の金属を表し、nは金属Mの原子価である。
(CH3COCHCOCH3)nM
式中、Mはn価の金属を表す。
R4R5R6N 式中、R4~R6は、それぞれ水素原子、アルキル基、アルケニル基、シクロアルキル基、アリール基、アルキルシリル基、アルキルアミノ基又はアルコキシ基を表す。アミン化合物の具体例として、メチルアミン、ジメチルアミン、トリメチルアミン、エチルアミン、ジエチルアミン、トリエチルアミン、プロピルアミン、ジプロピルアミン、トリプロピルアミン、ブチルアミン、ジブチルアミン、トリブチルアミン、ペンチルアミン、ジペンチルアミン、トリペンチルアミン、ヘキシルアミン、ジヘキシルアミン、トリヘキシルアミン、ヘプチルアミン、ジヘプチルアミン、トリヘプチルアミン、オクチルアミン、ジオクチルアミン、トリオクチルアミン、フェニルアミン、ジフェニルアミン、トリフェニルアミン、等が挙げられる。なお、これらアミン化合物に含まれる炭化水素鎖は、直鎖であっても分枝鎖であってもよい。特に好ましいアミン化合物は、トリエチルアミン、トリペンチルアミン、トリブチルアミン、トリヘキシルアミン、トリヘプチルアミン及びトリオクチルアミンである。
以上の遷移金属化合物の遷移金属種としては、白金(Pt)、ルテニウム(Ru)、ロジウム(Rh)、イリジウム(Ir)、鉄(Fe)、オスミニウム(Os)、コバルト(Co)、パラジウム(Pd)、ニッケル(Ni)、チタン(Ti)、バナジウム(V)、クロム(Cr)、マンガン(Mn)、モリブデン(Mo)、タングステン(W)、ニオブ(Nb)、タンタル(Ta)、ジルコニウム(Zr)、ハフニウム(Hf)、スカンジウム(Sc)、イットリウム(Y)、ランタン(La)、レニウム(Re)を含む化合物またはこれらの混合物である。
以上の遷移金属のハロゲン化物すべて有効に用いることができるが、より好ましくは、クロロ白金酸(H2PtCl6.nH2O )、PtCl2、PtCl4、PtCl2(NH3)2、Na2(PtCl4).nH2O、[PtCl(cyclohexene)2](μ-Cl)2、RhCl3、Tris(dibutylsulfide)RhCl3、(NH4)3[RhCl6] 、RhI3、(NH3)6RhCl3 、RuCl3、[Ru(p-cymeme)Cl2]2、[Ru(benzene) Cl2]2、(NH4)2RuCl6、(NH3)4[RuCl4(H2O)]2(μ-N)、Ni(triphenylphosphine)3Br2、Mn(CO)5Br、IrCl3、(NH4)2IrCl6、FeCl3、PdCl2・2H2O、NiCl2、TiCl4 、OsCl3、(NH4)2OsCl6、W(cyclopentadiene)2Cl2、これらの混合物が挙げられる。
前記遷移金属酸化物は、上記遷移金属に酸素原子が一つ以上結合した化合物のことである。
遷移金属化合物/ポリシラザン重量比は好ましくは0.0001~1.0、より好ましくは0.001~0.5、更により好ましくは0.01~0.2である。
ポリシラザン含有液は、溶媒に、ポリシラザンおよび必要に応じて用いられる触媒や金属微粒子等が溶解または分散している。
プラズマ処理を行うと、他のエネルギー線照射に比べて、窒素高濃度領域を均一に形成することが出来るため、シリコン含有層(B)のバリア性、特に水蒸気バリア性が優れる点で好ましい。
本発明で用いるプラズマ処理について以下に説明する。プラズマ処理は、低圧、大気圧近傍プラズマがある。より好ましくは低圧プラズマが好ましい処理方法である。
プラズマ処理に用いるガスとしては、シリコン含有層の窒素高濃度領域を形成する観点から、不活性ガスである窒素ガス、希ガスであるアルゴンガス、ヘリウムガス、ネオンガス、クリプトンガス、キセノンガス等、還元ガスである水素ガス、アンモニアガス等が挙げられる。さらに好ましいガスとしては、アルゴンガス、ヘリウムガス、窒素ガス、水素ガス、またはこれらの混合ガスが挙げられる。
低圧プラズマには、真空の密閉系内に公知の電極または導波管を配置し、直流、交流、ラジオ波あるいはマイクロ波等の電力を、電極または導波管を介して印加することにより任意のプラズマを発生させることができる。プラズマ処理時に印加する電力(W)は、電極の単位面積(cm2)あたり、好ましくは0.0001W/cm2~100W/cm2、より好ましくは0.001W/cm2~50W/cm2である。
低圧下における酸素濃度および水蒸気濃度は、一般的に、酸素分圧および水蒸気分圧で評価される。
低圧プラズマ処理では、前記のプラズマガス種を導入し、ガス分圧500Pa~0.1Paの低圧で行う。より好ましくは、100Pa~0.1Paで行うとプラズマ発生効率が良い。
本発明で用いるプラズマの生成方式は、従来から知られた方式を用いる事ができる。好ましくは、幅広の基材(A)に形成したポリシラザン膜の処理に対応できる方式が良く、例えば、次に示す(A)~(E)の方式が挙げられる。
高周波電力を印加した側の電極と接地側の電極との間にプラズマを生成する方式で、対向した平板電極が代表的な電極構造である。高周波電力を印加した側の電極は、平板状だけでなく、凹凸形状であっても良い。
アンテナコイルに高周波電流を流し、コイルが作る磁場による誘導電界でプラズマを生成する方式で、一般に容量結合プラズマに比べ高い電子密度(プラズマ密度)が得られるとされる。誘電体層を介してアンテナコイルをチャンバの外に置く外部アンテナ型、アンテナコイルをチャンバ内に設置する内部アンテナ型のどちらを採用してもよい。また、幅広の基材に対応するため、アンテナコイルをアレイ状に配置する等の工夫をしても良い。
(C)表面波プラズマ
(D)電子サイクロトロン共鳴(ECR)プラズマ
(E)ヘリコン波プラズマ
大気圧近傍プラズマ処理としては、二つの電極間にガスを通し、このガスをプラズマ化してから基材(A)に照射する方式や、二つの電極間に照射するポリシラザン膜付き基材を配置し、そこへガスを通してプラズマ化する方式などが挙げられる。
大気圧近傍プラズマ処理において、印加する電力(W)は、電極の単位面積(cm2)あたり、好ましくは0.0001W/cm2~100W/cm2、より好ましくは0.001W/cm2~50W/cm2である。大気圧プラズマ処理における、ポリシラザン膜付き基材の移動速度は、好ましくは0.001~1000m/minであり、より好ましくは0.001~500m/minである。
ポリウレタン系オリゴマーは、ポリイソシアネートとポリオールとの縮合生成物から得ることができる。具体的なポリイソシアネートとしては、メチレン・ビス(p-フェニレンジイソシアネート)、ヘキサメチレンジイソシアネート・ヘキサントリオールの付加体、ヘキサメチレンジイソシアネート、トリレンジイソシアネート、トリレンジイソシアネートトリメチロールプロパンのアダクト体、1,5-ナフチレンジイソシアネート、チオプロピルジイソシアネート、エチルベンゼン-2,4-ジイソシアネート、2,4-トリレンジイソシアネート二量体、水添キシリレンジイソシアネート、トリス(4-フェニルイソシアネート)チオフォスフェートなどが例示でき、また、具体的なポリオールとしては、ポリオキシテトラメチレングリコールなどのポリエーテル系ポリオール、ポリアジペートポリオール、ポリカーボネートポリオールなどのポリエステル系ポリオール、アクリル酸エステル類とヒドロキシエチルメタアクリレートとのコポリマーなどがある。アクリレートを構成する単量体としては、メチル(メタ)アクリレート、エチル(メタ)アクリレート、ブチル(メタ)アクリレート、2エチルヘキシル(メタ)アクリレート、メトキシエチル(メタ)アクリレート、ブトキシエチル(メタ)アクリレート、フェニル(メタ)アクリレートなどがある。
これらを紫外線で硬化して使用する場合は、アセトフェノン類、ベンゾフェノン類、ミフィラベンゾイルベンゾエート、α-アミロキシムエステルまたはチオキサントン類などを光重合開始剤として、また、n-ブチルアミン、トリエチルアミン、トリn-ブチルホスフィンなどを光増感剤として混合して使用するのが好ましい。本発明では、エポキシ(メタ)アクリレート系化合物とウレタン(メタ)アクリレート系化合物は、併用することも行われる。
これらのアンダーコート層は、通常0.05~5.0グラム/m2が通常であり、中でも0.1~3.0グラム/m2が好適である。
また、シリコン含有層(B)の表面は金属塩の重合体層(C)を設ける前に、コロナ処理、グロー放電処理、大気圧プラズマ処理、真空プラズマ放電処理などの前処理をすることが望ましい。中でもコロナ処理が好適である。コロナ処理の条件は、特に限定されないが、例えば放電周波数は、5~40kHz、中でも10~30kHz程度を用いることもでき、波形として例えば交流正弦波がある。電極と誘電体ロールとのギャップのクリアランスを0.1~10ミリメートル、中でも1.0~2.0ミリメートル程度とし、処理量として0.3~0.4KV・A・分/m2程度とすることもできる。空気中常圧で処理できる点で好適である。
また、プラズマ処理と同時に、ポリシラザン膜が塗工された基材の加熱処理を行うことで、より短時間で処理することができる。加熱処理温度としては、高ければ高いほど良いが、基材の特性を考慮すると、好ましくは25℃~1000℃、より好ましくは30℃~500℃、更に好ましくは60℃~300℃の範囲である。
(追加処理)
プラズマ処理により変性されたシリコン含有層(B)に対し、さらに活性エネルギー線の照射または加熱処理を施すことで、シリコン含有層(B)における窒素高濃度領域を増加させることができる。
重合体層(C)を構成する重合性基を有する有機酸金属塩は、分子内に重合性基および酸性官能基を有する。
重合性基は、ビニル基、エポキシ基、メルカプト基、ウレイド基、スルフィド基、イソシアネート基、アミノ基、水酸基、ハロゲン原子、オキサゾリン基、カルボジイミド基またはこれらの誘導体といった連鎖反応により重合する官能基であり、特に好ましくは、ビニル基またはこれらの誘導体である。
有機酸金属塩における金属塩とカウンターアニオンになる酸性官能基としては、カルボン酸、スルホン酸、フェノール等の酸性水酸基、メルカプト酸であり、好ましくはカルボン酸、スルホン酸、メルカプト酸であり、さらに好ましくはカルボン酸、スルホン酸である。
このような低分子重合体の重合度は、好ましくは重合度が20未満、さらに好ましくは単量体もしくは10以下の重合体である。
さらには、重合性基を有する有機酸金属塩を予め熱やエネルギー照射により重合し、得られた重合体の溶液を塗布して膜を形成した後に、溶媒を乾燥して重合体層(C)としてもよい。
本発明に用いられる金属塩を形成する金属化合物は、二価以上の金属化合物、もしくは一価の金属化合物、もしくはこれらの混合物から構成される。
二価以上の金属化合物は、周期表の2A~7A族、1B~3B族及び8族に属する金属及び金属化合物であり、具体的には、マグネシウム(Mg)、カルシウム(Ca)、ストロンチウム(Sr)、バリウム(Ba)、鉄(Fe)、コバルト(Co)、ニッケル(Ni)、銅(Cu)、亜鉛(Zn)、アルミニウム(Al)等の二価以上の金属、これら金属の酸化物、水酸化物、ハロゲン化物、炭酸塩、リン酸塩、亜リン酸塩、次亜リン酸塩、硫酸塩若しくは亜硫酸塩等である。これら金属化合物の中でも、二価の金属化合物が好ましく、特には酸化マグネシウム、酸化カルシウム、酸化バリウム、酸化亜鉛、水酸化マグネシウム、水酸化カルシウム、水酸化バリウム、水酸化亜鉛等が好ましい。これら二価の金属化合物を用いた場合は、前記不飽和カルボン酸化合物との塩を重合して得られる膜の高湿度下でのガスバリア性が特に優れている。これら二価以上の金属化合物は、少なくとも一種が使用され、一種のみの使用であっても、二種以上を併用してもよい。これら二価以上の金属化合物の中でもMg、Ca、Zn及びBaが好ましく、中でも、特にZnが好ましい。
一価の金属化合物は、周期表の1A族、即ち、アルカリ金属及びその金属化合物であり、具体的には、リチウム(Li)、ナトリウム(Na)、カリウム(K)等の一価金属、これら金属の酸化物、水酸化物、ハロゲン化物、炭酸塩、リン酸塩、亜リン酸塩、次亜リン酸塩、硫酸塩若しくは亜硫酸塩等であり、具体的には酸化リチウム、酸化ナトリウム、酸化カリウム、水酸化リチウム、水酸化ナトリウム、水酸化カリウム等を挙げることができる。
金属化合物として、2価以上の金属化合物と共にこれら一価の金属化合物を併用した場合は、前記不飽和カルボン酸化合物の金属塩として重合して得られる膜は、低湿度下でのガスバリア性が良好であるばかりではなく、高湿度下でのガスバリア性が特に優れている。これら一価の金属化合物は、少なくとも一種が使用され、一種のみの使用であっても、二種以上を併用してもよい。これら一価の金属化合物の中でもリチウム(Li)またはナトリウム(Na)が特に好ましい。
シランカップリング剤は、(メタ)アクリル系シランカップリング剤が好ましい。(メタ)アクリル系シランカップリング剤の具体例としては、3-メタクリロキシプロピルメチルジメトキシシラン、3-メタクリロキシプロピルトリメトキシシラン、3-メタクリロキシプロピルメチルジエトキシシラン、3-メタクリロキシプロピルトリエトキシシラン、及び、3-アクリロキシプロピルトリメトキシシランなどが挙げられる。
添加量は、重合性基を有する有機酸金属塩に対し0.1~20質量%が好ましい。
エネルギー線を使用する場合は、波長領域が0.0001~800nmの範囲のエネルギー線であれば特に限定されないが、かかるエネルギー線としては、α線、β線、γ線、X線、可視光線、紫外線、電子線等が挙げられる。これらのエネルギー線の中でも、波長領域が400~800nmの範囲の可視光線、50~400nmの範囲の紫外線及び0.01~0.002nmの範囲の電子線が、取り扱いが容易で、装置も普及しているので好ましい。
熱重合開始剤としては、例えば過硫酸塩、アゾ系重合開始剤、過酸化物、過酸化水素水が含まれる。熱重合開始剤を使用する場合には、重合性組成物中に、通常0.001~10重量%、好ましくは0.01~5重量%の割合で添加する。
エネルギー線を使用する場合は、波長領域が0.0001~800nmの範囲のエネルギー線であれば特に限定されないが、かかるエネルギー線としては、α線、β線、γ線、X線、可視光線、紫外線、電子線等が上げられる。これらの電離性放射線の中でも、50~400nmの範囲の紫外線及び0.01~0.002nmの範囲の電子線が好ましい。
一般的な熱硬化樹脂層や紫外線硬化樹脂、ハードコート樹脂をコートし、加熱や紫外線や電子線等により架橋させて形成することができる。具体的には、(メタ)アクリル樹脂や、エポキシ樹脂などである。また、これらの樹脂は、それぞれ単独で用いてもよいし、必要に応じて、併用してもよい。
紫外線で硬化して使用する場合は、光ラジカル開始剤、光カチオン開始剤、光酸発生剤を、また、光増感剤を混合して使用するのが好ましい。
また、熱硬化樹脂、紫外線硬化樹脂層、ハードコート樹脂層には、滑剤、スリップ剤、アンチ・ブロッキング剤、帯電防止剤、防曇剤、顔料、染料、無機また有機の充填剤等の各種添加剤を添加してもよい。
導電性を有する金属、セラミックス、カーボン材料を積層することで、電子部材として好適な積層フィルムが得られる。金属としては、特に限定されないが、金、銀、白金、銅、鉛などの金属が好適である。セラミックスでは、インジウムスズ酸化物、酸化亜鉛、酸化チタンなどが使用できる。
カーボン材料では、グラファイト、カーボンナノチューブ、グラフェンなどが使用できる。
導電層は、上記金属又はセラミックス又はカーボン材料の微粒子を水や有機溶媒に分散したペースト状の塗工液をコーティングしたり、蒸着やスパッタといった気相堆積法を用いて金属又はセラミックス又はカーボン材料の薄膜を作製することができる。
熱融着層を積層することで、熱ヒートシール可能な包装用フィルムとして好適な積層フィルムが得られる。このような熱融着層としては、通常熱融着層として公知のエチレン、プロピレン、ブテン-1、ヘキセン-1、4-メチル・ペンテン-1、オクテン-1等のα-オレフィンの単独若しくは共重合体、高圧法低密度ポリエチレン、線状低密度ポリエチレン(所謂LLDPE)、高密度ポリエチレン、ポリプロピレン、ポリプロピレンランダム共重合体、ポリブテン、ポリ4-メチル・ペンテン-1、低結晶性あるいは非晶性のエチレン・プロピレンランダム共重合体、エチレン・ブテン-1ランダム共重合体、プロピレン・ブテン-1ランダム共重合体等のポリオレフィンを単独若しくは2種以上の組成物、エチレン・酢酸ビニル共重合体(EVA)、エチレン・(メタ)アクリル酸共重合体あるいはその金属塩、EVAとポリオレフィンとの組成物等から得られる層である。
中でも、高圧法低密度ポリエチレン、線状低密度ポリエチレン(所謂LLDPE)、高密度ポリエチレン等のエチレン系重合体から得られる熱融着層が低温ヒートシール性、ヒートシール強度に優れるので好ましい。
このような熱融着層の厚さは通常1~50μm程度である。
本発明の電子部材10は、図1に示すように、ガラスや樹脂からなる基材12と、基材12上に搭載された素子14と、基材12上および素子14を覆う機能素子封止樹脂層16とからなる部材上に、基材(A)22とシリコン含有層(B)20と重合体層(C)18とからなる本発明の積層体を重合体層(C)18が部材側となるように配設して形成される。
素子14としては、液晶表示素子、有機EL等の素子、面状発光体、光デバイス等の有機機能素子、無機EL等の無機機能素子を挙げることができる。本発明の積層体は、特に、高度な水分・酸素バリアを要求される有機ELに対し、有効に用いることができる。
機能素子封止樹脂層16は、素子14を封止する樹脂層である。機能素子封止樹脂層16には、特に限定されないが、ヒートシール性熱可塑性樹脂や、または前記の熱硬化樹脂や紫外線硬化樹脂(以下、両者を「硬化樹脂」と表記することがある)が用いられる。
機能素子封止樹脂層16は、本発明の積層体における重合体層(C)18と、接着積層することができる。重合体層(C)18と封止樹脂層16の間に、必要に応じて接着層として硬化樹脂を用いることができる。
ヒートシール性熱可塑性樹脂層に用いられる熱可塑性樹脂は、特に限定されないが、中でも低密度ポリエチレン、エチレンと炭素数4ないし8のα-オレフィンとのランダム共重合体であるLLDPE、エチレン・プロピレン共重合体、エチレン・1-ブテン共重合体、エチレン-1-ヘキセン共重合体、1-オクテン共重合体などのエチレン・α-オレフィン共重合体エラストマー、プロピレン・エチレン共重合体、プロピレン・エチレン・1-ブテン共重合体などのプロピレン系エラストマー、ブテン・エチレン共重合体などのブテン系エラストマー、エチレン・酢酸ビニル共重合体、エチレン・アクリル酸共重合体などのエチレンと極性モノマーとの共重合体が好適例として例示される。
これらは、さらに、アクリル酸、マレイン酸、無水マレイン酸やエポキシ基含有モノマーなどの極性基含有モノマーで変性されたものでもよい。これらのヒートシール性熱可塑性樹脂は、ラミネートにより積層される方法、コーティングによりコート層として形成される方法がある。
このような層の中でも、コート剤としては、エチレン-ビニル酢酸共重合体、エチレン-酢酸ビニル共重合体、エチレン-アクリル酸共重合体、エチレン-メタクリル酸ナトリウム塩共重合体などのアイオノマーが例示される。
<評価方法>
(1)酸素透過率[ml/(m2・day・atm)]:積層体を、モコン社製OX-TRAN2/20を用いて、JIS K 7126に準じ、温度23℃、湿度90%R.H.の条件で測定した。
X線光電子分光(XPS)装置(「ESCALAB220iXL」,VG社製)を用い、膜深さ方向のシリコン含有層(B)の構成元素の組成比を測定した。(X線源 Al-Kα、アルゴンスパッタ SiO2換算0.05nm/スパッタ秒)
(4)折り曲げ試験(耐屈曲性試験)
実施例および比較例にある積層体のフィルム(10cm角)の中央に、半径5mmの円柱を置き、円柱側面を支点にフィルムを135°折り曲げた。この操作を100回繰り返した後、フィルムの外観を目視で観察した。続いて、前記評価方法にて酸素透過率を測定した。
(1)低圧容量結合プラズマ処理装置(ユーテック株式会社製)
SUS製の真空容器を用いた平行平板電極タイプの低圧容量結合プラズマ処理装置。一方は整合器を介して高周波電源に接続され、もう一方は接地されている。電極間隔は70mmとした。ポリシラザン膜は、接地されている電極側に設置して処理を行った。また、高周波電源側の対向している電極面の面積をプラズマ源の面積として投入電力密度を求めた。尚、電極は液体を流して温調する事ができ、ポリシラザン膜の基材を加熱する事ができる。
(2)低圧誘導結合プラズマ処理装置(ICP方式)
SUS製の筒型の真空容器に石英製の誘電体窓を介してシングルループのアンテナコイル設置した外部アンテナ方式の低圧誘導結合プラズマ処理装置。真空容器の上面全部が、誘導結合プラズマ源となっている。そのため、真空容器の内径からプラズマ源の面積を算出し、投入電力密度を求めた。アンテナコイルの一方は、整合器を介して高周波電源に接続され、もう一方は接地されている。ポリシラザン膜は、誘電体窓より200mm離した試料台上に設置した。
(3)誘電体バリア放電型プラズマ処理装置
ガラス製の真空容器に、ガラスで被覆された平行平板電極タイプの誘電体バリア放電型プラズマ処理装置。一方はインパルス型の高圧電源に接続され、もう一方は接地されている。電極間隔は5mmとした。ポリシラザン膜は、接地されている電極側に設置して処理を行った。また、高圧電源側の対向している電極面の面積をプラズマ源の面積として投入電力密度を求めた。
<溶液(W)作製>
アクリル酸亜鉛(アクリル酸のZn塩)水溶液(浅田化学社製、濃度30重量%(アクリル酸成分:20重量%、Zn成分10重量%))に、メチルアルコールで25重量%に希釈した光重合開始剤〔1-[4-(2-ヒドロキシエトキシ)-フェニル]-2-ヒドロキシ-2-メチル-1-プロパン-1-オン(チバ・スペシャリティ・ケミカルズ社製 商品名;イルガキュアー 2959)〕及び界面活性剤(花王社製 商品名;エマルゲン120)をアクリル酸に対して固形分比率でそれぞれ2%及び0.4%添加し、不飽和カルボン酸化合物Zn塩溶液(W)を作製した。
アクリル酸(単量体)(共栄社化学社製)を水で希釈して25%水溶液を作成した。この水溶液中のアクリル酸のカルボキシル基に対して等モルの水酸化リチウム一水和物(関東化学社製)を添加して、アクリル酸リチウム(アクリル酸のLi塩)水溶液を作製した。次に、作製したアクリル酸リチウム水溶液に、メチルアルコールで25重量%に希釈した光重合開始剤〔1-[4-(2-ヒドロキシエトキシ)-フェニル]-2-ヒドロキシ-2-メチル-1-プロパン-1-オン(チバ・スペシャリティ・ケミカルズ社製 商品名;イルガキュアー 2959)〕及び界面活性剤(花王社製 商品名;エマルゲン120)をアクリル酸に対して固形分比率でそれぞれ2%及び0.4%添加し、不飽和カルボン酸化合物のリチウム塩の溶液(X)を作製した。
アクリル酸(単量体)(共栄社化学社製)を水で希釈して25%水溶液を作成した。この水溶液中のアクリル酸のカルボキシル基に対して等モルの水酸化ナトリウム(関東化学社製)を添加して、アクリル酸ナトリウム(アクリル酸のNa塩)水溶液を作製した。次に、作製したアクリル酸ナトリウム水溶液に、メチルアルコールで25重量%に希釈した光重合開始剤〔1-[4-(2-ヒドロキシエトキシ)-フェニル]-2-ヒドロキシ-2-メチル-1-プロパン-1-オン(チバ・スペシャリティ・ケミカルズ社製 商品名;イルガキュアー 2959)〕及び界面活性剤(花王社製 商品名;エマルゲン120)をアクリル酸に対して固形分比率でそれぞれ2%及び0.4%添加し、不飽和カルボン酸化合物のナトリウム塩の溶液(Y)を作製した。
3-アクリロキシプロピルトリメトキシシラン(信越化学工業社製 商品名KBM5103)10gに精製水34.46gを加え、酢酸0.25gを加えて20分攪拌し、その後、イソプロピルアルコール34.46gを加えて3-アクリロキシプロピルトリメトキシシランの加水分解液である溶液(Z)を得た。
上記の不飽和カルボン酸化合物亜鉛塩溶液(W)及び不飽和カルボン酸化合物リチウム塩溶液(X)を75:25(モル比)の割合で混合し、溶液(A)を得た。
上記の不飽和カルボン酸化合物亜鉛塩溶液(W)及び不飽和カルボン酸化合物ナトリウム塩溶液(Y)を75:25(モル比)の割合で混合し、溶液(B)を得た。
2-アクリルアミド-2-メチルプロパンスルホン酸ナトリウム水溶液(ATBS 東亜合成(株)製)を水で希釈して25%水溶液を作成した。次に、メチルアルコールで25重量%に希釈した光重合開始剤〔1-[4-(2-ヒドロキシエトキシ)-フェニル]-2-ヒドロキシ-2-メチル-1-プロパン-1-オン(チバ・スペシャリティ・ケミカルズ社製 商品名;イルガキュアー 2959)〕を固形分比率でそれぞれ2%添加し、重合性スルホン酸化合物のナトリウム塩の溶液(C)を作製した。
<溶液(D)の作製>
上記の溶液(A)及び3-アクリロキシプロピルトリメトキシシラン(Z)を98:2(重量比)の割合で混合し、溶液(D)を得た。
基材(A)としてポリエチレンテレフタレート(PET)フィルム(厚さ50μm、「A4100」、東洋紡績株式会社製)上に、ポリシラザン(NL110A、AZエレクトロニックマテリアルズ株式会社製)の4.5wt%キシレン(脱水)溶液をバーコートし、150℃で90秒間乾燥して、厚さ0.15μmのポリシラザン膜を作製した。
真空プラズマ処理装置:低圧容量結合プラズマ処理装置(ユーテック株式会社製)
ガス:He
ガス流量:50mL/min
圧力:19Pa
電極単位面積あたりの印加電力:1.3W/cm2
周波数:13.56MHz
処理時間:30秒
酸素濃度:1ppm以下
水蒸気濃度:1ppm以下
なお、任意に複数箇所を選び、XPS測定を行ったところ、いずれの箇所においても図2の測定値と同様の結果が得られたことから、シリコン含有層(B)の表面全体に亘って窒素高濃度領域が形成されていることが確認された。
基材(A)としてポリエチレンテレフタレート(PET)フィルム(厚さ50μm、「A4100」、東洋紡績株式会社製)上に、ウレタンアクリレート(ウレタンアクリレート系UV硬化塗材(新中村化学社製 商品名 UA-100)を酢酸エチルで希釈し、メイヤーバーを用いて1.2g/m2(固形分)になるように塗布し、100℃、15秒間乾燥した。続いて、コート面にUV照射装置(アイグラフィック社製 EYE GRANDAGE 型式ECS 301G1)を用いて、UV強度:250mW/cm2、積算光量:117mJ/cm2の条件で光硬化し、アンダーコート層を設けた。さらにこの上にポリシラザン(NL110A、AZエレクトロニックマテリアルズ株式会社製)の4.5wt%キシレン(脱水)溶液をバーコートし、150℃で90秒間乾燥して、厚さ0.15μmのポリシラザン膜を作製した。その後、実施例1と同様の操作を行い、積層体を得た。得られた積層体の物性測定結果を表1に示す。
実施例2で使用した溶液Aを溶液Bに変更し、その他実施例2と同様の操作を行い、積層体を得た。得られた積層体の物性測定結果を表1に示す。
<実施例4>
実施例2で使用した溶液Aを溶液Cに変更し、その他実施例2と同様の操作を行い、積層体を得た。得られた積層体の物性測定結果を表1に示す。
実施例2で使用した溶液Aを溶液Dに変更し、その他実施例2と同様の操作を行い、積層体を得た。得られた積層体の物性測定結果を表1に示す。
実施例2と同様に塗工・乾燥してポリシラザン膜を調製し、実施例2のプラズマ処理を下記条件に変更して低圧プラズマ処理を施した。
真空プラズマ処理装置:低圧容量結合プラズマ処理装置(ユーテック株式会社製)
ガス:Ar
ガス流量:50mL/min
圧力:19Pa
電極単位面積あたりの印加電力:1.3W/cm2
周波数:13.56MHz
処理時間:5分
酸素濃度:1ppm以下
水蒸気濃度:1ppm以下
その後、実施例2と同様にシリコン含有層(B)の上に重合体層(C)を作製し、積層体を得た。得られた積層体の物性測定結果を表1に示す。
実施例2と同様に塗工・乾燥してポリシラザン膜を調製し、実施例2のプラズマ処理を下記条件に変更して低圧プラズマ処理を施した。
プラズマ処理装置:低圧容量結合プラズマ処理装置(ユーテック株式会社製)
ガス:He+H2(H2濃度:6vol%)
全圧力:19Pa
投入電力密度:1.3W/cm2
周波数:13.56MHz
処理時間: 60秒
酸素濃度:1ppm以下
水蒸気濃度:1ppm以下
その後、実施例2と同様にシリコン含有層(B)の上に重合体層(C)を作製し、積層体を得た。得られた積層体の物性測定結果を表1に示す。
実施例2と同様に塗工・乾燥してポリシラザン膜を調製し、実施例2のプラズマ処理を下記条件に変更して低圧プラズマ処理を施した。
プラズマ処理装置:低圧容量結合プラズマ処理装置(ユーテック株式会社製)
ガス:Ar+H2(H2濃度:6vol%)
全圧力:19Pa
投入電力密度:1.3W/cm2
周波数:13.56MHz
処理時間: 30秒
酸素濃度:1ppm以下
水蒸気濃度:1ppm以下
その後、実施例2と同様にシリコン含有層(B)の上に重合体層(C)を作製し、積層体を得た。得られた積層体の物性測定結果を表1に示す。
実施例2と同様に塗工・乾燥してポリシラザン膜を調製し、実施例2のプラズマ処理を下記条件に変更して低圧プラズマ処理を施した。
プラズマ処理装置:低圧誘導結合プラズマ処理装置(自作):ICP方式
ガス:He+H2(H2濃度:6vol%)
圧力:20Pa
投入電力密度: 2W/cm2 (4000W、プラズマ源の面積Φ250mm)
周波数: 13.56MHz
処理時間: 20秒
酸素濃度:1ppm以下
水蒸気濃度:1ppm以下
その後、実施例2と同様にシリコン含有層(B)の上に重合体層(C)を作製し、積層体を得た。得られた積層体の物性測定結果を表1に示す。
実施例2と同様に塗工・乾燥してポリシラザン膜を調製し、実施例2のプラズマ処理を下記条件に変更して大気圧近傍プラズマ処理を施した。
プラズマ処理装置:誘電体バリア放電型プラズマ処理装置(自作)
ガス:Ar
圧力:50kPa
基材加熱温度:室温
投入電力密度:0.4W/cm2
周波数:10kHz
処理時間: 600秒
酸素濃度:1ppm以下
水蒸気濃度:1ppm以下
その後、実施例2と同様にシリコン含有層(B)の上に重合体層(C)を作製し、積層体を得た。得られた積層体の物性測定結果を表1に示す。
基材(A)としてポリエチレンテレフタレート(PET)フィルム(厚さ50μm、「A4300」、東洋紡績株式会社製)上に、触媒-CVD装置により厚さ50ナノメータ(nm)の窒素酸化珪素膜を形成させた。
その後、前記の溶液(A)を2.8g/m2になるように塗布し、熱風乾燥器を使用して温度;60%、時間;30秒の条件で乾燥した。この後速やかに塗布面を上にしてステンレス板に固定し、UV照射装置(アイグラフィック社製 EYE GRANDAGE 型式ECS 301G1)を用いて、UV強度190mW/cm2、積算光量250mJ/cm2の条件で紫外線を照射して重合を行った後、得られたガスバリア性積層フィルムを熱板の上に載置して加熱処理し、積層体を得た。加熱処理の条件は、熱板の温度200℃、保持時間60分である。得られた積層体の物性測定結果を表1に示す。
基材(A)として、ポリエチレンテレフタレート(PET)フィルム(厚さ50μm、「A4300」、東洋紡績株式会社製)上に、ウレタンアクリレート(ウレタンアクリレート系UV硬化塗材(新中村化学社製 商品名 UA-100))を酢酸エチルで希釈し、メイヤーバーを用いて1.2g/m2(固形分)になるように塗布し、100℃、15秒間乾燥した。続いて、コート面にUV照射装置(アイグラフィック社製 EYE GRANDAGE 型式ECS 301G1)を用いて、UV強度:250mW/cm2、積算光量:117mJ/cm2の条件で光硬化し、アンダーコート層を設けた。
その後、比較例1と同様の操作を行ない、積層体を得た。得られた積層体の物性測定結果を表1に示す。
基材(A)として、ポリエチレンテレフタレート(PET)フィルム(厚さ50μm、「A4300」、東洋紡績株式会社製)上に、ウレタンアクリレート(ウレタンアクリレート系UV硬化塗材(新中村化学社製 商品名 UA-100))を酢酸エチルで希釈し、メイヤーバーを用いて1.2g/m2(固形分)になるように塗布し、100℃、15秒間乾燥した。
このポリシラザン(NL110A、AZエレクトロニックマテリアルズ株式会社製)の4.5wt%キシレン(脱水)溶液をバーコートし、150℃で90秒間乾燥して、厚さ0.15μmのポリシラザン膜を作製した。このポリシラザン膜に実施例2と同様の方法で低圧プラズマ処理を実施した。物性測定結果を表1に示す。
基材(A)として、ポリエチレンテレフタレート(PET)フィルム(厚さ50μm、「A4300」、東洋紡績株式会社製)上に、ウレタンアクリレート(ウレタンアクリレート系UV硬化塗材(新中村化学社製 商品名 UA-100))を酢酸エチルで希釈し、メイヤーバーを用いて1.2g/m2(固形分)になるように塗布し、100℃、15秒間乾燥した。
シリコン含有層(B)を介さず、前記の溶液(A)を2.8g/m2になるように塗布し、熱風乾燥器を使用して温度;60℃、時間;30秒の条件で乾燥した。この後速やかに塗布面を上にしてステンレス板に固定し、UV照射装置(アイグラフィック社製 EYE GRANDAGE 型式ECS 301G1)を用いて、UV強度190mW/cm2、積算光量250mJ/cm2の条件で紫外線を照射して重合を行った後、得られたガスバリア性積層フィルムを熱板の上に載置して加熱処理し、重合体層(C)を得た。加熱処理の条件は、熱板の温度200℃、保持時間60分である。物性測定結果を表1に示す。
基材(A)として、ポリエチレンテレフタレート(PET)フィルム(厚さ50μm、「A4300」、東洋紡績株式会社製)上に、ウレタンアクリレート(ウレタンアクリレート系UV硬化塗材(新中村化学社製 商品名 UA-100)を酢酸エチルで希釈し、メイヤーバーを用いて1.2g/m2(固形分)になるように塗布し、100℃、15秒間乾燥した。
このポリシラザン(NL110A、AZエレクトロニックマテリアルズ株式会社製)の4.5wt%キシレン(脱水)溶液をバーコートし、150℃で90秒間乾燥して、厚さ1.15μmのポリシラザン膜を作製した。 このポリシラザン膜に実施例2と同様の方法で低圧プラズマ処理を実施した。物性測定結果を表1に示す。
実施例2と同様に塗工・乾燥してポリシラザン膜を調製し、実施例2のプラズマ処理を下記条件に変更して大気圧近傍プラズマ処理を施した。
プラズマ処理装置: 大気圧プラズマ処理装置(APT-02、積水化学株式会社製)
ガス:Ar
圧力:大気圧
基材加熱温度:室温(23℃)
投入電力密度:1.3W/cm2
周波数:30kHz
処理時間: 600秒
酸素濃度: 20%(200,000ppm) at 23℃
水蒸気濃度: 50%RH at 23℃
その後、実施例2と同様にシリコン含有層(B)の上に重合体層(C)を作製し、積層体を得た。得られた積層体の物性測定結果を表1に示す。
また、実施例2と、比較例3、4および5との比較から、実施例2のように、基材(A)とシリコン含有層(B)と重合体層(C)の三つをこの順番で積層することによって初めて、それぞれ単層では発現しえない、非常に高い酸素または水蒸気バリア性が相乗的に発現するとともに良好な耐屈曲性を示すことが分かった。また、比較例5のようにシリコン含有層の膜厚が大きい場合、折り曲げ試験後、目視でクラックが発生しており、酸素バリア性が低下していた。一方、実施例1~10の積層体は、同じ膜厚でも、折り曲げ試験後もクラック発生なく、酸素バリア性は維持しており、フレキシブルであることが分かった。さらに、比較例6のように、高い酸素及び水蒸気雰囲気でプラズマ処理した場合、すなわち、N/(N+O)=0となる窒素不含のシリコン含有層(B)を使用した場合、実施例のような高い酸素及び水蒸気バリア性が発現しないことも確認された。
Claims (21)
- 基材(A)と、前記基材(A)の少なくとも一方の面に順に積層された、シリコン含有層(B)と、重合性基を有する有機酸金属塩から得られる重合体層(C)と、からなり、
前記シリコン含有層(B)は、珪素原子と窒素原子、または珪素原子と窒素原子と酸素原子、または珪素原子と窒素原子と酸素原子と炭素原子とからなる窒素高濃度領域を有し、
前記窒素高濃度領域は、前記基材(A)上に形成されたポリシラザン膜に酸素濃度5%以下および/または室温23℃における相対湿度30%以下でエネルギー線照射を行い、当該膜の少なくとも一部を変性することにより形成される、積層体。 - 前記窒素高濃度領域は、X線光電子分光法により測定した下記式(1)で表される窒素原子の組成比が、0.01以上、1以下の範囲である、請求項1に記載の積層体。
式(1):窒素原子の組成比/(酸素原子の組成比+窒素原子の組成比) - 前記ポリシラザン膜は、ポリシラザン含有溶液を、バーコート法、ロールコート法、グラビアコート法、スプレーコート法、エアナイフコート法、スピンコート法、ディップコート法、から選ばれる方法で前記基材(A)上に塗布することにより形成される、請求項1または2に記載の積層体。
- 前記重合体層(C)は、前記基材(A)上に形成された、前記窒素高濃度領域を有する前記シリコン含有層(B)上に、前記重合性基を有する有機酸金属塩膜を形成し、前記有機酸金属塩膜を紫外線、電子線または熱により重合して得られる、請求項1乃至3のいずれかに記載の積層体。
- 前記エネルギー線照射は、プラズマ照射により行われる、請求項1乃至4のいずれかに記載の積層体。
- 前記プラズマ照射は、不活性ガス、希ガスまたは還元ガスから選ばれる雰囲気にて行われる、請求項5に記載の積層体。
- 前記プラズマ照射は、酸素濃度5000ppm以下、かつ水蒸気濃度(室温23℃における水蒸気分圧/大気圧)8400ppm以下で行われる、請求項5または6に記載の積層体。
- 前記ポリシラザン膜は、ペルヒドロポリシラザン、オルガノポリシラザン、およびこれらの誘導体よりなる群から選択される1種以上である、請求項1乃至7のいずれかに記載の積層体。
- 前記有機酸金属塩は、カルボン酸、スルホン酸、メルカプト酸から選択される1種以上の有機酸の金属塩である、請求項1乃至8のいずれかに記載の積層体。
- 前記重合性基が、ビニル基、エポキシ基、メルカプト基、ウレイド基、スルフィド基、イソシアネート基、アミノ基、水酸基、ハロゲン原子、オキサゾリン基、カルボジイミド基またはそれらの誘導体から選択される1種以上の重合性基である、請求項1乃至9のいずれかに記載の積層体。
- 前記有機酸金属塩を形成する金属が、リチウム、ナトリウム、マグネシウム、カルシウム、亜鉛及びバリウムから選ばれる少なくとも1種以上の金属であることを特徴とする、請求項1乃至10のいずれかに記載の積層体。
- 前記有機酸金属塩は、重合性基としてビニル基を有するカルボン酸化合物の金属塩である、請求項1乃至11のいずれかに記載の積層体。
- 前記有機酸金属塩は、アクリル酸、メタアクリル酸、マレイン酸、イタコン酸から選ばれる有機酸の金属塩である、請求項12に記載の積層体。
- 前記有機酸金属塩は、重合性基としてビニル基を有するスルホン酸化合物の金属塩である、請求項1乃至11のいずれかに記載の積層体。
- 前記スルホン酸化合物は、ビニルスルホン酸、アリルスルホン酸、メタアリルスルホン酸、スルホン酸アクリレート、スルホン酸アクリルアミド、スルホン酸メタアクリレート、スチレンスルホン酸、イソプレンスルホン酸から選ばれる、請求項14に記載の積層体。
- 前記重合体層(C)は、更にシランカップリング剤を含んでなる、請求項1乃至15のいずれかに記載の積層体。
- 有機エレクトロルミネッセンス素子、電子ペーパー表示素子、液晶表示素子から選ばれる素子を含む部材と、重合体層(C)が該部材側となるように配設された請求項1乃至16のいずれかに記載の積層体とからなる、電子部材。
- 基材(A)の少なくとも一方の面にポリシラザン膜を形成する工程と、
前記ポリシラザン膜に酸素濃度5%以下および/または室温23℃における相対湿度30%以下でエネルギー線照射を行い当該膜の少なくとも一部を変性し、珪素原子と窒素原子、または珪素原子と窒素原子と酸素原子、または珪素原子と窒素原子と酸素原子と炭素原子とからなる窒素高濃度領域を含むシリコン含有層(B)を形成する工程と、
前記シリコン含有層(B)上に重合性基を有する有機酸金属塩から得られる重合体層(C)を形成する工程と、
を含む積層体の製造方法。 - 前記窒素高濃度領域は、X線光電子分光法により測定した下記式(1)で表される窒素原子の組成比が、0.01以上、1以下の範囲である、請求項18に記載の積層体の製造方法。
式(1):窒素原子の組成比/(酸素原子の組成比+窒素原子の組成比) - 前記エネルギー線照射は、プラズマ照射により行われる、請求項18または19に記載の積層体の製造方法。
- 前記プラズマ照射は、不活性ガス、希ガスまたは還元ガスから選ばれる雰囲気ガス中にて行われる請求項20に記載の積層体の製造方法。
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CN104379340B (zh) | 2016-06-15 |
TWI572492B (zh) | 2017-03-01 |
CN104379340A (zh) | 2015-02-25 |
EP2871054A1 (en) | 2015-05-13 |
KR20140036049A (ko) | 2014-03-24 |
EP2871054A4 (en) | 2016-03-02 |
EP2871054B1 (en) | 2017-04-05 |
JPWO2014007277A1 (ja) | 2016-06-02 |
KR101456420B1 (ko) | 2014-10-31 |
JP5469784B1 (ja) | 2014-04-16 |
US20150166751A1 (en) | 2015-06-18 |
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