TWI574836B - 阻氣複合膜 - Google Patents
阻氣複合膜 Download PDFInfo
- Publication number
- TWI574836B TWI574836B TW103137349A TW103137349A TWI574836B TW I574836 B TWI574836 B TW I574836B TW 103137349 A TW103137349 A TW 103137349A TW 103137349 A TW103137349 A TW 103137349A TW I574836 B TWI574836 B TW I574836B
- Authority
- TW
- Taiwan
- Prior art keywords
- layer
- gas barrier
- composite film
- inorganic
- barrier composite
- Prior art date
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- 230000004888 barrier function Effects 0.000 title claims description 62
- 239000002131 composite material Substances 0.000 title claims description 45
- 239000010410 layer Substances 0.000 claims description 125
- 239000002346 layers by function Substances 0.000 claims description 62
- 229920000139 polyethylene terephthalate Polymers 0.000 claims description 46
- 239000005020 polyethylene terephthalate Substances 0.000 claims description 46
- 239000011241 protective layer Substances 0.000 claims description 40
- 239000010408 film Substances 0.000 claims description 39
- 239000000758 substrate Substances 0.000 claims description 27
- 229920001577 copolymer Polymers 0.000 claims description 23
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 21
- FJKROLUGYXJWQN-UHFFFAOYSA-N 4-hydroxybenzoic acid Chemical compound OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 claims description 12
- UHESRSKEBRADOO-UHFFFAOYSA-N ethyl carbamate;prop-2-enoic acid Chemical compound OC(=O)C=C.CCOC(N)=O UHESRSKEBRADOO-UHFFFAOYSA-N 0.000 claims description 12
- 229910010272 inorganic material Inorganic materials 0.000 claims description 11
- 239000011147 inorganic material Substances 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 9
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 8
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 7
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 7
- 230000009975 flexible effect Effects 0.000 claims description 7
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 7
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 7
- 229940090248 4-hydroxybenzoic acid Drugs 0.000 claims description 6
- LGXVIGDEPROXKC-UHFFFAOYSA-N 1,1-dichloroethene Chemical compound ClC(Cl)=C LGXVIGDEPROXKC-UHFFFAOYSA-N 0.000 claims description 5
- KAUQJMHLAFIZDU-UHFFFAOYSA-N 6-Hydroxy-2-naphthoic acid Chemical compound C1=C(O)C=CC2=CC(C(=O)O)=CC=C21 KAUQJMHLAFIZDU-UHFFFAOYSA-N 0.000 claims description 5
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 5
- 239000004696 Poly ether ether ketone Substances 0.000 claims description 4
- NWAIGJYBQQYSPW-UHFFFAOYSA-N azanylidyneindigane Chemical compound [In]#N NWAIGJYBQQYSPW-UHFFFAOYSA-N 0.000 claims description 4
- 229920002530 polyetherether ketone Polymers 0.000 claims description 4
- 239000011787 zinc oxide Substances 0.000 claims description 4
- 229910000449 hafnium oxide Inorganic materials 0.000 claims description 3
- WIHZLLGSGQNAGK-UHFFFAOYSA-N hafnium(4+);oxygen(2-) Chemical compound [O-2].[O-2].[Hf+4] WIHZLLGSGQNAGK-UHFFFAOYSA-N 0.000 claims description 3
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 claims description 3
- 229920000058 polyacrylate Polymers 0.000 claims description 3
- 229910001936 tantalum oxide Inorganic materials 0.000 claims description 3
- 229920002845 Poly(methacrylic acid) Polymers 0.000 claims description 2
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 2
- 150000004702 methyl esters Chemical class 0.000 claims description 2
- 150000002923 oximes Chemical class 0.000 claims description 2
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims description 2
- 239000004417 polycarbonate Substances 0.000 claims description 2
- 229920000515 polycarbonate Polymers 0.000 claims description 2
- 229920000728 polyester Polymers 0.000 claims description 2
- 229920000570 polyether Polymers 0.000 claims description 2
- 239000011112 polyethylene naphthalate Substances 0.000 claims description 2
- -1 polyethylene terephthalate Polymers 0.000 claims description 2
- 239000004926 polymethyl methacrylate Substances 0.000 claims description 2
- KCTAWXVAICEBSD-UHFFFAOYSA-N prop-2-enoyloxy prop-2-eneperoxoate Chemical compound C=CC(=O)OOOC(=O)C=C KCTAWXVAICEBSD-UHFFFAOYSA-N 0.000 claims description 2
- 239000010409 thin film Substances 0.000 claims description 2
- 229910000420 cerium oxide Inorganic materials 0.000 claims 2
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims 2
- HOSGXJWQVBHGLT-UHFFFAOYSA-N 6-hydroxy-3,4-dihydro-1h-quinolin-2-one Chemical group N1C(=O)CCC2=CC(O)=CC=C21 HOSGXJWQVBHGLT-UHFFFAOYSA-N 0.000 claims 1
- 230000002452 interceptive effect Effects 0.000 claims 1
- 239000007789 gas Substances 0.000 description 50
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 44
- 239000011248 coating agent Substances 0.000 description 29
- 238000000576 coating method Methods 0.000 description 29
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 21
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 20
- 239000001301 oxygen Substances 0.000 description 20
- 229910052760 oxygen Inorganic materials 0.000 description 20
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 15
- 230000035699 permeability Effects 0.000 description 15
- 238000010998 test method Methods 0.000 description 14
- JLTRXTDYQLMHGR-UHFFFAOYSA-N trimethylaluminium Chemical compound C[Al](C)C JLTRXTDYQLMHGR-UHFFFAOYSA-N 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 13
- 238000000231 atomic layer deposition Methods 0.000 description 12
- DWCMDRNGBIZOQL-UHFFFAOYSA-N dimethylazanide;zirconium(4+) Chemical compound [Zr+4].C[N-]C.C[N-]C.C[N-]C.C[N-]C DWCMDRNGBIZOQL-UHFFFAOYSA-N 0.000 description 11
- 238000000151 deposition Methods 0.000 description 10
- 230000008021 deposition Effects 0.000 description 10
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 9
- 239000002243 precursor Substances 0.000 description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 229910001873 dinitrogen Inorganic materials 0.000 description 8
- 239000003292 glue Substances 0.000 description 8
- 230000005540 biological transmission Effects 0.000 description 6
- 239000012528 membrane Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 239000006227 byproduct Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 4
- WSLDOOZREJYCGB-UHFFFAOYSA-N 1,2-Dichloroethane Chemical group ClCCCl WSLDOOZREJYCGB-UHFFFAOYSA-N 0.000 description 3
- 229930185605 Bisphenol Natural products 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 3
- 230000001070 adhesive effect Effects 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 230000007062 hydrolysis Effects 0.000 description 3
- 238000006460 hydrolysis reaction Methods 0.000 description 3
- 230000035515 penetration Effects 0.000 description 3
- 239000004033 plastic Substances 0.000 description 3
- 229920003023 plastic Polymers 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 2
- 229920002799 BoPET Polymers 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000011888 foil Substances 0.000 description 2
- 235000019253 formic acid Nutrition 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- 230000008676 import Effects 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- BOXYODYSHAHWPN-UHFFFAOYSA-N 4-hydroxybenzoic acid Chemical compound OC(=O)C1=CC=C(O)C=C1.OC(=O)C1=CC=C(O)C=C1 BOXYODYSHAHWPN-UHFFFAOYSA-N 0.000 description 1
- 229910018626 Al(OH) Inorganic materials 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000001568 sexual effect Effects 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Classifications
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
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- H10K30/80—Constructional details
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- H—ELECTRICITY
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
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- Engineering & Computer Science (AREA)
- Microelectronics & Electronic Packaging (AREA)
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Description
本發明係有關於氣體與水氣之阻氣膜，特別是有關於一種具可撓曲之阻氣複合膜。
軟性電子為將光電元件製作於軟性基材上的新技術領域。由於其產品具有輕、薄、易攜帶等人性化之方便特性，近年來逐漸受到全世界高科技界的重視。軟性電子元件一般以塑膠或金屬薄片為基材，而塑膠基材相較於金屬薄片基材具有透明及可撓性較高的優點，然而塑膠基材對水氣、氧氣的阻障效果不佳，將使得光電元件中的作用層及高功函數電極易與空氣中的水氣、氧氣反應，成為了軟性電子產品發展上的限制。所以，軟性電子產品通常需要有一具阻氣功能的複合膜來阻隔水氣或氧氣進入光電元件內部，以維持光電元件的效能及延長其生命週期。
因此，開發具透明、可撓特性之阻氣複合膜，為軟性電子產品發展中的關鍵之一。
本申請案揭露之阻氣複合膜，可達到可撓及有效阻絕水氣，保護基板避免水解，維持長期穩定性，可應用於軟
性電子元件之阻氣基材或背板，該軟性電子元件包括電子紙、有機發光二極體、有機太陽能電池或薄膜太陽能電池。
本案之實施例提供之阻氣複合膜，上述阻氣複合膜包括基材層，表面機能層設置在基材層的一面或兩面上，其中該表面機能層包括對-羥基苯甲酸(p-hydroxybenzoic acid)與6-羥基-2-萘甲酸(6-hydroxy-2-naphthoic acid)之第一共聚物或丙烯酸(acrylic acid)與二氯乙烯(vinylidene dichloride)之第二共聚物，以及無機堆疊層，設置在表面機能層上。
100、200‧‧‧阻氣複合膜
110‧‧‧基材層
120‧‧‧表面機能層
130‧‧‧無機堆疊層
131‧‧‧第一層無機材料層
132‧‧‧第二層無機材料層
133‧‧‧第三層無機材料層
240‧‧‧保護層
第1圖為本發明一實施例揭露之阻氣複合膜之示意圖。
第2圖為本發明一實施例揭露之無機堆疊層之示意圖。
第3圖為本發明一實施例揭露之阻氣複合膜之示意圖。
根據本發明之一實施例，如第1圖所示，本發明揭露的阻氣複合膜100包括基材層110，表面機能層120設置在基材層110的一面或兩面，其中表面機能層120可例如是包括對-羥基苯甲酸(p-hydroxybenzoic acid)與6-羥基-2-萘甲酸(6-hydroxy-2-naphthoic acid)之第一共聚物或丙烯酸(acrylic acid)與二氯乙烯(vinylidene dichloride)之第二共聚物，以及無機堆疊層130，設置在表面機能層120上。
根據本發明之一實施例中，基材層110可為一軟性可撓材料，例如包含聚對苯二甲酸乙二酯(PET)、聚萘二甲酸乙二酯(PEN)、聚甲基丙烯酸甲酯(PMMA)、聚碳酸酯(PC)、聚醚碸(PES)、聚醚醚酮(PEEK)、或上述之組合。
根據本發明之一實施例中，表面機能層120可以用來增加基材層110的阻氣性與穩定性，因此表面機能層係選擇比基材層具更低氣體穿透率且高緻密性之材料，並利用例如是貼合或塗佈之方式設置於基材層上，使表面機能層120和無機堆疊層130形成交互作用(synergy)增加阻氣性。在一實施例中，表面機能層120例如包括莫爾比60-80%對-羥基苯甲酸(p-hydroxybenzoic acid)與莫爾比40-20% 6-羥基-2-萘甲酸(6-hydroxy-2-naphthoic acid)所形成之第一共聚物，當第一共聚物之對-羥基苯甲酸的莫爾比越多則加工性越佳，當第一共聚物之6-羥基-2-萘甲酸莫爾比越多則阻氣性越好，但加工性越差。在另一實施例中表面機能層120例如包括莫爾比10-50%丙烯酸(acrylic acid)與莫爾比90-50%二氯乙烯(vinylidene dichloride)所形成之第二共聚物。當第二共聚物之丙烯酸的莫爾比越多則加工性越佳，當二氯乙烯的莫爾比越多則阻氣性越好，但加工性則越差。在一實施例表面機能層厚度可為0.1μm至100μm，另一實施中表面機能層厚度為1μm至50μm。
根據本發明的另一實施例中，無機堆疊層130係由多層無機層所組成，如第2圖所示，例如是先沉積第一層無
機材料層131，再沉積第二層無機材料層132，又沉積第三層無機材料層133，以此類推，可以沉積多達數百層以上，而上述無機堆疊層130可使用兩種無機材料進行交替鍍膜，形成超低針孔密度、百層以上之原子層厚度之沉積，為主要的阻氣層之一。在本發明之一實施例中，無機堆疊層130的材料係選自於氧化鋁、氧化鋅、氧化鋯、氧化鉿、氧化矽、與氮化銦所組成的無機材料中的至少2種所交互堆疊而成。例如亦可包括一層氧化鋁與一層選自於氧化鋅、氧化鋯、氧化鉿、氧化矽、與氮化銦所組成的無機材料中的至少1種材料所交互堆疊而成，又例如可以是以一層氧化鋁與一層氧化鋯交互堆疊而成數百層以上的無機堆疊層。在一實施例中，無機堆疊層130的鍍膜方式包括可以是以化學蒸氣沉積(CVD)、脈衝雷射蒸鍍(PLD)、或原子層沉積(ALD)等鍍膜方式進行一層又一層的無機材料層交互堆疊而成的無機堆疊層，在另一實施例中，無機堆疊層可以是以ALD鍍膜方式設置在上述的表面機能層之上，利用表面機能層和無機堆積層形成交互作用(synergy)增加複合膜的阻氣性。
根據本發明之一實施例中，每一層無機材料層的厚度為1Å至2Å且無機材料層的總厚度約為10nm至50nm。
以一層氧化鋁與一層氧化鋯交互堆疊而成的無機堆疊層130為例，每一層氧化鋁與每一層氧化鋯的進料時間比介於20：10至20：100，在另一實施例氧化鋁與氧化鋯的進料時間比以可為
20：20至20：30，先沉積一層氧化鋁再沉積一層氧化鋯，在氧化鋯層之上再沉積一層氧化鋁，以此類推，而形成數百層無機堆疊層。
根據本發明之一實施例中，請參照第3圖，阻氣複合膜200，更包括保護層240設置於該無機堆疊層130之上，其中該保護層包括聚氨酯丙烯酸酯、環氧丙烯酸酯、聚丙烯酸酯、聚酯、或其組合。上述保護層240則兼具阻氣及防止無機堆積層的刮傷，對無機堆積層有物理性保護效果，在本發明之一實施例中，上述保護層係將一聚氨酯丙烯酸酯UV膠，塗佈在上述無機堆疊層之上並以UV曝光機固化而成聚丙烯酸酯保護層，形成基材層110/表面機能層120/無機堆疊層130/保護層240之阻氣複合膜結構。在一實施例中，上述保護層的厚度可為1μm至8μm，而另一實施例中保護層的厚度亦可為1μm至5μm。
為了讓本發明之上述和其他目的、特徵、和優點能更明顯易懂，下文特舉數實施例配合所附圖示，作詳細說明如下：實施例一至三係採用表面機能層為對羥基苯甲酸與6-羥基-2-萘甲酸共聚物(p-hydroxybenzoic acid-6-hydroxy-2-naphthoic acid copolymer)所形成之第一共聚物，其中p-hydroxybenzoic acid莫爾比佔73%，6-hydroxy-2-naphthoic acid莫爾比佔27%)，厚度為50μm。
實施例一：PET/表面機能層/(Al2O3)200層/保護層在PET之基材層(厚度188μm)上，利用UV膠貼合上述表面機能層(厚度50μm)，並進行UV固化，形成PET/表面機能層結構。並以三甲基鋁(trimethyl aluminum,TMA)及水為前驅物，進行純氧化鋁無機堆疊層之原子層沈積。實驗步驟如下：
(1)導入TMA 20ms，吸附於表面機能層表面，並與表面機能層表面的-OH官能基反應，產生副產物甲烷(CH4)。此步驟的反應式為：Al(CH3)3(g)+ -O-H(s)→-O-Al(CH3)2(s)+CH4。
(2)通入氮氣6s，流量為200sccm，以移除未反應的TMA及甲烷。
(3)導入水蒸氣20ms，與表面機能層表面的TMA分子之甲基反應，產生副產物甲烷。此步驟的反應式如下：2 H2O(g)+ -O-Al(CH3)2(s)→-O-Al(OH)2(s)+2 CH4。
(4)通入氮氣6s，流量為200sccm，以移除未反應的水蒸氣及甲烷。
以上完成一層Al2O3鍍膜週期(cycle)，並重複此鍍膜週期循環步驟200次，完成PET/表面機能層上之純氧化鋁無機堆積層((Al2O3)200層)沈積。再以旋轉塗佈機於無機堆疊層表面塗佈聚氨酯丙烯酸酯UV膠，並以UV曝光機固化而形成保護層，從而形成PET/表面機能層/(Al2O3)200層/保護層之
阻氣複合膜結構。此實施例一完成之阻氣複合膜並以ASTM D3985測試方法下，其氧氣穿透率為0.05cc/m2-day-atm。
實施例二：PET/表面機能層/(ZrO2)200層/保護層同實施例一之PET/表面機能層結構，以tetrakis(dimethylamido)zirconium(IV)(TDMAZr)及水為前軀物，進行純氧化鋯無機堆疊層之原子層沈積，實驗步驟如下：
(1)導入TDMAZr 20ms，吸附於表面機能層表面，並與表面機能層表面的-OH官能基反應，產生副產物HN(CH3)2。此步驟的反應式為：Zr[N(CH3)2]4(g)+ -O-H(s)→-O-Zr[N(CH3)2]3(s)+HN(CH3)2。
(2)通入氮氣6s，流量為200sccm，以移除未反應的TDMAZr及HN(CH3)2。
(3)導入水蒸氣20ms，與表面機能層表面的TDMAZr分子之甲基反應，產生副產物HN(CH3)2。此步驟的反應式如下：3 H2O(g)+ -O-Zr[N(CH3)2]3(s)→-O-Zr(OH)3(s)+3HN(CH3)2。
(4)通入氮氣6s，流量為200sccm。
以上完成一層ZrO2鍍膜週期，並重複此鍍膜週期循環步驟200次，完成PET/表面機能層上之純氧化鋯無機堆疊層((ZrO2)200層)的沈積。以旋轉塗佈機於無機堆疊層表面塗佈聚氨酯丙烯酸酯UV膠，並以UV曝光機固化而形成保護層，從而形成PET/表面機能層/(ZrO2)200層/保護層之阻氣複
合膜結構。實施例二所完成之阻氣複合膜並以ASTM D3985測試方法，其氧氣穿透率為0.41cc/m2-day-atm。
實施例三：PET/表面機能層/(Al2O3/ZrO2)200層/保護層
同實施例一之PET/表面機能層結構，以TMA、TDMAZr及水為前軀物，進行氧化鋯與氧化鋁交錯堆疊之原子層沈積，實驗中每一鍍膜週期固定TMA進料時間為20ms，改變不同氧化鋯之進料量(X ms)以觀察對阻氣性的影響。無機堆疊層的鍍膜步驟如下：
(1)導入TMA共20ms。
(2)通入氮氣6s，流量為200sccm。
(3)導入水蒸氣20ms。
(4)通入氮氣6s，流量為200sccm。
(5)導入TDMAZr共X ms(X=2,5,10,20,30,50,100,200,
300,500)。
(6)通入氮氣6s，流量為200sccm。
(7)導入水蒸氣20ms。
(8)通入氮氣6s，流量為200sccm。
以上完成一次Al2O3/ZrO2交互鍍膜週期，重複此鍍膜週期循環步驟200次，完成PET/表面機能層上之氧化鋁與氧化鋯交錯之無機堆疊層((Al2O3/ZrO2)200層)沈積。隨後以旋轉塗佈機於無機堆疊層表面塗佈聚氨酯丙烯酸酯UV膠，並
以UV曝光機固化而形成保護層，從而形成PET/表面機能層/(Al2O3/ZrO2)200層/保護層之阻氣複合膜結構。
氧化鋁與氧化鋯進料時間可以為20：20至20：100，也可以為20：20至20：30。其中，當氧化鋁與氧化鋯進料時間比為20：30時，於ASTM D3985測試方法下之氧氣穿透率為0.02cc/m2-day-atm，於ASTM F1249測試方法下水蒸氣穿透率為<0.0005g/m2-day。於25℃ 60%RH下放置30天後，氧氣穿透率為0.05cc/m2-day-atm，水蒸氣穿透率為0.001g/m2-day。
茲將實施例一至三整理如表一：
實施例4-6採用之表面機能層為丙烯酸與二氯乙烯所形成之第二共聚物(acrylic-vinylidene dichloride copolymer)，其中丙烯酸莫爾比佔30%，二氯乙烯莫爾比佔70%，厚度為10μm。
實施例四：PET/表面機能層/(Al2O3)200層/保護層
實施例四之實驗條件同實施例一，差別在於實施例四之表面機能層為上述丙烯酸與二氯乙烯共聚物(acrylic-vinylidene dichloride copolymer)(厚度10μm)形成PET/表面機能層結構。並以TMA及水為前驅物，進行純氧化鋁無機堆疊層之原子層沈積，鍍膜步驟如實施例一。
以上完成一層Al2O3鍍膜週期(cycle)，並重複此鍍膜週期循環步驟200次，完成PET/表面機能層上之純氧化鋁無機堆疊層((Al2O3)200層)沈積。再以旋轉塗佈機於無機堆疊層表面塗佈聚氨酯丙烯酸酯UV膠，並以UV曝光機固化而形成保護層，從而形成PET/表面機能層/(Al2O3)200層/保護層之阻氣複合膜結構。此實施例四完成之阻氣複合膜並以ASTM D3985測試方法下之氧氣穿透率為0.05cc/m2-day-atm。
實施例五：PET/表面機能層/(ZrO2)200層/保護層
同實施例四之PET/表面機能層結構，並以TDMAZr及水為前軀物，進行純氧化鋯無機堆疊層之原子層沈積，鍍膜步驟如實施例二。
以上完成一層ZrO2鍍膜週期，並重複此鍍膜週期循環步驟200次，完成PET/表面機能層上之純氧化鋯無機堆疊層((ZrO2)200層)沈積。並以旋轉塗佈機於無機堆疊層表面塗佈聚氨酯丙烯酸酯UV膠，並以UV曝光機固化而形成保護層，從而形成PET/表面機能層/(ZrO2)200層/保護層之阻氣複合膜結構。實施例五所完成之阻氣複合膜並以ASTM D3985測試方法，其氧氣穿透率為4.5cc/m2-day-atm。
實施例六：PET/表面機能層/(Al2O3/ZrO2)200層/保護層
同實施例四之PET/表面機能層結構，並以TMA、TDMAZr及水為前軀物，進行氧化鋯與氧化鋁交錯的無機堆疊層之原子層沈積，實驗中每一鍍膜週期固定TMA進料時間為20ms，改變不同氧化鋯之進料量(X ms)以觀察對阻氣性的影響。無機堆疊層的鍍膜步驟如實施例三。
完成一次Al2O3/ZrO2交互鍍膜週期，並重複此鍍膜週期循環步驟200次，完成PET/表面機能層上之氧化鋯與氧化鋁交錯之無機堆疊層((Al2O3/ZrO2)200層)沈積。隨後以旋轉塗佈機於無機堆疊層表面塗佈聚氨酯丙烯酸酯UV膠，並以UV曝光機固化而形成保護層，從而形成PET/表面機能層
/(Al2O3/ZrO2)200層/保護層之阻氣複合膜結構。當氧化鋁與氧化鋯進料時間比為20：30時，於ASTM D3985測試方法下之氧氣穿透率為0.02cc/m2-day-atm，於ASTM F1249測試方法下水蒸氣穿透率為<0.0005g/m2-day。於25℃ 60% RH下放置30天後，氧氣穿透率為0.04cc/m2-day-atm，水蒸氣穿透率為0.001g/m2-day。
茲將實施例四至六整理如表二：
從表一及表二推知，當無機堆疊層為Al2O3/ZrO2交互堆疊之組合時，其阻氣效果優於純Al2O3或純ZrO2等單一材料堆疊。
為了證明本發明表面機能層對於阻氣之功效，進行了比較例一至六之驗證，說明如下：
比較例一：PET/Al2O3 200層/保護層
以PET為基材層(厚度188μm)。以TMA及水為前驅物，進行純氧化鋁無機堆疊層之原子層沈積，鍍膜步驟如實施例一。
重複此鍍膜週期循環步驟200次，完成PET基材層上之純氧化鋁無機堆疊層沈積。並以旋轉塗佈機於無機堆疊層表面塗佈聚氨酯丙烯酸酯UV膠，並以UV曝光機固化而形成保護層，從而形成PET/(Al2O3)200層/保護層之阻氣複合膜結構。此比較例一之阻氣複合膜結構於ASTM D3985測試方法下，其氧氣穿透率為0.06cc/m2-day-atm。
比較例二：PET/ZrO2 200層/保護層
以PET膜為基材，TDMAZr及水為前軀物，進行純氧化鋯無機堆疊層之原子層沈積，鍍膜步驟如實施例二。
重複此鍍膜週期循環步驟200次，完成PET基材上之純氧化鋯無機堆疊層沈積。並以旋轉塗佈機於無機堆疊層表面塗佈聚氨酯丙烯酸酯UV膠，並以UV曝光機固化而形成保護層，從而形成PET/(ZrO2)200/保護層之阻氣複合膜結構。此比較例二之阻氣複合膜結構於ASTM D3985測試方法下其氧氣穿透率為8cc/m2-day-atm。
比較例三：PET/(Al2O3/ZrO2)200層/保護層
以PET膜為基材，TMA、TDMAZr及水為前軀物，進行氧化鋯與氧化鋁交錯的無機堆疊層之原子層沈積，實驗中每一鍍膜週期固定TMA進料時間為20ms，改變不同氧化鋯之進料量(X ms)以觀察對阻氣性的影響。鍍膜步驟如實施例三。
以上完成一鍍膜週期，重複此鍍膜週期循環步驟200次，完成PET基材上氧化鋯與氧化鋁交錯的無機堆疊層沈積。隨後以旋轉塗佈機於無機層表面塗佈聚氨酯丙烯酸酯UV膠，並以UV曝光機固化而形成保護層，從而形成PET/(Al2O3/ZrO2)200層/保護層之阻氣複合膜結構。當氧化鋁與氧化鋯進料時間比為20：30時，於ASTM D3985測試方法下之氧氣穿透率為0.03cc/m2-day-atm，於ASTM F1249測試方法下水蒸氣穿透率為<0.0005g/m2-day。於25℃ 60% RH下放置30天後，氧氣穿透率為0.1cc/m2-day-atm，水蒸氣穿透率為0.01g/m2-day。
比較例四：PET/表面機能層(雙酚A與碳醯氯共聚物)/(Al2O3)200層/保護層
同實施例四之阻氣複合膜結構，比較例四僅將表面機能層改為雙酚A與碳醯氯共聚物(bisphenol A-phosgene copolymer)(厚度80μm)，於ASTM D3985測試方法下之氧氣穿透率為3cc/m2-day-atm。
比較例五：PET/表面機能層(雙酚A與碳醯氯共聚物)/(ZrO2)200層/保護層
同實施例五之阻氣複合膜結構，比較例五僅將表面機能層改為雙酚A與碳醯氯共聚物(bisphenol A-phosgene copolymer)(厚度80μm)，於ASTM D3985測試方法下之氧氣穿透率為8cc/m2-day-atm。
比較例六：PET/表面機能層(雙酚A與碳醯氯共聚物)/(Al2O3/ZrO2)200層/保護層
同實施例六之阻氣複合膜結構，比較例六僅將表面機能層改為雙酚A與碳醯氯共聚物(bisphenol A-phosgene copolymer)(厚度80μm)，於ASTM D3985測試方法下之氧氣穿透率為1.5cc/m2-day-atm。
將使用不同表面機能層所製作出阻氣複合膜，以ASTM D3985測試方法對氧氣穿透率的影響整理如表三：
氧氣穿透率(OTR)單位cc/m2-day-atm
當PET在長時間置放過程中會造成表面水解，使PET與無機層接觸面產生缺陷，因而降低阻氣性。本發明藉由引入比PET具更高阻氣性與親和性之表面機能層，來避免PET水解造成缺陷，且進一步提高阻氣性，增加長期存放穩定性。
茲將實施例及比較例整理如表四：
雖然本發明已以數個實施例揭露如上，然其並非
用以限定本發明，任何熟習此技術者，在不脫離本發明之精神和範圍內，當可作任意之更動與潤飾，因此本發明之保護範圍當視後附之申請專利範圍所界定者為準。
100‧‧‧阻氣複合膜
110‧‧‧基材層
120‧‧‧表面機能層
130‧‧‧無機堆疊層
Claims (12)
- 一種阻氣複合膜，包括：一基材層；一表面機能層，設置在該基材層的一面或兩面，其中該表面機能層包括對-羥基苯甲酸(p-hydroxybenzoic acid)與6-羥基-2-萘甲酸(6-hydroxy-2-naphthoic acid)之第一共聚物或丙烯酸(acrylic acid)與二氯乙烯(vinylidene dichloride)之第二共聚物；以及一無機堆疊層，設置在該表面機能層上。
- 如申請專利範圍第1項所述之阻氣複合膜，其中該基材層的材料包括聚對苯二甲酸乙二酯(PET)、聚萘二甲酸乙二酯(PEN)、聚甲基丙烯酸甲酯(PMMA)、聚碳酸酯(PC)、聚醚碸(PES)、聚醚醚酮(PEEK)、或上述之組合。
- 如申請專利範圍第1項所述之阻氣複合膜，其中該第一共聚物係由60-80莫耳%之對-羥基苯甲酸(p-hydroxybenzoic acid)與40-20莫耳%之6-羥基-2-萘甲酸(6-hydroxy-2-naphthoic acid)聚合而成。
- 如申請專利範圍第1項所述之阻氣複合膜，其中該第二共聚物係由10-50莫耳%丙烯酸(acrylic acid)與90-50莫耳%的二氯乙烯(vinylidene dichloride)聚合而成。
- 如申請專利範圍第1項所述之阻氣複合膜，其中該表面機能層的厚度為0.1μm至100μm。
- 如申請專利範圍第5項所述之阻氣複合膜，其中該表面 機能層的厚度為1μm至50μm。
- 如申請專利範圍第1項所述之阻氣複合膜，其中該無機堆疊層係選自氧化鋁、氧化鋅、氧化鋯、氧化鉿、氧化矽、與氮化銦所組成的無機材料中至少2種材料交互堆疊而成。
- 如申請專利範圍第7項所述之阻氣複合膜，其中該無機堆疊層包括氧化鋁與選自氧化鋅、氧化鋯、氧化鉿、氧化矽、與氮化銦所組成的無機材料中的至少1種材料交互堆疊而成。
- 如申請專利範圍第7項所述之阻氣複合膜，其中該無機堆疊層中的每一層厚度介於1Å至2Å之間，且該無機堆疊層的總厚度介於10nm至50nm之間。
- 如申請專利範圍第8項所述之阻氣複合膜，其中該無機堆疊層包括氧化鋁與氧化鋯交互堆疊而成。
- 如申請專利範圍第1項所述之阻氣複合膜，更包括一保護層設置於該無機堆疊層之上，其中該保護層包括聚氨酯丙烯酸酯、環氧丙烯酸酯、聚丙烯酸酯、聚酯、或其組合。
- 如申請專利範圍第1-11項中任一項所述之阻氣複合膜，係應用於軟性電子元件之阻氣基材或背板，其中該軟性電子元件包括電子紙、有機發光二極體、有機太陽能電池或薄膜太陽能電池。
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| CN108162547A (zh) * | 2018-01-10 | 2018-06-15 | 安徽科瑞克保温材料有限公司 | 一种高效节能冷库保温板及其制备方法 |
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