JP5481370B2 - 大気圧プラズマ技術により被膜を作るための方法 - Google Patents
大気圧プラズマ技術により被膜を作るための方法 Download PDFInfo
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- JP5481370B2 JP5481370B2 JP2010501507A JP2010501507A JP5481370B2 JP 5481370 B2 JP5481370 B2 JP 5481370B2 JP 2010501507 A JP2010501507 A JP 2010501507A JP 2010501507 A JP2010501507 A JP 2010501507A JP 5481370 B2 JP5481370 B2 JP 5481370B2
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- HEQOJEGTZCTHCF-UHFFFAOYSA-N 2-amino-1-phenylethanone Chemical class NCC(=O)C1=CC=CC=C1 HEQOJEGTZCTHCF-UHFFFAOYSA-N 0.000 description 1
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- 239000012957 2-hydroxy-2-methyl-1-phenylpropanone Substances 0.000 description 1
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- GNSFRPWPOGYVLO-UHFFFAOYSA-N 3-hydroxypropyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCCCO GNSFRPWPOGYVLO-UHFFFAOYSA-N 0.000 description 1
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 description 1
- UITKHKNFVCYWNG-UHFFFAOYSA-N 4-(3,4-dicarboxybenzoyl)phthalic acid Chemical compound C1=C(C(O)=O)C(C(=O)O)=CC=C1C(=O)C1=CC=C(C(O)=O)C(C(O)=O)=C1 UITKHKNFVCYWNG-UHFFFAOYSA-N 0.000 description 1
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- SXNICUVVDOTUPD-UHFFFAOYSA-N CC1=CC(C)=CC(C)=C1C(=O)P(=O)C1=CC=CC=C1 Chemical compound CC1=CC(C)=CC(C)=C1C(=O)P(=O)C1=CC=CC=C1 SXNICUVVDOTUPD-UHFFFAOYSA-N 0.000 description 1
- 229920001651 Cyanoacrylate Polymers 0.000 description 1
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- 244000028419 Styrax benzoin Species 0.000 description 1
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- HGBBFIVJLKAPGV-UHFFFAOYSA-N [(2,4-dipentoxyphenyl)-(2,4,6-trimethylbenzoyl)phosphoryl]-(2,4,6-trimethylphenyl)methanone Chemical compound CCCCCOC1=CC(OCCCCC)=CC=C1P(=O)(C(=O)C=1C(=CC(C)=CC=1C)C)C(=O)C1=C(C)C=C(C)C=C1C HGBBFIVJLKAPGV-UHFFFAOYSA-N 0.000 description 1
- LFOXEOLGJPJZAA-UHFFFAOYSA-N [(2,6-dimethoxybenzoyl)-(2,4,4-trimethylpentyl)phosphoryl]-(2,6-dimethoxyphenyl)methanone Chemical compound COC1=CC=CC(OC)=C1C(=O)P(=O)(CC(C)CC(C)(C)C)C(=O)C1=C(OC)C=CC=C1OC LFOXEOLGJPJZAA-UHFFFAOYSA-N 0.000 description 1
- BEUGBYXJXMVRFO-UHFFFAOYSA-N [4-(dimethylamino)phenyl]-phenylmethanone Chemical compound C1=CC(N(C)C)=CC=C1C(=O)C1=CC=CC=C1 BEUGBYXJXMVRFO-UHFFFAOYSA-N 0.000 description 1
- GUCYFKSBFREPBC-UHFFFAOYSA-N [phenyl-(2,4,6-trimethylbenzoyl)phosphoryl]-(2,4,6-trimethylphenyl)methanone Chemical compound CC1=CC(C)=CC(C)=C1C(=O)P(=O)(C=1C=CC=CC=1)C(=O)C1=C(C)C=C(C)C=C1C GUCYFKSBFREPBC-UHFFFAOYSA-N 0.000 description 1
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229960002130 benzoin Drugs 0.000 description 1
- RWCCWEUUXYIKHB-UHFFFAOYSA-N benzophenone Chemical compound C=1C=CC=CC=1C(=O)C1=CC=CC=C1 RWCCWEUUXYIKHB-UHFFFAOYSA-N 0.000 description 1
- 239000012965 benzophenone Substances 0.000 description 1
- 229930006711 bornane-2,3-dione Natural products 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- ISAOCJYIOMOJEB-UHFFFAOYSA-N desyl alcohol Natural products C=1C=CC=CC=1C(O)C(=O)C1=CC=CC=C1 ISAOCJYIOMOJEB-UHFFFAOYSA-N 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000000539 dimer Substances 0.000 description 1
- 230000008034 disappearance Effects 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
- SUPCQIBBMFXVTL-UHFFFAOYSA-N ethyl 2-methylprop-2-enoate Chemical compound CCOC(=O)C(C)=C SUPCQIBBMFXVTL-UHFFFAOYSA-N 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 125000003709 fluoroalkyl group Chemical group 0.000 description 1
- XUCNUKMRBVNAPB-UHFFFAOYSA-N fluoroethene Chemical compound FC=C XUCNUKMRBVNAPB-UHFFFAOYSA-N 0.000 description 1
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical compound FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 description 1
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- 235000019382 gum benzoic Nutrition 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 239000012948 isocyanate Substances 0.000 description 1
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- 150000002576 ketones Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
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- FQPSGWSUVKBHSU-UHFFFAOYSA-N methacrylamide Chemical compound CC(=C)C(N)=O FQPSGWSUVKBHSU-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
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- QNILTEGFHQSKFF-UHFFFAOYSA-N n-propan-2-ylprop-2-enamide Chemical compound CC(C)NC(=O)C=C QNILTEGFHQSKFF-UHFFFAOYSA-N 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229920006254 polymer film Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- FBCQUCJYYPMKRO-UHFFFAOYSA-N prop-2-enyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCC=C FBCQUCJYYPMKRO-UHFFFAOYSA-N 0.000 description 1
- NHARPDSAXCBDDR-UHFFFAOYSA-N propyl 2-methylprop-2-enoate Chemical compound CCCOC(=O)C(C)=C NHARPDSAXCBDDR-UHFFFAOYSA-N 0.000 description 1
- 238000010526 radical polymerization reaction Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/46—Polymerisation initiated by wave energy or particle radiation
- C08F2/48—Polymerisation initiated by wave energy or particle radiation by ultraviolet or visible light
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D1/00—Processes for applying liquids or other fluent materials
- B05D1/62—Plasma-deposition of organic layers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D1/00—Processes for applying liquids or other fluent materials
- B05D1/02—Processes for applying liquids or other fluent materials performed by spraying
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/06—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to radiation
- B05D3/061—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to radiation using U.V.
- B05D3/065—After-treatment
- B05D3/067—Curing or cross-linking the coating
Description
− 基板を準備する、
− ガスの存在下に大気圧プラズマ放電を作る、
− 基板を前記大気圧プラズマ放電に少なくとも部分的に露出する、
− 被膜形成物質の液体エーロゾルを前記大気圧プラズマ放電中に導入し、それにより基板上に被膜を形成する、
− 基板を紫外光に露出することにより基板及び被膜を硬化する、
を含む。
プラズマ処理は、1.5kHzの特別に設計された平行なプレート設備で実施される。20×30cm2のポリ(エチレンテレフタレート)のシートが設備の下方の電極上に置かれる。活性化工程は40slmの流量の窒素下で0.8W/cm2の出力で30秒間実施される。出力は0.15W/cm2に下げられ、次いでエチルヘキシルアクリレートがエーロゾルの形で20slmの窒素流下でプラズマ領域に注入される。被膜付着は2分間実施される。被覆された基板は次いで約60sの時間の間、120mJ/cm2の出力でUVA(>320nm)照射に暴露される。
実施例2
実施例1に述べたように、基板はまず40slmの流量の窒素下で0.8W/cm2の出力で30秒間活性化工程に供される。出力は0.15W/cm2に下げられ、エチルヘキシルアクリレート(90重量%)及びペンタエリスリトールペンタ/ヘキサアクリレート(10重量%)の混合物が次いで20slmの窒素流下でエーロゾルの形でプラズマ領域に注入される。被膜付着は2分間実施される。被覆された基板は次いで120mJ/cm2の出力のUVA照射に暴露される。
実施例3
実施例1に述べたように、基板はまず40slmの流量の窒素下で0.8W/cm2の出力で30秒間活性化工程に供される。出力は0.15W/cm2に下げられ、エチルヘキシルアクリレート(90重量%)、ペンタエリスリトールペンタ/ヘキサアクリレート(8重量%)、4−(ジメチルアミノ)ベンゾフェノン(1重量%)及び4(ヒドロキシル)ベンゾフェノンの混合物が次いで20slmの窒素流下でエーロゾルの形でプラズマ領域に注入される。被覆付着は2分間実施される。被覆された基板は次いで120mJ/cm2の出力のUVA照射に暴露される。
実施例4
ポリプロピレン基板の接着性強化の典型例が述べられる。実施例1に示したように、ポリプロピレン基板はまず40slmの流量の窒素下で0.8W/cm2の出力で30秒間活性化工程に供される。出力は0.2W/cm2に下げられ、ヒドロキシエチルアクリレートが次いで20slmの窒素流下でエーロゾルの形でプラズマ領域に注入される。被膜付着は1分間実施される。被膜の赤外スペクトルは1615〜1640cm−1の非変換アクリレート結合の存在の減少を示す。300mm/分及び180°でのFinat 1法による剥離試験は、テープ付与後24時間で略1250cN/25mmの接着力を導くが、非被覆ポリプロピレン基板は略1000cN/25mmの接着力を示す。
もし同じプラズマ被覆基板が120mJ/cm2の出力で数秒間UVA照射に暴露されるなら、IRスペクトルはアクリレート官能によるバンドの完全な消失を示す。同じ条件下に実施された剥離試験は略1700cN/25mmの接着力を導く。従って、実施例4はUV照射の結果として被膜品質の効果的な強化を示す。
Claims (9)
- 基板を被覆する方法において、前記方法が次の工程:
− 基板(1)を準備する工程、
− ガスの存在下に大気圧プラズマ放電を作る工程、
− 基板を前記大気圧プラズマ放電に少なくとも部分的に露出する工程、
− 前記基板を前記大気圧プラズマ放電に少なくとも部分的に露出する工程の間に、被膜形成物質の液体エーロゾル(6)を前記大気圧プラズマ放電中に導入し、それにより基板上に被膜を形成する工程、
− 基板を紫外光に露出することにより基板及び被膜を硬化する工程、
を含むことを特徴とする方法。 - 前記紫外光の波長が290nm〜400nmであることを特徴とする請求項1に記載の方法。
- 前記硬化工程時の紫外光照射線量が5〜500mJ/cm2であることを特徴とする請求項1または2に記載の方法。
- 前記基板が、被膜形成物質の導入の前に、前記プラズマ放電により前処理されることを特徴とする請求項1〜3のいずれか一つに記載の方法。
- 前記被膜形成物質が、重合可能な前駆物質、または重合可能な前駆物質の幾つかの種類の混合物を含むことを特徴とする請求項1〜4のいずれか一つに記載の方法。
- 前記重合可能な前駆物質(単数または複数)がビニル化合物、アリル化合物、アルキン化合物、アクリレートまたはフッ素化アクリレート、メタクリレート及びフッ素化メタクリレートからなる群から選ばれることを特徴とする請求項5に記載の方法。
- 前記被膜形成物質が光重合開始剤をさらに含むことを特徴とする請求項5または6に記載の方法。
- 前記プラズマ放電が誘電体バリヤー放電であることを特徴とする請求項1〜7のいずれか一つに記載の方法。
- 前記ガスがHe,Ar,N2,CO2,O2,N2O,H2またはこれらの二つ以上の混合物からなる群から選ばれることを特徴とする請求項1〜8のいずれか一つに記載の方法。
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EP07105457A EP1978038A1 (en) | 2007-04-02 | 2007-04-02 | A method for producing a coating by atmospheric pressure plasma technology |
PCT/EP2008/053949 WO2008119823A1 (en) | 2007-04-02 | 2008-04-02 | A method for producing a coating by atmospheric pressure plasma technology |
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EP2589438B1 (en) * | 2011-11-07 | 2017-05-03 | Vlaamse Instelling voor Technologisch Onderzoek (VITO) | Plasma surface activation method and resulting object |
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