TWI476840B - Sealing method of electric device with transparent part, electric device with transparent part and thermosetting resin composition for sealing - Google Patents
Sealing method of electric device with transparent part, electric device with transparent part and thermosetting resin composition for sealing Download PDFInfo
- Publication number
- TWI476840B TWI476840B TW098107672A TW98107672A TWI476840B TW I476840 B TWI476840 B TW I476840B TW 098107672 A TW098107672 A TW 098107672A TW 98107672 A TW98107672 A TW 98107672A TW I476840 B TWI476840 B TW I476840B
- Authority
- TW
- Taiwan
- Prior art keywords
- sealing member
- oled
- resin composition
- thermosetting resin
- transmitting portion
- Prior art date
Links
- 238000007789 sealing Methods 0.000 title claims description 240
- 239000011342 resin composition Substances 0.000 title claims description 108
- 229920001187 thermosetting polymer Polymers 0.000 title claims description 81
- 238000000034 method Methods 0.000 title claims description 64
- 239000003822 epoxy resin Substances 0.000 claims description 40
- 229920000647 polyepoxide Polymers 0.000 claims description 40
- 238000000576 coating method Methods 0.000 claims description 31
- 239000011248 coating agent Substances 0.000 claims description 30
- 239000000758 substrate Substances 0.000 claims description 29
- 239000007822 coupling agent Substances 0.000 claims description 25
- 239000000203 mixture Substances 0.000 claims description 24
- 239000011521 glass Substances 0.000 claims description 21
- 229920005989 resin Polymers 0.000 claims description 19
- 239000011347 resin Substances 0.000 claims description 19
- 238000005304 joining Methods 0.000 claims description 15
- 239000003795 chemical substances by application Substances 0.000 claims description 14
- 238000001723 curing Methods 0.000 claims description 12
- DIOQZVSQGTUSAI-UHFFFAOYSA-N decane Chemical compound CCCCCCCCCC DIOQZVSQGTUSAI-UHFFFAOYSA-N 0.000 claims description 12
- 230000003647 oxidation Effects 0.000 claims description 11
- 238000007254 oxidation reaction Methods 0.000 claims description 11
- PXKLMJQFEQBVLD-UHFFFAOYSA-N bisphenol F Chemical compound C1=CC(O)=CC=C1CC1=CC=C(O)C=C1 PXKLMJQFEQBVLD-UHFFFAOYSA-N 0.000 claims description 10
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical class C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 9
- 239000011256 inorganic filler Substances 0.000 claims description 9
- 229910003475 inorganic filler Inorganic materials 0.000 claims description 9
- 239000007789 gas Substances 0.000 claims description 8
- 238000002347 injection Methods 0.000 claims description 8
- 239000007924 injection Substances 0.000 claims description 8
- 239000004848 polyfunctional curative Substances 0.000 claims description 8
- 125000003118 aryl group Chemical group 0.000 claims description 7
- FBHPRUXJQNWTEW-UHFFFAOYSA-N 1-benzyl-2-methylimidazole Chemical compound CC1=NC=CN1CC1=CC=CC=C1 FBHPRUXJQNWTEW-UHFFFAOYSA-N 0.000 claims description 6
- ULKLGIFJWFIQFF-UHFFFAOYSA-N 5K8XI641G3 Chemical compound CCC1=NC=C(C)N1 ULKLGIFJWFIQFF-UHFFFAOYSA-N 0.000 claims description 6
- 125000002723 alicyclic group Chemical group 0.000 claims description 5
- HECLRDQVFMWTQS-RGOKHQFPSA-N 1755-01-7 Chemical compound C1[C@H]2[C@@H]3CC=C[C@@H]3[C@@H]1C=C2 HECLRDQVFMWTQS-RGOKHQFPSA-N 0.000 claims description 4
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 claims description 4
- XXBDWLFCJWSEKW-UHFFFAOYSA-N dimethylbenzylamine Chemical compound CN(C)CC1=CC=CC=C1 XXBDWLFCJWSEKW-UHFFFAOYSA-N 0.000 claims description 4
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 4
- 229920003986 novolac Polymers 0.000 claims description 4
- 230000035515 penetration Effects 0.000 claims description 4
- 238000007650 screen-printing Methods 0.000 claims description 4
- 238000001029 thermal curing Methods 0.000 claims description 4
- 239000002966 varnish Substances 0.000 claims description 4
- MUTGBJKUEZFXGO-OLQVQODUSA-N (3as,7ar)-3a,4,5,6,7,7a-hexahydro-2-benzofuran-1,3-dione Chemical compound C1CCC[C@@H]2C(=O)OC(=O)[C@@H]21 MUTGBJKUEZFXGO-OLQVQODUSA-N 0.000 claims description 3
- KMOUUZVZFBCRAM-OLQVQODUSA-N (3as,7ar)-3a,4,7,7a-tetrahydro-2-benzofuran-1,3-dione Chemical compound C1C=CC[C@@H]2C(=O)OC(=O)[C@@H]21 KMOUUZVZFBCRAM-OLQVQODUSA-N 0.000 claims description 3
- XZKLXPPYISZJCV-UHFFFAOYSA-N 1-benzyl-2-phenylimidazole Chemical compound C1=CN=C(C=2C=CC=CC=2)N1CC1=CC=CC=C1 XZKLXPPYISZJCV-UHFFFAOYSA-N 0.000 claims description 3
- VILCJCGEZXAXTO-UHFFFAOYSA-N 2,2,2-tetramine Chemical compound NCCNCCNCCN VILCJCGEZXAXTO-UHFFFAOYSA-N 0.000 claims description 3
- LXBGSDVWAMZHDD-UHFFFAOYSA-N 2-methyl-1h-imidazole Chemical compound CC1=NC=CN1 LXBGSDVWAMZHDD-UHFFFAOYSA-N 0.000 claims description 3
- MWSKJDNQKGCKPA-UHFFFAOYSA-N 6-methyl-3a,4,5,7a-tetrahydro-2-benzofuran-1,3-dione Chemical compound C1CC(C)=CC2C(=O)OC(=O)C12 MWSKJDNQKGCKPA-UHFFFAOYSA-N 0.000 claims description 3
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims description 3
- LGRFSURHDFAFJT-UHFFFAOYSA-N Phthalic anhydride Natural products C1=CC=C2C(=O)OC(=O)C2=C1 LGRFSURHDFAFJT-UHFFFAOYSA-N 0.000 claims description 3
- 239000007983 Tris buffer Substances 0.000 claims description 3
- 150000004645 aluminates Chemical class 0.000 claims description 3
- IMUDHTPIFIBORV-UHFFFAOYSA-N aminoethylpiperazine Chemical compound NCCN1CCNCC1 IMUDHTPIFIBORV-UHFFFAOYSA-N 0.000 claims description 3
- ZRSKSQHEOZFGLJ-UHFFFAOYSA-N ammonium adipate Chemical compound [NH4+].[NH4+].[O-]C(=O)CCCCC([O-])=O ZRSKSQHEOZFGLJ-UHFFFAOYSA-N 0.000 claims description 3
- 235000019293 ammonium adipate Nutrition 0.000 claims description 3
- 239000012298 atmosphere Substances 0.000 claims description 3
- JHIWVOJDXOSYLW-UHFFFAOYSA-N butyl 2,2-difluorocyclopropane-1-carboxylate Chemical compound CCCCOC(=O)C1CC1(F)F JHIWVOJDXOSYLW-UHFFFAOYSA-N 0.000 claims description 3
- 230000005525 hole transport Effects 0.000 claims description 3
- JRMUNVKIHCOMHV-UHFFFAOYSA-M tetrabutylammonium bromide Chemical compound [Br-].CCCC[N+](CCCC)(CCCC)CCCC JRMUNVKIHCOMHV-UHFFFAOYSA-M 0.000 claims description 3
- BRKFQVAOMSWFDU-UHFFFAOYSA-M tetraphenylphosphanium;bromide Chemical compound [Br-].C1=CC=CC=C1[P+](C=1C=CC=CC=1)(C=1C=CC=CC=1)C1=CC=CC=C1 BRKFQVAOMSWFDU-UHFFFAOYSA-M 0.000 claims description 3
- XZZNDPSIHUTMOC-UHFFFAOYSA-N triphenyl phosphate Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)(=O)OC1=CC=CC=C1 XZZNDPSIHUTMOC-UHFFFAOYSA-N 0.000 claims description 3
- CHJMFFKHPHCQIJ-UHFFFAOYSA-L zinc;octanoate Chemical compound [Zn+2].CCCCCCCC([O-])=O.CCCCCCCC([O-])=O CHJMFFKHPHCQIJ-UHFFFAOYSA-L 0.000 claims description 3
- ZTTFLCGNQCKBRY-UHFFFAOYSA-N O=C1c2ccccc2-c2ccccc2P1=O Chemical compound O=C1c2ccccc2-c2ccccc2P1=O ZTTFLCGNQCKBRY-UHFFFAOYSA-N 0.000 claims description 2
- 125000004202 aminomethyl group Chemical group [H]N([H])C([H])([H])* 0.000 claims description 2
- 238000013007 heat curing Methods 0.000 claims description 2
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 claims 4
- LTVUCOSIZFEASK-MPXCPUAZSA-N (3ar,4s,7r,7as)-3a-methyl-3a,4,7,7a-tetrahydro-4,7-methano-2-benzofuran-1,3-dione Chemical compound C([C@H]1C=C2)[C@H]2[C@H]2[C@]1(C)C(=O)OC2=O LTVUCOSIZFEASK-MPXCPUAZSA-N 0.000 claims 2
- BGJSXRVXTHVRSN-UHFFFAOYSA-N 1,3,5-trioxane Chemical compound C1OCOCO1 BGJSXRVXTHVRSN-UHFFFAOYSA-N 0.000 claims 2
- SPSPIUSUWPLVKD-UHFFFAOYSA-N 2,3-dibutyl-6-methylphenol Chemical compound CCCCC1=CC=C(C)C(O)=C1CCCC SPSPIUSUWPLVKD-UHFFFAOYSA-N 0.000 claims 2
- 150000008064 anhydrides Chemical class 0.000 claims 2
- NKQIMNKPSDEDMO-UHFFFAOYSA-L barium bromide Chemical compound [Br-].[Br-].[Ba+2] NKQIMNKPSDEDMO-UHFFFAOYSA-L 0.000 claims 2
- 229910001620 barium bromide Inorganic materials 0.000 claims 2
- 125000001797 benzyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])* 0.000 claims 2
- 150000001622 bismuth compounds Chemical class 0.000 claims 2
- 235000010354 butylated hydroxytoluene Nutrition 0.000 claims 2
- 150000004985 diamines Chemical class 0.000 claims 2
- CZZYITDELCSZES-UHFFFAOYSA-N diphenylmethane Chemical compound C=1C=CC=CC=1CC1=CC=CC=C1 CZZYITDELCSZES-UHFFFAOYSA-N 0.000 claims 2
- DDFYFBUWEBINLX-UHFFFAOYSA-M tetramethylammonium bromide Chemical group [Br-].C[N+](C)(C)C DDFYFBUWEBINLX-UHFFFAOYSA-M 0.000 claims 2
- KSBAEPSJVUENNK-UHFFFAOYSA-L tin(ii) 2-ethylhexanoate Chemical compound [Sn+2].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O KSBAEPSJVUENNK-UHFFFAOYSA-L 0.000 claims 2
- OSNIIMCBVLBNGS-UHFFFAOYSA-N 1-(1,3-benzodioxol-5-yl)-2-(dimethylamino)propan-1-one Chemical compound CN(C)C(C)C(=O)C1=CC=C2OCOC2=C1 OSNIIMCBVLBNGS-UHFFFAOYSA-N 0.000 claims 1
- PMNLUUOXGOOLSP-UHFFFAOYSA-N 2-mercaptopropanoic acid Chemical class CC(S)C(O)=O PMNLUUOXGOOLSP-UHFFFAOYSA-N 0.000 claims 1
- DKIDEFUBRARXTE-UHFFFAOYSA-N 3-mercaptopropanoic acid Chemical compound OC(=O)CCS DKIDEFUBRARXTE-UHFFFAOYSA-N 0.000 claims 1
- 239000004841 bisphenol A epoxy resin Substances 0.000 claims 1
- 239000004842 bisphenol F epoxy resin Substances 0.000 claims 1
- 125000006222 dimethylaminomethyl group Chemical group [H]C([H])([H])N(C([H])([H])[H])C([H])([H])* 0.000 claims 1
- -1 amine compound Chemical class 0.000 description 22
- 230000008569 process Effects 0.000 description 19
- 238000004519 manufacturing process Methods 0.000 description 16
- 238000002834 transmittance Methods 0.000 description 14
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 description 11
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- 229910052751 metal Inorganic materials 0.000 description 5
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- 150000004714 phosphonium salts Chemical class 0.000 description 3
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
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- 238000007740 vapor deposition Methods 0.000 description 2
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- CCASNMYSKYYIDW-UHFFFAOYSA-N 1-(4-methylphenyl)-2,3-diphenyl-9H-fluorene trifluoromethanesulfonic acid Chemical compound FC(S(=O)(=O)O)(F)F.C1(=CC=CC=C1)C=1C(=C(C=2CC3=CC=CC=C3C2C1)C1=CC=C(C=C1)C)C1=CC=CC=C1 CCASNMYSKYYIDW-UHFFFAOYSA-N 0.000 description 1
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- KUBDPQJOLOUJRM-UHFFFAOYSA-N 2-(chloromethyl)oxirane;4-[2-(4-hydroxyphenyl)propan-2-yl]phenol Chemical compound ClCC1CO1.C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 KUBDPQJOLOUJRM-UHFFFAOYSA-N 0.000 description 1
- FRWYFWZENXDZMU-UHFFFAOYSA-N 2-iodoquinoline Chemical compound C1=CC=CC2=NC(I)=CC=C21 FRWYFWZENXDZMU-UHFFFAOYSA-N 0.000 description 1
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- 239000002841 Lewis acid Substances 0.000 description 1
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- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- GKXVJHDEWHKBFH-UHFFFAOYSA-N [2-(aminomethyl)phenyl]methanamine Chemical compound NCC1=CC=CC=C1CN GKXVJHDEWHKBFH-UHFFFAOYSA-N 0.000 description 1
- DRMAIBPBPJNFDH-UHFFFAOYSA-M [4-(2-methylpropyl)phenyl]-diphenylsulfanium;trifluoromethanesulfonate Chemical compound [O-]S(=O)(=O)C(F)(F)F.C1=CC(CC(C)C)=CC=C1[S+](C=1C=CC=CC=1)C1=CC=CC=C1 DRMAIBPBPJNFDH-UHFFFAOYSA-M 0.000 description 1
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- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 1
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- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- FAYMLNNRGCYLSR-UHFFFAOYSA-M triphenylsulfonium triflate Chemical compound [O-]S(=O)(=O)C(F)(F)F.C1=CC=CC=C1[S+](C=1C=CC=CC=1)C1=CC=CC=C1 FAYMLNNRGCYLSR-UHFFFAOYSA-M 0.000 description 1
- 230000037303 wrinkles Effects 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
- H10K50/00—Organic light-emitting devices
- H10K50/80—Constructional details
- H10K50/84—Passivation; Containers; Encapsulations
- H10K50/844—Encapsulations
-
- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on liquid crystals, e.g. single liquid crystal display cells
- G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
- G02F1/1333—Constructional arrangements; Manufacturing methods
- G02F1/1339—Gaskets; Spacers; Sealing of cells
-
- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F2202/00—Materials and properties
- G02F2202/02—Materials and properties organic material
- G02F2202/022—Materials and properties organic material polymeric
-
- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F2202/00—Materials and properties
- G02F2202/28—Adhesive materials or arrangements
Description
本發明係有關於一種具有透光部之電元件之密封方法及具有透光部之電元件，特別是有關於一種具有透光部之電元件之密封方法、具有透光部之電元件及適用於前述密封方法之熱硬化性樹脂組成物，可構造成電元件內之電裝置有效地受到保護，具有優異的壽命特性，並構造成有效地進行光的流入，具有優異的裝置特性者，可改善電元件之強度，特別是，適用於本發明之密封用熱硬化性樹脂組成物係黏度低，具有能適用在ODF(One Drop Fill)步驟(液晶滴入步驟)，塗佈量的控制容易，塗佈速度亦快速等製程上的優點，用在製程的費用少，可縮短硬化時間，光穿透度特性優異，亦可適用在頂部發射(Top emission)方式之顯示器，可截斷密封時流入面板之內部之氣體及水分，亦可適用在採用彩色濾光片之面板，在元件無劣化之狀態下可製作元件，硬化溫度低，可有效地保護不耐熱之物質，同時實現足夠的接著強度及防止著色等之特性，製造成本低，且經濟性優異。The present invention relates to a method for sealing an electrical component having a light transmitting portion and an electrical component having a light transmitting portion, and more particularly to a method for sealing an electrical component having a light transmitting portion, an electrical component having a light transmitting portion, and an application. The thermosetting resin composition of the sealing method can be configured such that the electric device in the electric component is effectively protected, has excellent life characteristics, and is configured to efficiently carry out light inflow, and has excellent device characteristics. In particular, the thermosetting resin composition for sealing which is suitable for use in the present invention has a low viscosity and can be applied to an ODF (One Drop Fill) step (liquid crystal dropping step), and the coating amount is easily controlled. The coating speed is also fast and the advantages of the process are small, the cost of the process is small, the hardening time can be shortened, the light transmittance is excellent, and the display can be applied to the top emission type display, and can be cut off when the seal is inflow. The gas and moisture inside the panel can also be applied to the panel using the color filter. The component can be fabricated without deterioration of the component, and the curing temperature is low, which is effective. The material is protected from heat-resistant substances, and at the same time, sufficient bonding strength and properties such as coloring are achieved, the manufacturing cost is low, and the economy is excellent.
一般，OLED或集成該元件之顯示器面板、LED或集成該元件之顯示器面板、或者是如太陽電池般之電元件係具有透光部，使其內部所存在之電裝置所產生之光線朝外部 傳遞，或將外部的光線傳遞至其內部所存在之電裝置，其等兩種中任一者係於進行光線傳遞之過程中而發光或吸光或透光者，在製造具有如此電裝置及透光部之電元件之過程中，包括有將上部密封構件及下部密封構件密封之密封步驟。Generally, an OLED or a display panel incorporating the component, an LED or a display panel integrated with the component, or an electrical component such as a solar cell has a light transmitting portion, such that the light generated by the electrical device existing inside faces the outside Transmitting, or transmitting external light to an electrical device present therein, either of which is in the process of transmitting light to illuminate or absorb or transmit light, in the manufacture of such an electrical device and through In the process of electrical components of the light portion, a sealing step of sealing the upper sealing member and the lower sealing member is included.
舉一具體例來說，對於作為前述電元件之一之顯示器元件利用OLED之顯示器面板係與現有的顯示器面板相比，可以較薄的厚度製作面板，在製作面板時，製程上的容易性佳，以具有作為下一世代顯示器之可撓性顯示器之製程上的適合性，因此作為下一世次顯示器而受到矚目。又，OLED顯示器非常明亮，且具有優異的彩色對比(contrast)及寬廣的視野角度(viewing angle)，具備高亮度及輕量性(重量輕)、低的驅動電壓等很多長處。As a specific example, the display panel using the OLED as one of the above-mentioned electrical components can be made with a thinner thickness than the conventional display panel, and the process is easy to manufacture when manufacturing the panel. In order to have suitability for the process of a flexible display as a display of the next generation, it has attracted attention as a next-generation display. Moreover, the OLED display is very bright, has excellent color contrast and a wide viewing angle, and has many advantages such as high brightness and light weight (light weight) and low driving voltage.
惟，OLED元件對水分極弱，金屬電極與有機物EL層間之接觸面受到水分的影響而造成剝離，金屬電極與氧及水分反應而容易劣化，藉此而衍生暗點(dark spot)、像素皺紋(pixel shrinkage)等，有使產率降低之缺點。However, the OLED element has extremely weak moisture, and the contact surface between the metal electrode and the organic EL layer is affected by moisture, causing peeling, and the metal electrode reacts with oxygen and moisture to be easily deteriorated, thereby deriving dark spots and pixel wrinkles. (pixel shrinkage) and the like have the disadvantage of lowering the yield.
為解決如此課題，而創作一種在元件製造時使用之密封方法，該方法在製作元件時，沿著元件的外部，在框架(frame)形態下塗佈樹脂組成物，將除氣組成物安裝在元件的上面，以製作元件者，在框架(frame)形態下在元件的外部塗佈樹脂組成物來製作元件時，在硬化反應時所產生的氣體會流入面板內部，不能形成完善的密封，造成暗點(dark spot)、像素皺紋(pixel shrinkage)等衍生，不研究開發出透 明除氣物質，就無法適用頂部發射(Top emission)方式。In order to solve such a problem, a sealing method is used in the manufacture of components, in which a resin composition is applied along the outside of the component in a frame form, and the degassing composition is mounted on the component. On the upper surface of the component, when a component is formed by coating a resin composition on the outside of the component in the form of a frame, gas generated during the hardening reaction flows into the panel, and a perfect seal cannot be formed. Derived from dark spots, pixel shrinkage, etc. The top emission method cannot be applied to the degassing material.
又，使用紅色(Red)、綠色(Green)、藍色(Blue)三種發光物質而製造之OLED元件，藍色(Blue)的壽命與紅色(Red)、綠色(Green)相比壽命較短，在顯示器的使用時間增加時，因藍色像素(Blue pixel)的劣化，而會觀察到有影像殘留之現象。Moreover, the OLED element manufactured using red, green, and blue light-emitting materials has a shorter life span than red (Red) and green (Green). When the use time of the display increases, the phenomenon of image sticking is observed due to the deterioration of the blue pixel.
為解決如此課題，而創作一種技術，即，將三種發光物質形成為3層，或者是將三種發光物質溶解在溶媒後製作元件，使其發出白光(white light)，通過彩色濾光片，以實現紅色(Red)、綠色(Green)、藍色(Blue)者。惟，如此製作元件時，廣為使用之光硬化型樹脂組成物係使光源通過彩色濾光片而到達組成物者，使得組成物不能吸收UV，而不能適用。In order to solve such a problem, a technique is created in which three kinds of luminescent substances are formed into three layers, or three kinds of luminescent substances are dissolved in a solvent to form an element to emit white light through a color filter. Realize red, green, and blue. However, when the device is fabricated in this manner, the widely used photocurable resin composition allows the light source to pass through the color filter to reach the composition, so that the composition cannot absorb UV, and is not applicable.
由如此層面來看時，對於將具有透光部之多種電元件能有效地密封之技術開發以及藉此製造劃時代地改善耐久性之電元件之開發需求仍然迫切。From such a level, there is still a demand for development of a technology for effectively sealing a plurality of electric components having a light transmitting portion and manufacturing an electric component for epoch-making improvement of durability.
因此，本發明之目的係於提供一種具有透光部之電元件之密封方法及具有透光部之電元件，其構造成有效地保護電元件內之電裝置，具有優異的壽命特命，使光的流入有效地進行，具有優異的裝置特性，可改善電元件之強度，特別是可適用於ODF(One Drop Fill)步驟，具有塗佈量之控 制容易，塗佈速度亦快速等製程上的優點，使花費在製程的費用少，可縮短硬化時間，光穿透度特性優異，亦適用於頂部發射(Top emission)方式之顯示器，可截斷密封時流入面板內部之氣體及水分，亦適用於採用彩色濾光片之面板，可在元件無劣化之狀態下製作元件，硬化溫度低，可有效地保護不耐熱之物質，可同時實現足夠的接著強度及防止著色等特性，製造成本低，且經濟性佳。Accordingly, it is an object of the present invention to provide a method of sealing an electrical component having a light transmitting portion and an electrical component having a light transmitting portion configured to effectively protect an electrical device within the electrical component, having an excellent life life and enabling light The inflow is effective, has excellent device characteristics, can improve the strength of the electrical component, and is particularly applicable to the ODF (One Drop Fill) step, with the control of the coating amount Easy to manufacture, fast coating speed, and other advantages in the process, the cost of the process is small, the hardening time can be shortened, the light transmittance is excellent, and it is also suitable for the top emission type display, which can cut off the seal. The gas and moisture flowing into the inside of the panel are also applicable to the panel using the color filter. The component can be fabricated without deterioration of the component, and the curing temperature is low, which can effectively protect the heat-resistant material and simultaneously achieve sufficient follow-up. Characteristics such as strength and coloring prevention, low manufacturing cost, and good economy.
又，本發明之另一目的係於提供一種密封用熱硬化性樹脂組成物，其黏度低，適用於ODF(One Drop Fill)步驟，具有塗佈量之控制容易，塗佈速度亦快速等製程上的優點，使花費在製程的費用少，可縮短硬化時間，光穿透度特性優異，亦適用於頂部發射(Top emission)方式之顯示器，可截斷密封時流入面板內部之氣體及水分，亦適用於採用彩色濾光片之面板，可在元件無劣化之狀態下製作元件，硬化溫度低，可有效地保護不耐熱之物質，同時可實現足夠的接著強度及防止著色等特性，製造成本低，且經濟性佳。Further, another object of the present invention is to provide a thermosetting resin composition for sealing which has low viscosity and is suitable for an ODF (One Drop Fill) step, and has an easy control of coating amount and a rapid coating speed. The advantages are that the cost of the process is small, the hardening time can be shortened, and the light transmittance is excellent. It is also suitable for the top emission type display, which can cut off the gas and moisture flowing into the panel inside the seal. Applicable to panels using color filters, which can be fabricated without deterioration of components. The curing temperature is low, which can effectively protect non-heat-resistant materials. At the same time, it can achieve sufficient bonding strength and color resistance, and has low manufacturing cost. And the economy is good.
為達成前述目的，本發明係提供一種具有透光部之電元件之密封方法，其係將下部密封構件與上部密封構件接合而形成之具有透光部之電元件密封之方法，包含有以下步驟，即：(a)以熱硬化性樹脂組成物全面地塗佈於上部密封構件之接合前最終下面或下部密封構件之接合前最終上面；(b)在將上部密封構件之塗佈面與下部密封構件之最終 上面或上部密封構件之最終下面與下部密封構件之塗佈面相接之狀態下將上部密封構件與下部密封構件接合；及(c)對前述業已接合之結合體加熱，使熱硬化性樹脂組成物硬化。In order to achieve the above object, the present invention provides a method of sealing an electric component having a light transmitting portion, which is a method of sealing an electric component having a light transmitting portion formed by joining a lower sealing member and an upper sealing member, and includes the following steps That is, (a) the thermosetting resin composition is applied over the entire surface of the upper sealing member before the final sealing of the lower or lower sealing member before bonding; (b) the coated surface of the upper sealing member and the lower portion The final part of the sealing member And bonding the upper sealing member to the lower sealing member in a state where the lower surface of the upper or upper sealing member is in contact with the coated surface of the lower sealing member; and (c) heating the bonded body to form a thermosetting resin Hardening of matter.
又，本發明係提供一種具有透光部之電元件，其包含有下部密封構件；與前述下部密封構件相隔之狀態下而位於前述下部密封構件之上部之上部密封構件；位於前述下部密封構件與前述上部密封構件之間之電裝置；及充填於前述上部密封構件與前述下部密封構件之接合面之間，且將前述電裝置包圍在內，將前述上部密封構件與前述下部密封構件接合之熱硬化性樹脂組成物之硬化體層，且使前述熱硬化性樹脂組成物之硬化體層形成透光部之部分或全部。Furthermore, the present invention provides an electric component having a light transmitting portion, comprising a lower sealing member; a sealing member located above the lower sealing member in a state of being spaced apart from the lower sealing member; and the lower sealing member being located An electric device between the upper sealing members; and a heat filled between the upper sealing member and the lower sealing member, and the electric device is surrounded by the upper sealing member and the lower sealing member The hardened layer of the curable resin composition, and the hardened layer of the thermosetting resin composition forms part or all of the light transmitting portion.
又，本發明係提供一種密封用熱硬化性樹脂組成物，其係於電元件或光元件之密封用樹脂組成物中，包含有：(a)環氧樹脂25~90重量份；(b)熱硬化劑9-70重量份；及，(c)硬化促進劑0.1~5重量份，且黏度為10-3000cps(25℃下)。Moreover, the present invention provides a thermosetting resin composition for sealing, which is a resin composition for sealing an electric element or an optical element, comprising: (a) 25 to 90 parts by weight of an epoxy resin; (b) The heat hardener is 9-70 parts by weight; and, (c) the hardening accelerator is 0.1 to 5 parts by weight, and the viscosity is 10-3000 cps (at 25 ° C).
依本發明之具有透光部之電元件及如此電元件之密封方法，構成為有效地保護電元件內之電裝置，具有優異之壽命特性，且構成為有效地進行光之流入，具有優異之元件特性，可改善電元件的強度，特別是，適用於本發明之密封用熱硬化性樹脂組成物係黏度低，具有適用於ODF(One Drop Fill)步驟，塗佈量的控制容易，塗佈速度亦快速 等製程上的優點，因此在製程上之費用少，可縮短硬化時間，光穿透特性佳，亦適用於頂部發射(Top emission)方式之顯示器，截斷密封時流入面板內部之氣體及水分，亦可適用於採用彩色濾光片之面板，可在元件無劣化之狀態下製作元件，硬化溫度低，有效地保護不耐熱之物質，同時實現足夠的接著強度及防止著色等之特性，具有製造成本低且經濟性優異之效果。The electric component having the light transmitting portion and the sealing method of the electric component according to the present invention are configured to effectively protect the electric device in the electric component, have excellent life characteristics, and are configured to efficiently perform light inflow, and are excellent. The element characteristics can improve the strength of the electric component. In particular, the thermosetting resin composition for sealing which is suitable for use in the present invention has a low viscosity, and is suitable for an ODF (One Drop Fill) step, and the coating amount is easily controlled. Speed is also fast The advantages of the process, so the cost of the process is small, the hardening time can be shortened, the light transmission characteristics are good, and it is also suitable for the top emission type display, and the gas and moisture flowing into the panel inside the seal are cut off. It can be applied to panels using color filters, which can be fabricated without deterioration of components, with low curing temperature, effectively protecting non-heat-resistant materials, and achieving sufficient bonding strength and coloring resistance, and manufacturing costs. Low and economical effects.
又，本發明之密封用熱硬化性樹脂組成物係黏度低，具有適用於ODF(One Drop Fill)步驟，塗佈量之控制容易，塗佈速度亦快等製程上之優點，因此製程上的費用少，可縮短硬化時間，光穿透特性佳，亦可適用於頂部發射(Top emission)方式之顯示器，截斷密封時流入面板內部之氣體及水分，亦可適用於採用彩色濾光片之面板，可在元件不劣化之狀態下製作元件，硬化溫度低，可有效地保護不耐熱之物質，同時實現足夠的接著強度及防止著色等特性，製造成本低且經濟性佳，特別是對於上部密封構件及下部密封構件皆為玻璃之元件，且對於具有將前述構件接著充填之型態之電元件或光元件密封時特別有效。Further, the thermosetting resin composition for sealing of the present invention has a low viscosity, and has an advantage of being suitable for an ODF (One Drop Fill) step, an easy control of a coating amount, and a coating speed, and the like. Low cost, shortened hardening time, good light transmission characteristics, can also be applied to top emission display, cut off gas and moisture flowing into the panel when sealed, and can also be applied to panels with color filters The device can be fabricated in a state where the component is not deteriorated, the curing temperature is low, the heat-resistant material can be effectively protected, and sufficient bonding strength and coloring prevention characteristics are achieved, and the manufacturing cost is low and the economy is good, especially for the upper seal. Both the member and the lower sealing member are elements of glass and are particularly effective for sealing electrical or optical elements having the form in which the aforementioned members are subsequently filled.
第1圖係本發明一實施型態之顯示器元件之模式圖。Fig. 1 is a schematic view showing a display element of an embodiment of the present invention.
第2及3圖係本發明一實施型態之密封方法之製程圖。2 and 3 are process diagrams of a sealing method according to an embodiment of the present invention.
本發明係有關於一種具有透光部之電元件之密封方法，更詳而言之，在將下部密封構件與上部密封構件接合而形成之具有透光部之電元件之密封方法中，包含有下列步驟，即：(a)將熱硬化性樹脂組成物全面地塗佈在上部密封構件之接合前最終下面或下部密封構件之接合前最終上面；(b)在上部密封構件之塗佈面與下部密封構件之最終上面、或上部密封構件之最終下面與下部密封構件之塗佈面相接之狀態下將上部密封構件與下部密封構件接合；及(c)對前述業已接合之結合體加熱，使熱硬化性樹脂組成物硬化。The present invention relates to a sealing method for an electric component having a light transmitting portion, and more particularly, a sealing method for an electric component having a light transmitting portion formed by joining a lower sealing member and an upper sealing member, The following steps are: (a) applying the thermosetting resin composition to the entire surface before the joining of the upper or lower sealing members before the joining of the upper sealing member; (b) coating the surface of the upper sealing member with The upper sealing member is joined to the lower sealing member in a state where the lower surface of the lower sealing member or the final lower surface of the upper sealing member is in contact with the coated surface of the lower sealing member; and (c) heating the previously joined combination, The thermosetting resin composition is cured.
即，前述具有透光部之電元件係一種電元件，即，經由發光、吸光或透光，以達成電元件之目的者，在內部有達成發光或吸光或透光之電裝置存在，具有構造成在如此電裝置與外部之間進行透光之透光部，其外部具有藉下部密封構件與上部密封構件而密封之構造。與此有關之具體例，諸如有OLED、LED本身(此時，電極或發光層等即為電裝置)，或集成其等而形成單一面板之顯示器面板(此時，OLED或LED等即為電裝置)，或利用其等之信號燈或電燈(此時，OLED或LED等即為電裝置)，或太陽電池(特別是染料感應式太陽電池)細胞單元之子模組(此時，太陽電池細胞單元等即為電裝置)，或將其等集成之太陽電池模組(此時，太陽電池子模組等即為電裝置)，或光連結端子或集成其等之中心模組等。That is, the electric component having the light transmitting portion is an electrical component, that is, an electric device that achieves light emission, light absorption, or light transmission through the light source, the light absorption, or the light transmission to achieve the purpose of the electrical component, and has a structure. The light transmitting portion that transmits light between the electric device and the outside has a structure in which the outside is sealed by the lower sealing member and the upper sealing member. Specific examples related to this are, for example, an OLED, an LED itself (in this case, an electrode or a light-emitting layer, etc.), or a display panel in which a single panel is integrated to form a single panel (in this case, an OLED or an LED is electrically Device), or a sub-module of a cell unit of a solar cell (especially a dye-sensing solar cell) using a signal lamp or an electric lamp (in this case, an OLED or an LED, etc.) (at this time, a solar cell cell unit) The solar cell module (that is, the solar cell sub-module or the like is an electric device), or the optical connection terminal or a central module integrated with the same, or the like.
其等各為了元件的構成，在下部密封構件或上部密封構件或其等兩側上形成所要求之電裝置，最後將其等結合，此時，上部密封構件係因應需要，在其下面形成所要求之裝置，形成上部密封構件之接合前最終下面(也有不形成任何物的型態)，以及，下部密封構件亦同樣形成下部密封構件之接合前最終上面，之後在其等上部密封構件之接合前最終下面或下部密封構件之接合前最終上面全面地塗佈熱硬化性樹脂組成物。此時，透過前述全面塗佈，內部的電裝置藉樹脂組成物而呈完全氣密之狀態。For each of the components, the required electrical devices are formed on both sides of the lower sealing member or the upper sealing member or the like, and finally they are combined. At this time, the upper sealing member is formed underneath as needed. The required device forms the final underside of the upper sealing member before joining (there is also a form in which no material is formed), and the lower sealing member also forms the final upper surface of the lower sealing member before joining, and then is joined at its upper sealing member. The thermosetting resin composition is finally applied over the entire front surface before the final lower or lower sealing member is joined. At this time, the internal electric device is completely airtight by the resin composition by the above-described overall coating.
在此，前述熱硬化性樹脂組成物，較佳的是包含有(a)環氧樹脂25~90重量份；(b)熱硬化劑9~70重量份；及(c)硬化促進劑0.1~5重量份，且黏度為10~3000cps(25℃下)時，因為可得到低的熱硬化溫度及高黏度，在硬化過程中使裝置的毀損達到最少，容易進行塗佈作業，所以為佳。Here, the thermosetting resin composition preferably contains (a) 25 to 90 parts by weight of the epoxy resin; (b) 9 to 70 parts by weight of the heat curing agent; and (c) a curing accelerator 0.1~ When 5 parts by weight and the viscosity is 10 to 3000 cps (at 25 ° C), since a low heat hardening temperature and a high viscosity can be obtained, the damage of the apparatus is minimized during the hardening process, and coating work is easy, so that it is preferable.
即，本發明之密封用熱硬化性樹脂組成物係於25℃下具有10~3000cps的黏度，較佳的是100~2,000cps，更佳的是100~1,000cps之黏度時，在將密封用熱硬化性樹脂組成物塗佈在密封構件時，具有可進行ODF(One Drop Fill)步驟，塗佈量的控制容易，且塗佈速度亦快速等製程上的優點，花費在製程上的費用亦少，可縮短硬化時間。That is, the thermosetting resin composition for sealing of the present invention has a viscosity of 10 to 3000 cps at 25 ° C, preferably 100 to 2,000 cps, more preferably 100 to 1,000 cps, and is used for sealing. When the thermosetting resin composition is applied to the sealing member, it has an ODF (One Drop Fill) step, the coating amount is easily controlled, and the coating speed is also fast, and the manufacturing process is expensive. Less, can shorten the hardening time.
又，本發明所適用之前述密封用熱硬化性樹脂組成物係連同環氧樹脂在內分散有熱硬化劑、硬化促進劑之低黏度之樹脂組成物，且選擇性地可更含有耦合劑或氧化防止劑。Further, the thermosetting resin composition for sealing according to the present invention is a low-viscosity resin composition in which a thermosetting agent and a curing accelerator are dispersed together with an epoxy resin, and optionally further contains a coupling agent or Oxidation inhibitor.
詳細說明本發明密封用熱硬化性樹脂組成物所使用之成分。The components used in the thermosetting resin composition for sealing of the present invention will be described in detail.
(1)環氧樹脂：適用於本發明之密封用熱硬化性樹脂組成物之環氧樹脂乃可舉出有雙酚A型環氧樹脂、雙酚F型環氧樹脂、氫化雙酚型環氧樹脂、脂環式環氧樹脂、芳香族環氧樹脂、清漆樹脂型、二環戊二烯型環氧樹脂等為例，其等具有環氧基之化合物可單獨或混合使用。又，前述具有環氧基之化合物之黏度係以100~1000cps為佳。(1) Epoxy Resin: The epoxy resin to be used in the thermosetting resin composition for sealing of the present invention includes bisphenol A type epoxy resin, bisphenol F type epoxy resin, and hydrogenated bisphenol type ring. Examples of the oxygen resin, the alicyclic epoxy resin, the aromatic epoxy resin, the varnish resin type, the dicyclopentadiene type epoxy resin, and the like, and the epoxy group-containing compound may be used singly or in combination. Further, the viscosity of the compound having an epoxy group is preferably from 100 to 1,000 cps.
(2)熱硬化劑：通常只要是可使用在用以將環氧樹脂熱硬化者即可使用，並無特別限定。以具體例而言，可使用二乙撐三胺、三乙撐四胺、N-胺基乙基哌嗪、二胺基二苯基甲烷、己二酸二醯肼等之聚胺系硬化劑；鄰苯二甲酸酐、四氫鄰苯二甲酸酐、六氫鄰苯二甲酸酐、甲基四氫鄰苯二甲酸酐、甲基六氫鄰苯二甲酸酐、甲基納迪克(methyl nadic)酸酐等之酸酐硬化劑；酚醛清漆樹脂型硬化劑；三噁烷三伸乙基硫醇等之聚硫醇硬化劑；苯甲基二甲胺、2,4,6-三(二甲基胺基甲基)苯酚等之第三胺化合物；2-甲基咪唑、2-乙基-4-甲基咪唑、1-苯甲基-2-甲基咪唑等之咪唑化合物等。又，亦可使用其他固體分散型之潛在性硬化劑或封入微型膠囊之潛在性硬化劑等。(2) Thermal curing agent: Usually, it can be used as long as it can be used for thermally curing an epoxy resin, and is not particularly limited. As a specific example, a polyamine-based hardener such as diethylenetriamine, triethylenetetramine, N-aminoethylpiperazine, diaminodiphenylmethane or diammonium adipate can be used. Phthalic anhydride, tetrahydrophthalic anhydride, hexahydrophthalic anhydride, methyltetrahydrophthalic anhydride, methylhexahydrophthalic anhydride, methyl nadic An acid anhydride hardener such as an acid anhydride; a novolak resin type hardener; a polythiol hardener such as trioxane tri-ethyl thiol; benzyl dimethylamine, 2,4,6-tris(dimethyl A third amine compound such as aminomethyl)phenol; an imidazole compound such as 2-methylimidazole, 2-ethyl-4-methylimidazole or 1-benzyl-2-methylimidazole. Further, other solid dispersion type latent hardeners or latent hardeners encapsulated in microcapsules may be used.
(3)硬化促進劑：以硬化促進劑而言，可使用4級銨鹽、4級鎏鹽、各種金屬鹽、咪唑、3級胺等。以具體例而言，對於4級銨鹽，可舉四甲基溴化銨、四丁基溴化銨為例，對於4級鎏鹽，可舉四苯基溴化鏻、四丁基溴化鏻等為例，對於金屬鹽，可舉辛酸鋅、辛酸錫等為例，對於咪唑，可舉1-苯甲基-2-甲基咪唑、1-苯甲基-2-苯基咪唑、2-乙基-4-甲基咪唑等為例，以3級胺而言，則可舉苯甲基二甲胺等為例。(3) Hardening accelerator: As the hardening accelerator, a grade 4 ammonium salt, a grade 4 phosphonium salt, various metal salts, imidazole, a tertiary amine, or the like can be used. Specific examples include 4-methylammonium bromide and tetrabutylammonium bromide. For the 4-stage phosphonium salt, tetraphenylphosphonium bromide and tetrabutyl bromide are mentioned. For example, examples of the metal salt include zinc octoate and tin octylate. Examples of the imidazole include 1-benzyl-2-methylimidazole and 1-benzyl-2-phenylimidazole. -ethyl-4-methylimidazole or the like is exemplified, and in the case of a tertiary amine, benzyl dimethylamine or the like can be exemplified.
(4)耦合劑：作為耦合劑，例如有矽烷耦合劑、鈦酸酯系耦合劑、鋁酸酯系耦合劑、矽化合物等，其等耦合劑可單獨或混合使用。含有耦合劑時，可提昇樹脂組成物之接著性，具有減少黏度之效果，本發明之密封用熱硬化性樹脂組成物係含有0.001至5重量份，較佳的是0.01至1重量份者為佳。(4) Coupling agent: Examples of the coupling agent include a decane coupling agent, a titanate coupling agent, an aluminate coupling agent, a hydrazine compound, and the like, and the coupling agents thereof may be used singly or in combination. When the coupling agent is contained, the adhesion of the resin composition can be improved, and the viscosity is reduced. The thermosetting resin composition for sealing of the present invention contains 0.001 to 5 parts by weight, preferably 0.01 to 1 part by weight. good.
(5)氧化防止劑：為了藉於本發明之密封用熱硬化性樹脂組成物防止熱硬化時之氧化劣化，而進一步提高硬化物之耐熱安定性時，可添加氧化防止劑。前述氧化防止劑乃可使用苯酚系、硫系、磷系氧化防止劑等。以具體例而言，可舉二丁基羥基甲苯、2,6-二-四-丁基-對甲酚(以下稱為BHT)等之苯酚系氧化防止劑、巰基丙酸衍生物等之硫系酸化防止剤、磷酸三苯酯、9,10-二氫-9-氧-10-磷菲-10-氧化物(以下稱為HCA)等之磷系氧化防止劑等為例，前述氧化防止劑可單獨或混合2種以上使用，在本發明之密封用熱硬化性樹脂組成物中含有0.001至5重量份，較佳的是含有0.01至0.5重量份為佳。(5) Oxidation inhibitor: When the thermosetting resin composition for sealing of the present invention prevents oxidative degradation during thermal curing and further improves the heat resistance stability of the cured product, an oxidation preventing agent may be added. A phenol type, a sulfur type, a phosphorus type oxidation inhibitor, etc. can be used for the said oxidation inhibitor. Specific examples thereof include sulfur compounds such as dihydroxy hydroxytoluene and 2,6-di-tetra-butyl-p-cresol (hereinafter referred to as BHT), and thiol propionate derivatives. For example, a phosphorus-based oxidation preventing agent such as hydrazine, triphenyl phosphate, 9,10-dihydro-9-oxo-10-phosphaphenanthrene-10-oxide (hereinafter referred to as HCA) is used as an example, and the oxidation prevention is performed. The agent may be used singly or in combination of two or more kinds, and it is preferably contained in the thermosetting resin composition for sealing of the present invention in an amount of 0.001 to 5 parts by weight, preferably 0.01 to 0.5 part by weight.
如此本發明之密封方法，適用於OLED元件或集成該元件之面板時，因為可將其效果極大化，所以較佳。即，如第1圖至第3圖顯示其具體例般，前述電元件係一種將含有下板基材以及在該下板基材上堆疊之陽極(正極)、發光層及陰極(負極)之下部密封構件與上部密封構件接合而成之有機發光元件，前述(a)步驟為以熱硬化性樹脂組成物全面地塗佈於上部密封構件之一面或下部密封構件之陰極(負極)面之步驟，前述(b)步驟是在將上部密封構件之塗佈面與下部密封構件之陰極(負極)面、或上部密封構件之一面與下部密封構件之塗佈面相接之狀態下將上部密封構件及下部密封構件接合之步驟，前述(c)步驟係對前述已接合之結合體加熱，使熱硬化性樹脂組成物硬化之步驟，進行其等步驟後，可製作如第1圖般之有機發光元件。Thus, the sealing method of the present invention is preferably applied to an OLED element or a panel in which the element is integrated, since the effect can be maximized. That is, as shown in FIGS. 1 to 3, the electric component is an anode (positive electrode), a light-emitting layer, and a cathode (negative electrode) which are provided with a lower substrate and stacked on the lower substrate. The organic light-emitting element in which the lower sealing member and the upper sealing member are joined, the step (a) is a step of applying the thermosetting resin composition to the cathode (negative) surface of one of the upper sealing member or the lower sealing member. In the above step (b), the upper sealing member is placed in a state where the coated surface of the upper sealing member and the cathode (negative electrode) surface of the lower sealing member or the surface of the upper sealing member and the coated surface of the lower sealing member are brought into contact with each other. And the step of joining the lower sealing member, wherein the step (c) is a step of heating the joined bonded body to cure the thermosetting resin composition, and after performing the steps, the organic light emitting as shown in FIG. 1 can be produced. element.
在此，前述下部密封構件係於下板基材上依序具備陽極(正極)、發光層及陰極(負極)者，較佳的是，可追加地含有電洞注入層(HIL)、電洞傳輸層(HTL)、電子注入層(EIL)、或電子傳輸層(ETL)。前述下板基材上所形成之陽極(正極)、發光層、陰極(負極)、電洞注入層(HIL)、電洞傳輸層(HTL)、電子注入層(EIL)或電子傳輸層(ETL)之形成可經由通常的方法進行者。Here, the lower sealing member is provided with an anode (positive electrode), a light-emitting layer, and a cathode (negative electrode) in this order on the lower substrate, and it is preferable to additionally include a hole injection layer (HIL) and a hole. Transport layer (HTL), electron injection layer (EIL), or electron transport layer (ETL). An anode (positive electrode), a light-emitting layer, a cathode (negative electrode), a hole injection layer (HIL), a hole transport layer (HTL), an electron injection layer (EIL) or an electron transport layer (ETL) formed on the lower substrate The formation can be carried out by a usual method.
又，較佳的是，如前述，本發明之密封方法係於將下部密封構件與上部密封構件接合以將元件密封之方法中，藉液晶滴入(One Drop Filling)步驟而將前述密封用熱硬化性樹脂組成物全面地塗佈於上部密封構件之一面或下部密封構件之一面，將前述上部密封構件與下部密封構件接合，且對前述業已接合之上部密封構件與下部密封構件加熱，使前述密封用熱硬化性樹脂組成物硬化者。Further, preferably, as described above, the sealing method of the present invention is a method of joining the lower sealing member and the upper sealing member to seal the element, and the sealing heat is applied by a one-drop filling step. The curable resin composition is applied to one surface of the upper sealing member or one surface of the lower sealing member, the upper sealing member is joined to the lower sealing member, and the above-mentioned bonded upper sealing member and lower sealing member are heated, so that the aforementioned The thermosetting resin composition for sealing is hardened.
以一具體例來說，本發明之OLED元件之密封方法，較佳的是，含有利用ODF步驟(有利於製程特性)而將前述熱硬化性樹脂組成物全面地塗佈於上部密封構件之一面或下部密封構件之陰極(負極)面之步驟。進行如此塗佈之後，進行兩密封構件之接合，這可以通常的接合方法進行，較佳的是，上部密封構件與下部密封構件之接合係於氮環境氣體下，較佳的是10-6 torr以下，更佳的是10-7 torr以下之真空環境氣體中進行時，對於清淨度及防止污染之方面來說較佳。尤其在製作OLED時，如前述，在上部密封構件之塗佈面與下部密封構件之陰極(負極)面，或上部密封構件之一面與下部密封構件之塗佈面相接之狀態下將上部密封構件與下部密封構件接合，這可以在氮環境氣體下，較佳的是10-6 torr以下，更佳的是10-7 torr以下之真空環境氣體中進行。In a specific example, the sealing method of the OLED element of the present invention preferably comprises applying the thermosetting resin composition to one side of the upper sealing member by using an ODF step (facilitating process characteristics). Or the step of the cathode (negative electrode) face of the lower sealing member. After such coating, the joining of the two sealing members is carried out, which can be carried out by a usual joining method. Preferably, the joining of the upper sealing member and the lower sealing member is under a nitrogen atmosphere, preferably 10 -6 torr. In the following, more preferably, it is preferably carried out in a vacuum atmosphere of 10 -7 torr or less in terms of cleanliness and prevention of contamination. In particular, in the production of the OLED, as described above, the upper portion is sealed in a state where the coated surface of the upper sealing member and the cathode (negative electrode) surface of the lower sealing member or the surface of the upper sealing member is in contact with the coated surface of the lower sealing member. The member is joined to the lower sealing member, which may be carried out under a nitrogen atmosphere, preferably 10 -6 torr or less, more preferably 10 -7 torr or less.
在如此接合步驟之後進行熱硬化步驟，該步驟是對前述業已接合之上部密封構件或下部密封構件(其等之結合體)加熱，使密封用熱硬化性樹脂組成物硬化者，為前述組成物時，適合的熱硬化溫度係以75至120℃範圍內者為佳。After the joining step, a heat hardening step is performed in which the above-mentioned bonded upper sealing member or lower sealing member (the combination thereof) is heated to cure the thermosetting resin composition for sealing, and the composition is the same. A suitable heat hardening temperature is preferably in the range of 75 to 120 °C.
又，因應所需，可在上部密封構件之下面周緣、或下部密封構件之上面周緣追加地塗佈光硬化性樹脂組成物或玻璃料。以與此有關之具體例來說，針對OLED步驟，乃如第2至3圖所示者。經由如此方式進行電裝置之氣密外，亦可以另外的材料將電元件之周緣氣密化，以滿足電元件所需之其他特性者。Further, a photocurable resin composition or a glass frit may be additionally applied to the lower periphery of the upper sealing member or the upper periphery of the lower sealing member as needed. For the specific examples related thereto, the steps for the OLED are as shown in Figures 2 to 3. In addition to the airtightness of the electrical device in this manner, additional materials may be used to hermetically seal the periphery of the electrical component to meet other characteristics required for the electrical component.
即，如圖所示，OLED時，可利用通常的塗佈方法，較佳的是利用網版印刷步驟(有利於精密性及作業性)而將公知之光硬化性樹脂組成物或玻璃料塗佈在上部密封構件之一面周緣或下部密封構件之陽極(正極)、發光層及陰極(負極)積層面之周緣。That is, as shown in the figure, in the case of an OLED, a conventional coating method can be used, and a known photocurable resin composition or glass frit is preferably coated by a screen printing step (facilitating precision and workability). It is disposed on the periphery of one of the upper sealing members or the periphery of the anode (positive electrode), the luminescent layer, and the cathode (negative electrode) of the lower sealing member.
將前述光硬化性樹脂組成物塗佈在密封構件之周緣時，可與前述熱硬化同時，或依序進行光硬化步驟，以安定度觀點來看，在光硬化後再熱硬化者為佳。前述光乃可使用可使光硬化性樹脂組成物硬化之光，以具體例而言，可使用紫外線。又，將玻璃料塗佈於密封構件之周緣時，為了燒成玻璃料粉末，可使用雷射。經由如此加熱，使前述密封用熱硬化性樹脂組成物硬化，形成硬化體，上部密封構件與下部密封構件之間被前述硬化體氣密充填而接著者。When the photocurable resin composition is applied to the periphery of the sealing member, the photocuring step may be performed simultaneously with the thermal curing or sequentially, and it is preferable to thermally harden after photocuring from the viewpoint of stability. As the light, a light which can cure the photocurable resin composition can be used, and in a specific example, ultraviolet rays can be used. Further, when the glass frit is applied to the periphery of the sealing member, a laser can be used for firing the glass frit powder. By heating in this manner, the thermosetting resin composition for sealing is cured to form a cured body, and the upper sealing member and the lower sealing member are hermetically filled with the hardened body.
本發明所使用之前述光硬化性樹脂組成物係以含有(1)環氧樹脂50~90重量份、(2)光引發劑0.1~5重量份、(3)無機充填劑1~40重量份及(4)耦合劑0.1~5重量份為佳，更可選擇地含有(5)間隔件1~20重量份及光酸發生劑0.001~1重量份。The photocurable resin composition used in the present invention contains (1) 50 to 90 parts by weight of the epoxy resin, (2) 0.1 to 5 parts by weight of the photoinitiator, and (3) 1 to 40 parts by weight of the inorganic filler. And (4) the coupling agent is preferably 0.1 to 5 parts by weight, and more preferably contains (5) 1 to 20 parts by weight of the spacer and 0.001 to 1 part by weight of the photoacid generator.
本發明之光硬化性樹脂組成物係藉具有5,000~150,000cps(25℃下)，較佳的是具有10,000~100,000cps之黏度(25℃下)，具有可進行網版印刷步驟，可將製程時間縮短，可節省製程上所花費之費用之長處。The photocurable resin composition of the present invention has a viscosity of 5,000 to 150,000 cps (at 25 ° C), preferably 10,000 to 100,000 cps (at 25 ° C), and has a screen printing step, which can be processed. Shorter time saves the cost of the process.
(1)環氧樹脂組成物：作為可適用於本發明光硬化性樹脂組成物之環氧樹脂組成物，乃可使用廣泛使用之芳香族環氧樹脂、脂環式環氧樹脂、或可使用其等之混合物。以前述芳香族環氧樹脂而言，可使用聯苯型、雙酚A型、雙酚F型、酚醛清漆樹脂型、二環戊二烯型環氧樹脂，亦可使用其等混合物。(1) Epoxy resin composition: As an epoxy resin composition applicable to the photocurable resin composition of the present invention, a widely used aromatic epoxy resin, alicyclic epoxy resin, or usable can be used. a mixture of such. As the aromatic epoxy resin, a biphenyl type, a bisphenol A type, a bisphenol F type, a novolac resin type, a dicyclopentadiene type epoxy resin, or a mixture thereof can be used.
(2)光引發劑：可適用於本發明之光硬化性樹脂組成物之光引發劑，只要是可藉光將前述環氧樹脂硬化者，即無特別限制。以前述光引發劑之具體例而言，可舉芳香族重氮鎓鹽、芳香族鎏鹽、芳香族碘鋁鹽、芳香族鎏鋁鹽、芳環烯金屬衍生物化合物及鐵芳烴系化合物等為例。較佳的是，可使用芳香族鎏鹽，其具體例乃可舉芳香族鎏六氟磷酸鹽化合物、芳香族鎏六氟銻酸鹽化合物等為例。(2) Photoinitiator: A photoinitiator which can be suitably used for the photocurable resin composition of the present invention is not particularly limited as long as it can cure the epoxy resin by light. Specific examples of the photoinitiator include an aromatic diazonium salt, an aromatic sulfonium salt, an aromatic iodine aluminum salt, an aromatic sulfonium aluminum salt, an aromatic cycloolefin metal derivative compound, and an iron aromatic hydrocarbon compound. For example. An aromatic sulfonium salt can be preferably used, and specific examples thereof include an aromatic hexafluorophosphate compound and an aromatic hexafluoroantimonate compound.
(3)無機充填劑：作為可適用於本發明光硬化性樹脂組成物之無機充填劑，可使用滑石(talc)、二氧化矽、氧化鎂、雲母(mica)、蒙脫石、氧化鋁、石墨、氧化鈹(beryllium oxide)、氮化鋁、碳化矽、模來石(mullite)、矽等之板狀或球形的無機充填劑、或將取代基導入前述無機充填劑且直徑或長軸為0.1至20μm之無機充填劑。添加在樹脂組成物之無機充填劑係均等地分散在硬化後組成物之內部，不僅可將作用在組成物之應力分散，強化接著力，亦具有有效地防止侵入組成物內部而擴散之水分，使水分穿透特性提昇之效果。(3) Inorganic filler: As an inorganic filler which can be suitably used for the photocurable resin composition of the present invention, talc, cerium oxide, magnesium oxide, mica, montmorillonite, alumina, or the like can be used. a plate-like or spherical inorganic filler of graphite, beryllium oxide, aluminum nitride, tantalum carbide, mullite, lanthanum, or the like, or a substituent introduced into the above inorganic filler and having a diameter or a major axis 0.1 to 20 μm of inorganic filler. The inorganic filler added to the resin composition is uniformly dispersed in the interior of the cured composition, and not only the stress acting on the composition is dispersed, but also the adhesion force is enhanced, and moisture which is infiltrated into the inside of the composition is effectively prevented from being diffused. The effect of improving the moisture penetration characteristics.
(4)耦合劑：可適用在本發明之光硬化性樹脂組成物之耦合劑係可單獨或混合使用矽烷系或鈦系耦合劑、矽化合物。較佳的是，以一分子內含有烷氧基矽烷及二縮水甘油醚之矽烷耦合劑為佳。(4) Coupling agent: A coupling agent which can be applied to the photocurable resin composition of the present invention may be a decane-based or titanium-based coupling agent or a ruthenium compound, alone or in combination. Preferably, a decane coupling agent containing an alkoxysilane and a diglycidyl ether in one molecule is preferred.
(5)間隔件：可適用於本發明之光硬化性樹脂組成物之間隔件只要是硬化後可維持一定的面板厚度者，即無特別限制，以可將面板之厚度維持在5~50μm、較佳的是5~25μm者為佳。間隔件之型態係包括球形或圓木形等，間隔件之型態亦只要是可將面板之厚度維持一定者，即無特別限制。(5) Spacer: The spacer which can be applied to the photocurable resin composition of the present invention is not particularly limited as long as it can maintain a certain panel thickness after hardening, so that the thickness of the panel can be maintained at 5 to 50 μm. Preferably, it is preferably 5 to 25 μm. The type of the spacer includes a spherical shape or a round shape, and the shape of the spacer is not particularly limited as long as the thickness of the panel can be maintained constant.
(6)光酸發生劑：作為可適用於本發明之光硬化性樹脂組成物之光酸發生劑，只要是可藉曝光產生路易斯酸或布氏酸之物時，即無特別限定，可使用有機磺酸等之硫化鹽系化合物、鎓鹽等之鎓系化合物。較佳的是，可使用苯二甲醯亞胺三氟甲磺酸鹽、二硝苯甲基甲苯磺酸鹽、磺酸正癸酯、萘醯亞胺三氟甲磺酸鹽、二苯基錪鎓鹽、六氟磷酸鹽、六氟砷酸鹽、六氟銻酸鹽、二苯基對甲氧基苯基鎏酸氟甲磺酸鹽、二苯基對甲苯基鎏三氟甲磺酸鹽、二苯基對異丁基苯基鎏三氟甲磺酸鹽、三苯基鎏六氟砷酸鹽、三苯基鎏六氟銻酸鹽、三苯基鎏三氟甲磺酸鹽、二丁基萘鎏三氟磺酸鹽及其等混合物。(6) Photoacid generator: The photoacid generator which is applicable to the photocurable resin composition of the present invention is not particularly limited as long as it can be used to generate a Lewis acid or a Brine acid by exposure, and can be used. A sulfonate compound such as an organic sulfonic acid or a sulfonium compound such as a phosphonium salt. Preferably, xylylenediamine triflate, dinitrobenzyltoluenesulfonate, n-decyl sulfonate, naphthyl imine triflate, diphenyl can be used. Bismuth salt, hexafluorophosphate, hexafluoroarsenate, hexafluoroantimonate, diphenyl-p-methoxyphenyl decanoate fluoromethanesulfonate, diphenyl-p-tolyl fluorene trifluoromethanesulfonic acid Salt, diphenyl-p-isobutylphenyl sulfonium trifluoromethanesulfonate, triphenylsulfonium hexafluoroarsenate, triphenylsulfonium hexafluoroantimonate, triphenylsulfonium trifluoromethanesulfonate, Dibutylnaphthoquinone trifluorosulfonate and mixtures thereof.
又，本發明係提供具有透光部之電元件，其包含有：下部密封構件；與前述下部密封構件相隔之狀態下位於前述下部密封構件之上部之上部密封構件；位於前述下部密封構件與上部密封構件之間之電裝置；及，充填於前述上部密封構件及下部密封構件之接著面之間，且將前述電裝置包圍，使前述上部密封構件與下部密封構件接著之熱硬化性樹脂組成物之硬化體層，又，前述熱硬化性樹脂組成物之硬化體層具有形成前述透光部之一部分或全部之構成。Moreover, the present invention provides an electric component having a light transmitting portion, comprising: a lower sealing member; a sealing member located above an upper portion of the lower sealing member in a state of being spaced apart from the lower sealing member; and a lower sealing member and an upper portion An electric device between the sealing members; and a thermosetting resin composition which is filled between the upper surface of the upper sealing member and the lower sealing member and surrounds the electric device to surround the upper sealing member and the lower sealing member Further, the hardened layer of the thermosetting resin composition has a configuration in which part or all of the light transmitting portion is formed.
在此，具有前述透光部之電元件及其內部所含之電裝置係如前述，且對於與此有關之具體例，前述元件可舉OLED、LED或染料感應式太陽電池等為例，特別是，以一具體例而言，如第1圖所示之OLED具有藉熱硬化性樹脂組成物之硬化體而在形成無空隙之狀態下被充填接著之上部密封構件與下部密封構件，可具有優異之壽命特性。Here, the electric component having the light transmitting portion and the electric device included therein are as described above, and for the specific example related thereto, the above-mentioned components may be exemplified by an OLED, an LED, or a dye-inductive solar cell, and the like. In a specific example, the OLED as shown in FIG. 1 has a hardened body of a thermosetting resin composition and is filled in a state in which no voids are formed, and then the upper sealing member and the lower sealing member may have Excellent life characteristics.
又，在此，本發明之電元件可更包含有光硬化性樹脂組成物硬化體周緣，其充填在前述上部密封構件與下部密封構件之接著面之間的周緣，且包圍前述熱硬化性樹脂組成物層，該光硬化性樹脂組成物硬化體周緣可經由第2至3圖所提示之方法等形成者。Moreover, the electric component of the present invention may further include a peripheral edge of the cured body of the photocurable resin composition, which is filled around the periphery between the upper sealing member and the lower surface of the lower sealing member, and surrounds the thermosetting resin. The composition layer, the periphery of the hardened body of the photocurable resin composition can be formed by a method as shown in FIGS. 2 to 3 and the like.
前述之本發明之具有透光部之電元件乃可經由前述之本發明之具有透光部之電元件之密封方法而製作者，特別是在前述電元件為OLED時，可具有如第1圖至第3圖所示之最終構成，如此構成係可經由第2至3圖之製造方法製作者為佳。此時，前述電元件係一種有機發光二極體，其係由下板基材、堆疊於該下板基材上且具有陽極(正極)、發光層及陰極(負極)之下部密封構件、及上部密封構件接合而構成者，較佳的是，前述下部密封構件係於下板基材之上，可追加地含有電洞注入層(HIL)、電洞傳輸層(HTL)、電子注入層(EIL)、或電子傳輸層(ETL)。The above-described electrical component having a light transmitting portion of the present invention can be produced by the sealing method of the electrical component having the light transmitting portion of the present invention described above, and particularly when the electrical component is an OLED, it can have a first image as shown in FIG. The final configuration shown in Fig. 3 is preferably such that it can be produced by the manufacturing method of Figs. 2 to 3. In this case, the electric component is an organic light emitting diode which is a lower plate substrate, is stacked on the lower plate substrate, and has an anode (positive electrode), a light emitting layer, and a cathode (negative electrode) lower sealing member, and Preferably, the upper sealing member is joined to the lower plate base material, and may further include a hole injection layer (HIL), a hole transport layer (HTL), and an electron injection layer ( EIL), or electron transport layer (ETL).
如此，有機發光二極體係使如此電元件之上部密封構件及下部密封構件藉熱硬化性樹脂組成物之硬化體充填接著而形成無空隙之狀態，而提昇耐久性，因此為佳。In the organic light-emitting diode system, it is preferable that the upper sealing member and the lower sealing member of the electric component are filled with a hardened body of the thermosetting resin composition to form a void-free state, thereby improving durability.
另外，前述電元件之下部密封構件及上部密封構件皆為玻璃為佳，藉此，可確保強度及安定性。Further, it is preferable that the electric component lower sealing member and the upper sealing member are glass, whereby strength and stability can be ensured.
以下為了理解本發明而提示較佳之實施例，但下述實施例只是舉例說明本發明者，本發明之範圍不限定於下述實施例者。The preferred embodiments are described below in order to understand the present invention, but the following examples are merely illustrative of the present invention, and the scope of the present invention is not limited to the following examples.
以如下述表1所示之組成製造密封用熱硬化性樹脂組成物。A thermosetting resin composition for sealing was produced in the composition shown in the following Table 1.
EPOLIGHT 100MF：脂肪族縮水甘油醚化合物(KYOEISHA)EPOLIGHT 100MF: Aliphatic glycidyl ether compound (KYOEISHA)
YL983U：雙酚F型環氧樹脂(日本艾波吉思公司)YL983U: Bisphenol F type epoxy resin (Japan Aibojisi Company)
CELLOXIDE 2021P：脂環式環氧樹脂(Daicel Chemical Industries,Ltd.)CELLOXIDE 2021P: alicyclic epoxy resin (Daicel Chemical Industries, Ltd.)
Epikote 152：甲酚-清漆樹脂型環氧樹脂(日本艾波吉思公司)Epikote 152: Cresol-Varnish Resin Type Epoxy Resin (Abbott, Japan)
RIKACID MH-700：液状脂環式酸無水物硬化剤(新日本理化公司)RIKACID MH-700: Liquid alicyclic acid anhydrate hardening 新 (New Japan Physical and Chemical Company)
EMI-24：咪唑類硬化促進剤(Air Products公司)EMI-24: Imidazole hardening promotes 剤 (Air Products)
K61B：胺類硬化促進劑(Air Products公司)K61B: Amine hardening accelerator (Air Products)
測定以前述實施例1-6製造之熱硬化性樹脂組成物各自的光穿透度、接著強度、黏度及硬化性，各示於下述表2。The light transmittance, the adhesion strength, the viscosity, and the curability of each of the thermosetting resin compositions produced in the above Examples 1 to 6 were measured and shown in Table 2 below.
1.光穿透度測定：光穿透度之測定係利用撒布器(dispenser)將熱硬化性組成物以同一間隙塗佈在塗佈面全面，以於50mm×50mm×0.7mm之透明玻璃基材(三星康寧精密玻璃公司、製品名稱：Eagle 2000)之上形成約20μm之厚度。在100℃之烤盤上硬化1小時之後，使用Reference玻璃基材(三星康寧精密玻璃公司、製品名稱：Eagle 2000)，測定光通過基材時之透射率，測定機器是使用大塚公司之光譜分析機器之MCPD-3000，並在380至780nm之波長範圍內，按塗佈有前述熱硬化性組成物之玻璃基材之6點分別測定透射率所得到之波長範圍內之平均值。1. Measurement of light transmittance: The measurement of light transmittance is carried out by using a dispenser to apply a thermosetting composition on the coated surface in the same gap to cover a transparent glass base of 50 mm × 50 mm × 0.7 mm. A thickness of about 20 μm was formed on the material (Samsung Corning Precision Glass Co., Ltd., product name: Eagle 2000). After hardening on a baking tray at 100 ° C for 1 hour, the transmittance of the light passing through the substrate was measured using a Reference glass substrate (Samsung Corning Precision Glass Co., Ltd., product name: Eagle 2000), and the measurement machine was subjected to spectral analysis using Otsuka Corporation. The MCPD-3000 of the machine has an average value in the wavelength range obtained by measuring the transmittance at six points of the glass substrate coated with the thermosetting composition in the wavelength range of 380 to 780 nm.
2.接著強度之測定：在將50mm×50mm×1.1mm之玻璃作為下板之基材上以直徑2mm大小滴落熱硬化性樹脂組成物之後，將上板與下板接合後，在100℃之烤盤上硬化1小時後，使用T字型夾具(Instron公司、製品名稱：Stud set)，以接著強度測定器(Instron公司、製品名稱：UTM-5566)測定。2. Measurement of strength: After the thermosetting resin composition was dropped by a diameter of 2 mm on a substrate of 50 mm × 50 mm × 1.1 mm as a lower plate, the upper plate and the lower plate were joined, and then at 100 ° C. After hardening for 1 hour on the baking sheet, it was measured using a T-shaped jig (Instron, product name: Stud set), followed by a strength measuring instrument (Instron, product name: UTM-5566).
3.黏度之測定：黏度係利用黏度測定器(商品名稱：Brook Field viscometer)，而對熱硬化性組成物0.5g測定顯示接近80%之扭力矩時之黏度。3. Measurement of viscosity: The viscosity was measured by a viscosity measuring device (trade name: Brook Field viscometer), and the viscosity of the thermosetting composition of 0.5 g was measured to be close to 80% of the torsional moment.
4.硬化性：令於100℃之烤盤上熱硬化性組成物以1小時可硬化的時候為Good，而在前述硬化條件下硬化不夠充分時，則為Not good。4. Curability: When the thermosetting composition on the baking sheet at 100 ° C is hardened in one hour, it is good, and when the hardening is insufficient under the above curing conditions, it is Not good.
由前述表2之結果可確認到，本發明之實施例1至6之密封用熱硬化性樹脂組成物係適於密封，並具有優異的物性。As a result of the above-mentioned Table 2, it was confirmed that the thermosetting resin compositions for sealing of Examples 1 to 6 of the present invention are suitable for sealing and have excellent physical properties.
YL983U：雙酚F型環氧樹脂(日本艾波機思公司)YL983U: bisphenol F type epoxy resin (Japan Aibo Machines Co., Ltd.)
NC7300L：聯苯型環氧樹脂(日本化藥公司)NC7300L: Biphenyl type epoxy resin (Nippon Chemical Co., Ltd.)
SP170：陽離子聚合引發劑(旭電化公司)SP170: Cationic polymerization initiator (Asahi Kasei Corporation)
P-3：無機充填劑、滑石(日本塔爾克公司)P-3: Inorganic filler, talc (Talker, Japan)
KBM403：矽烷耦合劑(信越公司)KBM403: decane coupling agent (Shin-Etsu)
測定前述實施例7至11所製造之光硬化性樹脂組成物之各光穿透度、水分穿透度、接著強度、熱安定性及黏度，各示於下述表4。The light transmittance, water permeability, adhesive strength, thermal stability, and viscosity of the photocurable resin composition produced in the above Examples 7 to 11 were measured and shown in Table 4 below.
1.水分穿透度之測定：利用桿塗器，而在聚對苯二甲酸乙二酯薄膜之表面塗佈光硬化性樹脂組成物成為50mm×50mm×0.1mm大小之後，照射6000mJ/cm2 之UV，在80℃之烤盤上硬化1小時後，以ASTM F1249之方法且在37.8℃、100%RH之條件下以水分穿透度測定器(製品名稱：PERMATRAN-W3/33)測定24小時之水分穿透度。1. Measurement of water penetration: After applying a photocurable resin composition to a surface of a polyethylene terephthalate film to a size of 50 mm × 50 mm × 0.1 mm by a bar coater, irradiation of 6000 mJ/cm 2 UV, after hardening on a baking tray at 80 ° C for 1 hour, measured by ASTM F1249 and at 37.8 ° C, 100% RH with a water permeability tester (product name: PERMATRAN-W3/33) 24 The moisture penetration of the hour.
2.接著強度之測定：在50mm×50mm×1.1mm之下板玻璃基材上以直徑5mm大小滴落光硬化性樹脂組成物之後，上板是準備與下板同一大小之玻璃基材，將上板與下板接合後，照射6000mJ/cm2 之UV，在80℃之烤盤上硬化1小時後，使用T字型夾具(Instron公司、製品名稱：Studset)，以接著強度測定器(Instron公司、製品名稱：UTM-5566)測定。2. Measurement of strength: After dropping a photocurable resin composition on a plate glass substrate at a diameter of 5 mm under a size of 50 mm × 50 mm × 1.1 mm, the upper plate is a glass substrate of the same size as the lower plate. After the upper plate and the lower plate were joined, UV was irradiated at 6000 mJ/cm 2 and hardened on a baking plate at 80 ° C for 1 hour, and then a T-shaped jig (Instron, product name: Studset) was used to carry out the strength measuring device (Instron). Company, product name: UTM-5566) determination.
3.熱安定性之測定：利用桿塗器，而在業經脫模處理之聚對苯二甲酸乙二酯薄膜之表面形成光硬化性樹脂組成物為50mm×50mm×0.1mm大小之後，照射6000mJ/cm2 之UV，在80℃之烤盤上硬化1小時後所得到之塗膜中將一部分切斷，利用微差掃描熱析儀(TA公司、製品名稱：DSC)，測定光硬化性樹脂組成物之玻璃轉移溫度(Tg)。3. Determination of thermal stability: using a bar coater, and forming a photocurable resin composition on the surface of the release-treated polyethylene terephthalate film to have a size of 50 mm × 50 mm × 0.1 mm, and irradiating 6000 mJ / cm UV 2, the portion in the coating film obtained after curing in the oven of 80 deg.] C one hour off, using a differential scanning calorimetry analyzer (TA company, product name: DSC), the measurement light curing resin The glass transition temperature (Tg) of the composition.
4.光穿透度之測定：光穿透度之測定係利用桿塗器(bar applicator)，將熱硬化性樹脂組成物塗佈在50mm×50mm×0.7mm之透明玻璃基材(三星康寧公司、製品名稱：Eagle 2000)之上形成20μm，且在100℃的烤盤上硬化1小時後，並使用對照玻璃基材(三星康寧公司、製品名：Eagle 2000)，測定光通過基材時之透射率，測定儀器是使用大塚公司之光譜分析機器之MCPD-3000，在380至780nm之波長範圍內，依照塗佈有前述熱硬化性樹脂組成物之玻璃基材之6點分別測定透射率而所得到之波長範圍內之平均值。4. Measurement of light transmittance: The measurement of light transmittance is carried out by using a bar applicator to coat a thermosetting resin composition on a transparent glass substrate of 50 mm × 50 mm × 0.7 mm (Samsung Corning Co., Ltd. , product name: Eagle 2000) formed 20 μm, and hardened on a baking tray at 100 ° C for 1 hour, and using a control glass substrate (Samsung Corning, product name: Eagle 2000), when measuring light through the substrate The transmittance and the measuring instrument are MCPD-3000 using a spectral analysis machine of Otsuka Co., Ltd., and the transmittance is measured in accordance with the six points of the glass substrate coated with the thermosetting resin composition in the wavelength range of 380 to 780 nm. The average of the wavelengths obtained.
5.黏度之測定：利用黏度測定器(商品名稱：Brook Field viscometer)，而對樹脂組成物0.5g測定顯示接近80%之扭力矩時之黏度。5. Measurement of viscosity: A viscosity measuring device (trade name: Brook Field viscometer) was used, and the viscosity of the resin composition of 0.5 g was measured to show a torque of approximately 80%.
由前述表4之結果乃可確認到，本發明之實施例7至11之光硬化性樹脂組成物係適於使用目的，亦具有優異之物性者。From the results of the above Table 4, it was confirmed that the photocurable resin compositions of Examples 7 to 11 of the present invention are suitable for the purpose of use and also have excellent physical properties.
準備含有下板基材、以及在其上積層之陽極(正極)、發光層(紅色、綠色、藍色面發光)及陰極(負極)之下部密封構件、和上部密封構件。利用ODF步驟，而在下部密封構件之陰極(負極)面全面塗佈前述實施例1之熱硬化性樹脂組成物。除此外，另外利用網版印刷步驟，將光硬化性樹脂組成物塗佈在上部密封構件之周緣。在上部密封構件之塗佈面與下部密封構件之塗佈面相接之狀態下將上部密封構件與下部密封構件在氮環境氣體下10-7 torr之真空環境氣體中接合。在已接合之上部密封構件及下部密封構件照射6000mJ/cm2 之UV，使光硬化性樹脂組成物硬化之後，以80℃加熱，將熱硬化性樹脂組成物硬化，製造顯示器元件，在第2圖顯示製程圖(在第2圖中，(1)：陽極(正極)蒸鍍步驟、(2)：發光體(紅色、綠色、藍色面發光)、(3)：陰極(負極)蒸鍍步驟、(4)：彩色濾光片成膜步驟、(5)光硬化樹脂塗佈步驟、(6)：密封用熱硬化樹脂塗佈步驟(ODF步驟：以一定間隔塗佈在基板全面)、(7)：接合後之熱硬化步驟、(a)：撒布器、(b)：熱硬化性組成物、(c)：加熱(heating))。An underlying sealing member including a lower substrate and an anode (positive electrode), a light-emitting layer (red, green, and blue-surface light-emitting), a cathode (negative electrode), and an upper sealing member which are laminated thereon are prepared. The thermosetting resin composition of the above-described Example 1 was entirely coated on the cathode (negative electrode) surface of the lower sealing member by the ODF step. Further, in addition, a photocurable resin composition is applied to the periphery of the upper sealing member by a screen printing step. The upper sealing member and the lower sealing member are joined in a vacuum atmosphere gas of 10 -7 torr under a nitrogen atmosphere in a state where the coated surface of the upper sealing member is in contact with the coated surface of the lower sealing member. After the bonded upper sealing member and the lower sealing member are irradiated with UV of 6000 mJ/cm 2 to cure the photocurable resin composition, the composition is cured at 80° C. to cure the thermosetting resin composition to produce a display element. The figure shows the process chart (in Figure 2, (1): anode (positive) evaporation step, (2): illuminant (red, green, blue), (3): cathode (negative) evaporation Step, (4): color filter film forming step, (5) photo-curing resin coating step, (6): sealing thermosetting resin coating step (ODF step: coating at a certain interval on the entire substrate), (7): thermal hardening step after joining, (a): spreader, (b): thermosetting composition, (c): heating.
使用玻璃料代替前述實施例12之光硬化性樹脂之外，其餘以同一方法進行密封，在第3圖顯示製程圖(第3圖中，(1)：陽極(正極)蒸鍍步驟、(2)：發光體(紅色、綠色、藍色面發光)、(3)：陰極(負極)蒸鍍步驟、(4)：玻璃料塗佈及前燒成(可塑性)步驟、(5)彩色濾光片成膜步驟、(6)：熱硬化樹脂塗佈步驟(ODF步驟：以一定間隔塗佈在基板全面)、(7)：接合後之熱硬化步驟、(a)：撒布器、(b)：熱硬化性組成物、(c)：加熱(heating))。The glass frit was used instead of the photocurable resin of the above-mentioned Example 12, and the other method was sealed in the same manner, and the process chart was shown in FIG. 3 (Fig. 3, (1): anode (positive electrode) vapor deposition step, (2) ): illuminant (red, green, blue illuminating), (3): cathode (negative) vapor deposition step, (4): frit coating and pre-firing (plasticity) step, (5) color filter Film forming step, (6): thermosetting resin coating step (ODF step: coating on the substrate at regular intervals), (7): thermal hardening step after bonding, (a): spreader, (b) : thermosetting composition, (c): heating.
前述實施例12及實施例13所製造之元件具有如第1圖之構造，在光穿透度、水分穿透度、接著強度及熱安定性面上全部都很優異，基本上可防止發生上部密封構件及下部密封構件之發光體接觸而造成損傷者。The elements manufactured in the above-mentioned Embodiments 12 and 13 have the structure as shown in Fig. 1, and are excellent in light transmittance, moisture permeability, adhesion strength, and thermal stability, and substantially prevent the upper portion from being generated. The illuminant of the sealing member and the lower sealing member are in contact with each other to cause damage.
1．．．下板玻璃基材1. . . Lower glass substrate
2．．．陽極(正極)2. . . Anode (positive)
3．．．發光層3. . . Luminous layer
4．．．陰極(負極)4. . . Cathode (negative)
5．．．熱硬化性樹脂組成物5. . . Thermosetting resin composition
6．．．彩色濾光片6. . . Color filter
7．．．玻璃料或光硬化型樹脂組成物7. . . Glass frit or photohardenable resin composition
8．．．上板玻璃基材8. . . Upper plate glass substrate
(1)．．．陽極(正極)蒸鍍步驟(1). . . Anode (positive) evaporation step
(2)．．．發光體(紅色、綠色、藍色面發光)(2). . . Luminous body (red, green, blue surface)
(3)．．．陰極(負極)蒸鍍步驟(3). . . Cathode (negative electrode) evaporation step
(4)．．．彩色濾光片成膜步驟(第2圖)或玻璃料塗佈及前燒成步驟(第3圖)(4). . . Color filter film forming step (Fig. 2) or frit coating and pre-firing step (Fig. 3)
(5)．．．光硬化型樹脂塗佈(第2圖)或彩色濾光片成膜步驟(第3圖)(5). . . Photocurable resin coating (Fig. 2) or color filter film forming step (Fig. 3)
(6)．．．熱硬化樹脂塗佈步驟(ODF步驟：以一定間隔塗佈在基板全面)(6). . . Thermosetting resin coating step (ODF step: coating on the substrate at regular intervals)
(7)．．．接合後之熱硬化步驟(7). . . Thermal hardening step after bonding
(a)．．．撒布器(a). . . Spreader
(b)．．．熱硬化組成物(b). . . Thermosetting composition
(c)．．．加熱(heating)(c). . . Heating
第1圖係本發明一實施型態之顯示器元件之模式圖。Fig. 1 is a schematic view showing a display element of an embodiment of the present invention.
第2圖係本發明一實施型態之密封方法之製程圖。Fig. 2 is a process diagram of a sealing method according to an embodiment of the present invention.
第3圖係本發明一實施型態之密封方法之製程圖。Fig. 3 is a process diagram of a sealing method according to an embodiment of the present invention.
1‧‧‧下板玻璃基材1‧‧‧Under glass substrate
2‧‧‧陽極(正極)2‧‧‧Anode (positive)
3‧‧‧發光層3‧‧‧Lighting layer
4‧‧‧陰極(負極)4‧‧‧ cathode (negative)
5‧‧‧熱硬化性樹脂組成物5‧‧‧ thermosetting resin composition
6‧‧‧彩色濾光片6‧‧‧Color filters
7‧‧‧玻璃料或光硬化型樹脂組成物7‧‧‧Frit material or photohardenable resin composition
8‧‧‧上板玻璃基材8‧‧‧Upper glass substrate
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| CN102315311A (en) * | 2010-07-06 | 2012-01-11 | 杜邦太阳能有限公司 | Solar cell module device and banding coating method thereof |
| US20120044445A1 (en) | 2010-08-17 | 2012-02-23 | Semiconductor Energy Laboratory Co., Ltd. | Liquid Crystal Device and Manufacturing Method Thereof |
| KR101293803B1 (en) * | 2010-11-02 | 2013-08-06 | 주식회사 엘지화학 | Adhesive Film and Encapsulation Method of Organic Electronic Device Using the Same |
| CN102558769B (en) * | 2010-12-31 | 2015-11-25 | 第一毛织株式会社 | For the composition epoxy resin of encapsulated semiconductor device and the semiconducter device that encapsulated by this composition epoxy resin |
| KR101385034B1 (en) * | 2011-04-05 | 2014-04-14 | 제일모직주식회사 | An adhesive film for organic EL device, a composition for the same, and an organic EL device comprising the same |
| CN102226032A (en) * | 2011-04-11 | 2011-10-26 | 复旦大学 | Low-modulus epoxy resin system and preparation method thereof |
| CN102775736A (en) * | 2012-08-16 | 2012-11-14 | 上纬（上海）精细化工有限公司 | LED (Light-Emitting Diode) package material and composite used in same |
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| KR101469131B1 (en) * | 2013-05-27 | 2014-12-05 | 전자부품연구원 | Film for monitoring the degradation of photovoltaic module |
| CN103490021B (en) * | 2013-09-30 | 2015-12-02 | 上海大学 | Packaging system |
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