KR20140092268A - A polymer/inorganic multi-layer thin film encapsulation for organic electronic devices - Google Patents
A polymer/inorganic multi-layer thin film encapsulation for organic electronic devices Download PDFInfo
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- 239000010409 thin film Substances 0.000 title claims abstract description 101
- 229920000642 polymer Polymers 0.000 title claims abstract description 49
- 238000005538 encapsulation Methods 0.000 title claims abstract description 21
- 239000002243 precursor Substances 0.000 claims abstract description 14
- 239000000463 material Substances 0.000 claims abstract description 9
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 13
- 238000000231 atomic layer deposition Methods 0.000 claims description 10
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 claims description 10
- 239000000126 substance Substances 0.000 claims description 6
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 4
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 3
- 229910018557 Si O Inorganic materials 0.000 abstract description 4
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 abstract description 4
- 238000000034 method Methods 0.000 description 21
- 239000000758 substrate Substances 0.000 description 21
- 238000007789 sealing Methods 0.000 description 20
- VNRWTCZXQWOWIG-UHFFFAOYSA-N tetrakis(trimethylsilyl) silicate Chemical compound C[Si](C)(C)O[Si](O[Si](C)(C)C)(O[Si](C)(C)C)O[Si](C)(C)C VNRWTCZXQWOWIG-UHFFFAOYSA-N 0.000 description 16
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 10
- 229910052760 oxygen Inorganic materials 0.000 description 10
- 239000001301 oxygen Substances 0.000 description 10
- 239000010408 film Substances 0.000 description 9
- 239000011112 polyethylene naphthalate Substances 0.000 description 9
- 229920003207 poly(ethylene-2,6-naphthalate) Polymers 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000005229 chemical vapour deposition Methods 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 230000008859 change Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000035699 permeability Effects 0.000 description 3
- 239000004033 plastic Substances 0.000 description 3
- 229920003023 plastic Polymers 0.000 description 3
- 229920006254 polymer film Polymers 0.000 description 3
- 239000012495 reaction gas Substances 0.000 description 3
- 125000000217 alkyl group Chemical group 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 2
- 230000035515 penetration Effects 0.000 description 2
- 238000007740 vapor deposition Methods 0.000 description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 238000003848 UV Light-Curing Methods 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005670 electromagnetic radiation Effects 0.000 description 1
- 239000008393 encapsulating agent Substances 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 229920002457 flexible plastic Polymers 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 238000005240 physical vapour deposition Methods 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000000565 sealant Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- IXSPLXSQNNZJJU-UHFFFAOYSA-N trimethyl(silyloxy)silane Chemical compound C[Si](C)(C)O[SiH3] IXSPLXSQNNZJJU-UHFFFAOYSA-N 0.000 description 1
- JLTRXTDYQLMHGR-UHFFFAOYSA-N trimethylaluminium Chemical compound C[Al](C)C JLTRXTDYQLMHGR-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
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- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02109—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates
- H01L21/02205—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates the layer being characterised by the precursor material for deposition
- H01L21/02208—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates the layer being characterised by the precursor material for deposition the precursor containing a compound comprising Si
- H01L21/02211—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates the layer being characterised by the precursor material for deposition the precursor containing a compound comprising Si the compound being a silane, e.g. disilane, methylsilane or chlorosilane
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- H—ELECTRICITY
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- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
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- H01L21/02271—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase deposition by decomposition or reaction of gaseous or vapour phase compounds, i.e. chemical vapour deposition
- H01L21/02274—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase deposition by decomposition or reaction of gaseous or vapour phase compounds, i.e. chemical vapour deposition in the presence of a plasma [PECVD]
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- H10K10/00—Organic devices specially adapted for rectifying, amplifying, oscillating or switching; Organic capacitors or resistors having potential barriers
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- H10K50/844—Encapsulations
- H10K50/8445—Encapsulations multilayered coatings having a repetitive structure, e.g. having multiple organic-inorganic bilayers
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Abstract
Description
본 발명은 유기전자소자용 다층 박막 봉지에 관한 것으로, 더욱 상세하게는 유연성이 확보되고 봉지 특성이 향상된 유기전자소자용 다층 박막 봉지에 관한 것이다.
BACKGROUND OF THE
유기소자를 이용한 유기전자 기술은 기존 반도체 기술과는 달리 도포와 인쇄공정을 이용하여 플렉서블 플라스틱 기판 상에 실온에 가까운 저온에서 디스플레이, 회로, 전지, 센서 등의 기능을 집적화할 수 있다. 이 기술은 저가격으로 대면적의 플렉서블 기판에 전자소자를 구현할 수 있는 장점을 가지고 있다.
Organic electronic technology using organic devices can integrate functions of display, circuit, battery and sensor on flexible plastic substrate at a low temperature close to room temperature by using coating and printing process unlike existing semiconductor technology. This technology is advantageous in that electronic devices can be implemented on a large-area flexible substrate at a low cost.
그러나, 유기전자소자는 수분이나 산소의 침투에 취약하므로, 고수명의 유기전자소자를 제작하기 위하여 수분과 산소를 차단하는 봉지층 (encapsulation layer)이 필요하다. 초기에 이러한 봉지층으로 유리나 금속덮개(Metal lid)를 사용하여 봉지(encapsulation) 하였으나 기판 사이의 실런트를 통하여 수분이 투과 되고, 유연소자에 적용하게 되면 봉지층의 유연성확보가 어렵다는 단점이 있다. 이러한 유리나 금속덮개의 단점을 극복하기 위한 대안으로서 무기 또는 유기의 단층 또는 이들 조합의 다층 박막 구조를 이용한 박막 봉지 기술이 연구되고 있다.
However, since the organic electronic device is vulnerable to penetration of water or oxygen, an encapsulation layer that blocks moisture and oxygen is required to fabricate a high number of organic electronic devices. Initially, this encapsulation layer was encapsulated with glass or a metal lid. However, when moisture is permeated through the sealant between the substrates, it is difficult to secure the flexibility of the encapsulation layer when applied to a flexible device. As an alternative to overcoming the disadvantages of such glass or metal covers, thin film encapsulation techniques using multilayer thin film structures of inorganic or organic monolayers or combinations thereof have been studied.
종래 유기 광전자 코팅에 대한 기술로서 대한민국 특허공개 제10-2011-0081215호는 진공장비를 이용한 무기층 및 폴리머층을 포함하는 밀봉 다층 봉지구조로 코팅하는 기법을 개시하고 있다. 상기 기술은 열 및 전자기 방사선에 의해 가교되는 무기층 및 폴리머층을 포함하는 밀봉 다층 봉지구조를 코팅하여 유기소자를 수분과 산소로부터 보호하는 방법이다. 또한, 대한민국 특허공개 제10-2011-0062382호는 플렉서블 디스플레이 장치의 제조 방법에 관한 것으로서 플라스틱 기판 사이에 유기소자를 제작한 기술을 개시하고 있다. 상기 기술은 플라스틱 기판 표면에 배리어층을 제작하여 박막 트렌지스터와 유기발광소자를 제작하는 방법이다.
Korean Patent Laid-Open No. 10-2011-0081215 discloses a technique for coating with a sealing multilayer encapsulation structure including an inorganic layer and a polymer layer using vacuum equipment as a technique for conventional organic photoelectron coating. The technique is a method of protecting an organic device from moisture and oxygen by coating a sealed multilayer encapsulation structure comprising an inorganic layer and a polymer layer bridged by heat and electromagnetic radiation. Korean Patent Laid-Open Publication No. 10-2011-0062382 discloses a manufacturing method of a flexible display device, and discloses a technique of manufacturing an organic device between plastic substrates. The above technique is a method of fabricating a thin film transistor and an organic light emitting diode by fabricating a barrier layer on the surface of a plastic substrate.
상기 종래 봉지 기술은 주로 화학적 기상 증착법을 이용한 SiO2, SiNx, In2O3 등의 무기 박막을 증착하여 소자를 수분으로부터 봉지하는 방식이다. 그러나 무기박막 증착 시 핀홀이 형성되고, 플렉서블 소자에 적용 시 물리적인 손상으로 인해 생기는 결함이 발생할 수 있어 수분 및 산소가 투과되는 현상이 생기게 되어 봉지막으로서의 기능을 상실하게 된다. 이러한 휘어짐에 따른 봉지층의 결함을 줄이기 위해 최근에는 무기 박막과 폴리머 박막을 교대로 적층하는 방식이 연구되고 있다. 한편, 박막 내의 핀홀 형성의 억제 및 얇은 박막을 제작하기 위해 자기 제한 반응(self-limiting-reaction)을 기반으로 한 원자층 증착법을 이용하여 Al2O3, SiO2, TiO2 등의 무기박막을 제작하는 방식이 연구되고 있지만 한주기당 0.1nm 정도로 증착되는 느린 증착 속도로 인해 생산 공정에 적용하기 어려운 점이 있다.
The conventional sealing technique is a method in which an inorganic thin film such as SiO 2 , SiN x , or In 2 O 3 is deposited by chemical vapor deposition to seal the device from moisture. However, when an inorganic thin film is deposited, a pinhole is formed, and when applied to a flexible device, a defect caused by physical damage may occur, causing a phenomenon that moisture and oxygen are permeated, and the function as a sealing film is lost. Recently, a method of alternately stacking an inorganic thin film and a polymer thin film has been studied in order to reduce defects in the sealing layer due to such warpage. On the other hand, inorganic thin films such as Al 2 O 3 , SiO 2 and TiO 2 are formed by atomic layer deposition based on the self-limiting-reaction to suppress the formation of pinholes in thin films and to fabricate thin films. However, it is difficult to apply to the production process due to the slow deposition rate which is deposited to about 0.1 nm per one week.
이러한 배경 하에, 본 발명자들은 아주 얇은(~25nm) 무기박막층을 원자층 증착법을 이용하여 제작하고 플라즈마 보강 화학기상 증착법을 이용하여 상대적으로 두꺼운 폴리머박막을 증착함으로써 핀홀이 적은 무기박막 제작과 빠른 증착 속도로 폴리머박막을 제작하여 이들 막들을 적층할 수 있었다. 폴리머 박막층과 무기박막층의 적층 구조에서 Si-O 결합을 갖는 십자형태의 물질(예를 들어, 테트라키스(트리메틸실릴옥시)실란)을 폴리머 박막층의 전구체로 사용하였다. 본 발명은 플라즈마 보강 화학기상 증착법을 사용하여 플라즈마 폴리머를 증착함으로써 기존의 화학적 폴리머에 비하여 폴리머 형성시간 및 폴리머 특성을 크게 향상시킬 수 있다.
Under these circumstances, the present inventors fabricated a very thin (~ 25 nm) inorganic thin film layer using an atomic layer deposition method and deposited a relatively thick polymer thin film by using a plasma enhanced chemical vapor deposition method, The polymer thin films were fabricated and laminated. A cross-shaped substance (for example, tetrakis (trimethylsilyloxy) silane) having Si-O bonds in the laminated structure of the polymer thin film layer and the inorganic thin film layer was used as a precursor of the polymer thin film layer. The present invention can significantly improve polymer formation time and polymer properties compared to conventional chemical polymers by depositing a plasma polymer using plasma enhanced chemical vapor deposition.
본 발명의 목적은 유연성이 확보되고 봉지 특성이 향상된 유기전자소자용 다층 박막 봉지를 제공하는 것이다.SUMMARY OF THE INVENTION An object of the present invention is to provide a multilayer thin film encapsulation for an organic electronic device in which flexibility is secured and encapsulation characteristics are improved.
본 발명의 다른 목적은 상기 유기전자소자용 다층 박막 봉지를 포함하는 유기전자소자를 제공하는 것이다.
Another object of the present invention is to provide an organic electronic device including the multilayer thin film bag for the organic electronic device.
상기 과제를 해결하기 위하여, 본 발명은 하기 화학식 1로 표시되는 전구체 물질을 사용하여 제조되는 플라즈마 중합체 박막, 및 무기 박막을 포함하는 유기전자소자용 다층 박막 봉지를 제공한다.In order to solve the above problems, the present invention provides a multilayer thin film encapsulation for an organic electronic device comprising a thin film of a plasma polymer prepared using a precursor material represented by the following formula (1) and an inorganic thin film.
[화학식 1][Chemical Formula 1]
상기 식에서, R1 내지 R12는 각각 독립적으로 H 또는 C1-C5 알킬이다.Wherein R 1 to R 12 are each independently H or C 1 -C 5 alkyl.
종래의 화학적 기상 증착법이나 물리적 기상 증착법을 이용한 박막은 핀홀 생성으로 인하여 무기층의 봉지 특성이 저하되는 단점을 가지고 있으며 폴리머막의 경우 단일막으로는 수분이나 산소를 차단하는 능력이 거의 없다.
Conventional thin films using chemical vapor deposition or physical vapor deposition have the disadvantage that the sealing property of the inorganic layer is deteriorated due to the formation of pinholes. In the case of the polymer film, the single film has little ability to block moisture or oxygen.
본 발명은 화학 구조상 상, 하, 좌, 우가 대칭인 십자형태의 분자구조를 가지면서 Si-O 결합을 가진 상기 화학식 1로 표시되는 유·무기 전구체를 이용하여 증착된 폴리머 박막은 소수성을 가지며, 이를 무기 박막과 적층하여 무기층의 봉지 특성 저하를 방지하고 폴리머막의 차단 능력을 향상시키는 것을 특징으로 한다.
The present invention relates to a polymer thin film deposited by using an organic / inorganic precursor represented by Chemical Formula 1 having a Si-O bond and having a cross-shaped molecular structure symmetrical in chemical structure, lower, left, and right symmetry, Which is laminated with an inorganic thin film to prevent the degradation of the sealing property of the inorganic layer and to improve the blocking ability of the polymer film.
상기 전구체 물질과 관련하여, 상기 화학식 1에서 R1 내지 R12는 각각 독립적으로 H 또는 C1-C5 알킬일 수 있으며, 상기 알킬의 예로는 메틸, 에틸, 프로필 및 부틸 등을 들 수 있다. 이들 알킬은 직쇄형(linear) 또는 분지형(branched)일 수 있다.Regarding the precursor material, R 1 to R 12 in
본 발명의 일 실시예에 있어서, 상기 화학식 1로 표시되는 전구체 물질은 하기 화학식 2로 표시되는, R1 내지 R12가 각각 메틸인 테트라키스(트리메틸실릴옥시)실란 (Tetrakis(trimethylsilyloxy)silane, TTMSS)일 수 있다.In one embodiment of the present invention, the precursor material represented by Formula 1 is a tetrakis (trimethylsilyloxy) silane, TTMSS (trimethylsilyloxy) silane, wherein R 1 to R 12 are each methyl, ).
[화학식 2](2)
본 발명에서는 폴리머 박막층과 무기박막층의 적층 구조에서 상기 화학식 1로 표시되는 물질을 폴리머 박막층의 전구체로 사용하여 상대적으로 낮은 두께로 봉지막의 기능을 향상시킬 수 있어 유연성 확보 뿐만 아니라 봉지막 역할을 할 수 있는 폴리머 박막층을 통해 소자 구현 시 기존 제품보다 낮은 두께로 높은 성능의 봉지막을 구현할 수 있다.
In the present invention, the polymer thin film layer and the inorganic thin film layer can be used as a precursor of the polymer thin film layer in the laminated structure of the polymer thin film layer and the inorganic thin film layer to improve the function of the sealing film with a relatively low thickness, Through the polymer thin film layer, it is possible to realize a high performance sealing film with lower thickness than the existing product.
본 발명에서, 상기 플라즈마 중합체 박막은 무기 박막 상부 또는 하부에 적층되거나, 또는 무기 박막 사이에 적층될 수 있다. 바람직하기로, 상기 플라즈마 중합체 박막은 무기 박막 사이에 적층될 수 있다.
In the present invention, the plasma polymer thin film may be laminated on or under the inorganic thin film, or laminated between the inorganic thin films. Preferably, the plasma polymer thin film may be laminated between the inorganic thin films.
본 발명에서, 상기 플라즈마 중합체 박막은 플라즈마 보강 화학기상 증착법(Plasma Enhanced Chemical Vapor Deposition, PECVD)을 이용하여 제조될 수 있다. 이때, 플라즈마로 인한 데미지를 최소화 하기 위해 10W 이하의 파워를 사용하여서 중합체 박막을 증착할 수 있다.
In the present invention, the plasma polymer thin film may be manufactured by using Plasma Enhanced Chemical Vapor Deposition (PECVD). At this time, the polymer thin film can be deposited using a power of 10 W or less in order to minimize the damage caused by the plasma.
본 발명에서, 상기 무기 박막은 원자층 증착법을 이용하여 제조될 수 있다. 상기 원자층 증착법은 유기소자에 적용가능한 낮은 공정온도(100℃ 이하)에서 수행된다. 바람직하기로, 상기 원자층 증착법은 박막 내의 핀홀 형성의 억제 및 얇은 박막을 제작하기 위해 자기 제한 반응(self-limiting-reaction)을 기반으로 한 원자층 증착법을 이용하여 증착시킬 수 있다.
In the present invention, the inorganic thin film can be produced by atomic layer deposition. The atomic layer deposition method is performed at a low process temperature (100 DEG C or less) applicable to organic devices. Preferably, the atomic layer deposition method can be deposited using atomic layer deposition based on self-limiting-reaction to suppress pinhole formation in the thin film and to form a thin film.
본 발명에서, 상기 무기 박막은 Al2O3, SiO2, TiO2 또는 이의 조합을 사용하여 제조될 수 있다.
In the present invention, the inorganic thin film may be produced using Al 2 O 3 , SiO 2 , TiO 2, or a combination thereof.
본 발명의 일 실시예에서는 핀홀 생성을 줄이기 위해 원자층 증착법을 이용하여 Al2O3 무기 박막을 제작하고 소수성인 테트라키스(트리메틸실릴옥시)실란 폴리머층을 플라즈마를 이용한 화학 기상 증착법을 이용하여 제작하였다.
In an embodiment of the present invention, an Al 2 O 3 inorganic thin film is formed by atomic layer deposition to reduce pinhole formation, and a hydrophobic tetrakis (trimethylsilyloxy) silane polymer layer is formed by a chemical vapor deposition method using a plasma Respectively.
본 발명에서, 상기 유기전자소자는 플렉서블 유기전자소자일 수 있다.
In the present invention, the organic electronic device may be a flexible organic electronic device.
본 발명에서, 상기 유기전자소자는 유기 발광 다이오드, 유기 태양 전지 또는 유기 박막 트랜지스터일 수 있다.
In the present invention, the organic electronic device may be an organic light emitting diode, an organic solar cell, or an organic thin film transistor.
본 발명의 일 실시예에서는 TTMSS 폴리머를 사용함으로써 휘어지는 폴리머층의 특성뿐만 아니라 무기층과 적층구조로 사용하였을 때 봉지 특성이 상당히 향상되는 것을 확인할 수 있었다. 이로써 본 발명의 무기층과 폴리머층을 적층하는 구조의 봉지 기술이 적용되는 플렉서블 유기전자소자, 구체적으로 유기 발광 다이오드, 유기 태양 전지 또는 유기 박막 트랜지스터 등의 다양한 제품에 있어서 산소 및 수분을 차단할 수 있음을 알 수 있다.
It was confirmed that, in one embodiment of the present invention, when the TTMSS polymer is used, not only the characteristics of the bent polymer layer but also the sealing properties when used as a laminate structure with the inorganic layer are significantly improved. Thus, it is possible to block oxygen and moisture in various products such as a flexible organic electronic device to which a sealing technique of stacking an inorganic layer and a polymer layer of the present invention is applied, specifically organic light emitting diodes, organic solar cells or organic thin film transistors .
또한, 본 발명은 상기 화학식 1로 표시되는 전구체 물질을 사용하여 제조되는 플라즈마 중합체 박막, 및 무기 박막을 포함하는 유기전자소자용 다층 박막 봉지를 포함하는 유기전자소자를 제공한다.
The present invention also provides an organic electronic device including a multilayer thin film encapsulation for an organic electronic device including a thin film of a plasma polymer produced using the precursor material represented by the above formula (1) and an inorganic thin film.
본 발명에서, 상기 유기전자소자는 플렉서블 유기전자소자일 수 있다.
In the present invention, the organic electronic device may be a flexible organic electronic device.
본 발명에서, 상기 유기전자소자는 유기 발광 다이오드, 유기 태양 전지 또는 유기 박막 트랜지스터일 수 있다.
In the present invention, the organic electronic device may be an organic light emitting diode, an organic solar cell, or an organic thin film transistor.
본 발명은 Si-O 결합을 갖는 십자형태의 유·무기 전구체 물질을 사용하여 제조되는 플라즈마 중합체 박막, 및 무기 박막을 포함하는 유기전자소자용 다층 박막 봉지를 제공함으로써 유기전자소자에 산소나 수분의 침투를 효과적으로 억제하여 소자 열화 현상을 방지할 수 있다. 본 발명의 다층 박막 봉지는 상기 전구체 물질을 사용하여 제조된 플라즈마 중합체 박막을 폴리머 박막으로서 사용함으로써 유연성을 구현할 수 있어 디스플레이 산업분야에서 특히 플렉서블 유기전자소자에 사용되는 다양한 기판에 적용 가능하다. 또한, 박막을 사용하는 봉지기술에서 무기층 사이에 상기 전구체 물질을 사용하여 제조된 플라즈마 중합체 박막을 삽입하여 봉지 특성을 향상시키고 휘어짐에 대한 내구성을 강화시킬 수 있다.
The present invention provides a multilayer thin film encapsulation for an organic electronic device comprising a thin film of a plasma polymer produced by using a cross-shaped oil-and-inorganic precursor material having Si-O bonds and an inorganic thin film, The penetration can be effectively suppressed and the device deterioration phenomenon can be prevented. The multilayer thin film encapsulation of the present invention can realize flexibility by using a plasma polymer thin film produced using the precursor material as a polymer thin film, and is applicable to various substrates used in flexible organic electronic devices in the display industry. In addition, in a sealing technique using a thin film, the plasma polymer thin film produced using the precursor material between the inorganic layers can be inserted to improve the sealing characteristics and enhance the durability against warping.
도 1은 무기박막을 제작하기 위해 사용되는 원자층 증착 장치의 개략도이다.
도 2는 폴리머 박막을 제작하기 위한 플라즈마 보강 화학기상 증착(Plasma Enhanced Chemical Vapor Deposition, PECVD) 장치의 개략도이다.
도 3은 수분 및 산소 투과도 측정에 사용된 필름의 형태 모식도이다.
도 4는 Ca-test 장비의 개략도이다.
도 5는 TTMSS 폴리머 박막을 무기박막 사이에 증착하였을 때의 봉지 특성효과를 측정한 결과이다.1 is a schematic view of an atomic layer deposition apparatus used for manufacturing an inorganic thin film.
2 is a schematic view of a plasma enhanced chemical vapor deposition (PECVD) apparatus for fabricating a polymer thin film.
FIG. 3 is a schematic view of the morphology of a film used for measurement of moisture and oxygen permeability. FIG.
Figure 4 is a schematic view of a Ca-test instrument.
FIG. 5 shows the results of measurement of the sealing characteristics of the TTMSS polymer thin film deposited between the inorganic thin films.
이하, 실시예를 통해 본 발명의 구성 및 효과를 보다 더 구체적으로 설명하고자 하나, 이들 실시예는 본 발명의 예시적인 기재일뿐 본 발명의 범위가 이들 실시예에만 한정되는 것은 아니다.
It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory only and are not restrictive of the invention, as claimed.
실시예Example 1: One: 원자층Atomic layer 증착법을 이용한 무기박막 제작 Fabrication of inorganic thin film by vapor deposition
도 1에 도시된 장치를 사용하여 원자층 증착법을 수행하여 무기박막을 제작하였다. 이때 진공 챔버는 500 mTorr로 유지하고 트리메틸알루미늄(trimethylaluminum), H2O를 챔버와의 압력차이를 통해 주입되는 방식으로 무기박막인 Al2O3를 제작하였다. 플라스틱 기판으로 사용된 폴리에틸렌 나프탈레이트(polyethylene naphthalate, PEN) 표면 전면에 고르게 증착되게 하기 위해서 기판 온도를 85℃로 유지하여 화학반응이 충분히 발생할 수 있는 열에너지를 공급하고 무기물의 주입시간과 잔여가스를 배기하는 시간을 조절하여 공정조건(TMA 1초 - 배기 15초 - H2O 1초 - 배기 15초)을 결정하였다. 한 주기공정을 통해서 0.12 nm 두께의 박막이 증착됨을 확인하였고, 200번 반복하여 두께 24nm~25nm의 무기박막을 제작하였다.
An inorganic thin film was prepared by atomic layer deposition using the apparatus shown in FIG. At this time, the vacuum chamber was maintained at 500 mTorr, and trimethylaluminum and H 2 O were injected through a pressure difference between the chamber and the inorganic thin film Al 2 O 3 . Polyethylene naphthalate (PEN) used as a plastic substrate is kept at a substrate temperature of 85 ° C in order to uniformly deposit on the surface, thereby supplying sufficient thermal energy to cause chemical reaction and exhausting the inorganic material injection time and residual gas (
실시예Example 2: 2: 플라즈마plasma 보강 Reinforcement 화학기상증착법을Chemical vapor deposition 이용한 Used 폴리머박막Polymer thin film 제작 making
도 2에 도시된 플라즈마 보강 화학기상 증착(Plasma Enhanced Chemical Vapor Deposition, PECVD) 장치를 사용하여 폴리머 박막을 제작하였다. 상부의 챔버리드(chamber lid)와 하부의 챔버 바디(chamber body)로 구성되는 공정 챔버를 통해 폴리머 박막 증착공정을 진행하였다. 폴리머 박막의 전구체로서 테트라키스(트리메틸실릴옥시)실란 (tetrakis(trimethylsilyloxy)silane, TTMSS)을 사용하였다. 상기 전구체(precursor)를 반응 가스로 사용하였으며, 200 mTorr로 유지하고 있는 챔버 리드 쪽에 형성된 샤워링을 통해 상기 반응 가스를 챔버 바디 내에 있는 기판받침대(susceptor)의 상면에 안착된 기판 상에 균일하게 분사시켜 박막을 증착시켰다. 반응가스로 사용된 테트라키스(트리메틸실릴옥시)실란은 거품기(bubbler)에서 증기(vapor) 상태를 유지하면서 나올 수 있도록 88℃ 이상의 온도를 유지했으며 챔버(chamber)까지 이동하는 라인에서도 증기 상태를 유지시키기 위해 라인 온도는 99℃로 유지시켜 비활성 기체인 He가스와 함께 챔버로 이동시켰다. 증기 상태인 테트라키스(트리메틸실릴옥시)실란은 기판 받침대(susceptor)로 이루어지는 하부전극에 의해 공급되는 RF(radio frequency) 플라즈마 에너지를 5W로 하여 5분간 증착되어 약 70-80nm의 테트라키스(트리메틸실릴옥시)실란 폴리머 형태의 박막을 생성하였다.
A polymer thin film was prepared using the plasma enhanced chemical vapor deposition (PECVD) apparatus shown in FIG. The polymer film deposition process was performed through a process chamber consisting of a chamber lid on the top and a chamber body on the bottom. Tetrakis (trimethylsilyloxy) silane (TTMSS) was used as a precursor of the polymer thin film. Using the precursor as a reaction gas, the reaction gas was uniformly injected onto a substrate placed on the upper surface of a substrate susceptor in the chamber body through a shower ring formed on the chamber lid side maintained at 200 mTorr To deposit a thin film. The tetrakis (trimethylsilyloxy) silane used as the reaction gas maintained a temperature of 88 ° C or higher so that it could come out while maintaining the vapor state in the bubbler, and maintained the vapor state even in the line moving to the chamber The line temperature was maintained at 99 ° C and transferred to the chamber with He gas as an inert gas. The tetrakis (trimethylsilyloxy) silane in a vapor state was deposited for 5 minutes at a RF power (radio frequency) plasma energy of 5 W supplied by a lower electrode made of a susceptor to form tetrakis (trimethylsilyloxy) silane Oxy) silane polymer.
실시예Example 3: 본 발명 다층 박막 봉지의 수분 및 산소 투과도 측정 3: Measurement of moisture and oxygen permeability of the multilayer thin film encapsulation of the present invention
Ca-test를 이용하여 본 발명 다층 박막 봉지의 수분 및 산소 투과도를 측정하였다.The moisture and oxygen permeability of the multi-layer thin film encapsulant of the present invention was measured using a Ca-test.
측정에 사용된 필름의 형태 모식도는 도 3에 나타내었다. 이때 (a)는 25nm의 Al2O3 층으로 증착된 PEN 기판, (b)는 80nm의 TTMSS 폴리머 층으로 증착된 PEN 기판, (c)는 50nm의 Al2O3 층으로 증착된 PEN 기판, (d)는 25nm의 Al2O3 층 / 80nm의 TTMSS 폴리머 층 / 25nm의 Al2O3 층으로 증착된 PEN 기판을 나타낸다. 상기 기판들에 대하여 도 4에 나타낸 Ca-test 장비를 통해서 봉지 특성을 비교 분석하였다. 유리기판 위에 열 증기 증착법을 이용하여 150nm의 Al을 양쪽 전극에 증착하고 그 사이에 1.0 cm × 1.5 cm의 패턴으로 두께 약 300nm의 Ca을 증착하였다. 전극과 Ca이 증착된 유리기판과 제작된 필름을 레진으로 붙이고 UV 경화를 이용하여 밀봉하여 85℃, 85% 상대습도를 유지하면서 일정 전류를 흘려주었다. 박막이 코팅된 PEN 기판을 투과한 산소와 수분은 Ca을 CaO, Ca(OH)2로 변화시키면서 부도체의 성질을 가지게 한다. 일정 크기로 흐르던 전류는 변화된 Ca 양이 많아짐에 따라 비례하여 감소하게 되고 고전류 유지시간이 봉지 특성의 정도를 나타낸다.The morphology of the film used for the measurement is shown in Fig. (A) is a PEN substrate deposited with a 25 nm Al 2 O 3 layer, (b) a PEN substrate deposited with a TTMSS polymer layer of 80 nm, (c) a PEN substrate deposited with a 50 nm Al 2 O 3 layer, (d) shows a PEN substrate deposited with 25 nm Al 2 O 3 layer / 80 nm TTMSS polymer layer / 25 nm Al 2 O 3 layer. The sealing properties of the substrates were compared and analyzed through the Ca-test equipment shown in FIG. On the glass substrate, 150 nm of Al was deposited on both electrodes by thermal vapor deposition, and Ca of about 300 nm in thickness was deposited therebetween in a pattern of 1.0 cm x 1.5 cm. The electrode and the glass substrate on which the Ca was deposited and the prepared film were attached with resin and sealed with UV curing to maintain a constant current at 85 ° C and 85% relative humidity. Oxygen and moisture permeating through the PEN substrate coated with the thin film change the Ca to CaO and Ca (OH) 2, and make them nonconductive. The current flowing in a certain size decreases proportionally as the amount of Ca changed, and the high current holding time indicates the degree of the sealing characteristic.
그 결과를 도 5에 나타내었다.The results are shown in Fig.
도 5에서, PEN 기판만을 봉지막으로 사용하였을 때 급격하게 Ca의 전도도 특성이 감소하는 경향을 볼 수 있으며 TTMSS 폴리머를 증착한 PEN 기판은 약간의 성능 향상이 있지만 그 효과는 미비한 것을 확인할 수 있다. 무기박막인 Al2O3 25nm, Al2O3 50nm의 결과를 보면 PEN 기판보다는 Ca의 전도도를 오랜 시간 유지할 수 있는 것을 확인할 수 있었고 무기막의 두께 증가로는 봉지 특성이 비효율적으로 상승하는 것을 확인할 수 있었다. 또한, Al2O3(25nm) / TTMSS폴리머(80nm) / Al2O3(25nm) 의 결과를 보면 단일 TTMSS 폴리머 박막으로 사용될 때 낮은 봉지 특성을 보인 것과는 다르게 무기박막과 적층구조로 사용되었을 때 봉지 특성이 매우 향상된 것을 확인할 수 있다. 폴리머박막 삽입이 되지 않은 Al2O3 50nm과 비교하였을 때, 무기층의 두께 변화만을 통한 성능 향상보다 TTMSS 폴리머를 사용한 구조변화를 사용하였을 때 성능, 즉 봉지 특성이 매우 향상되는 것을 볼 수 있다.
In FIG. 5, when the PEN substrate alone is used as a sealing film, the conductivity characteristic of Ca tends to decrease rapidly, and the PEN substrate on which the TTMSS polymer is deposited has a slight improvement in performance, but the effect is insignificant. An inorganic thin film of Al 2 O 3 25nm, Al 2 O The results of 3 50nm PEN substrate than was confirmed that the Ca in the conductivity can be maintained long inorganic film thickness increase is found that the sealing property is inefficient rise there was. In addition, the results of Al 2 O 3 (25 nm) / TTMSS polymer (80 nm) / Al 2 O 3 (25 nm) show that when used as a single TTMSS polymer thin film, It can be confirmed that the sealing characteristic is improved remarkably. Compared with 50 nm of Al 2 O 3 not doped with a polymer thin film, it is seen that the performance, that is, the sealing characteristic, is greatly improved when the structural change using the TTMSS polymer is used rather than only the change in the thickness of the inorganic layer.
Claims (9)
[화학식 1]
상기 식에서, R1 내지 R12는 각각 독립적으로 H 또는 C1-C5 알킬이다.
A multilayer thin film encapsulation for an organic electronic device comprising a thin film of a plasma polymer produced by using a precursor material represented by the following formula (1), and an inorganic thin film:
[Chemical Formula 1]
Wherein R 1 to R 12 are each independently H or C 1 -C 5 alkyl.
The multi-layer thin film pouch for organic electronic devices according to claim 1, wherein the plasma polymer thin film is laminated on or under the inorganic thin film.
The multi-layer thin film pouch for organic electronic devices according to claim 1, wherein the plasma polymer thin film is laminated between inorganic thin films.
The multi-layer thin film pouch for organic electronic devices according to claim 1, wherein the plasma polymer thin film is produced by plasma enhanced chemical vapor deposition (PECVD).
The multi-layer thin film pouch for organic electronic devices according to claim 1, wherein the inorganic thin film is produced by atomic layer deposition.
The multi-layer thin film pouch for organic electronic devices according to claim 1, wherein the inorganic thin film is made of Al 2 O 3 , SiO 2 , TiO 2 or a combination thereof.
The multilayer thin film encapsulation for organic electronic devices according to claim 1, wherein the organic electronic device is a flexible organic electronic device.
The multi-layer thin film pouch for organic electronic devices according to claim 1, wherein the organic electronic device is an organic light emitting diode, an organic solar cell or an organic thin film transistor.
9. An organic electronic device comprising the multilayer thin film bag for an organic electronic device according to any one of claims 1 to 8.
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| KR20160150606A (en) * | 2015-06-22 | 2016-12-30 | 도쿄엘렉트론가부시키가이샤 | Laminated sealing film forming method and forming apparatus |
| KR20170019553A (en) * | 2015-08-11 | 2017-02-22 | 삼성디스플레이 주식회사 | Display apparatus and method of manufacturing the same |
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| KR20190093833A (en) * | 2018-02-01 | 2019-08-12 | 삼성디스플레이 주식회사 | Encapsulating Structure, Organic light emitting display having the encapsulating structure, and method of manufacturing thereof |
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| KR101255232B1 (en) | 2006-01-27 | 2013-04-16 | 삼성디스플레이 주식회사 | A composition for an electron transporting layer, an electron transporting layer prepared therefrom, and an organic electroluminescence device comprising the electron transmitting layer |
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| KR20120138307A (en) * | 2011-06-14 | 2012-12-26 | 삼성디스플레이 주식회사 | Organic light emitting diode display and method for manufacturing the same |
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| KR20160150606A (en) * | 2015-06-22 | 2016-12-30 | 도쿄엘렉트론가부시키가이샤 | Laminated sealing film forming method and forming apparatus |
| KR20170019553A (en) * | 2015-08-11 | 2017-02-22 | 삼성디스플레이 주식회사 | Display apparatus and method of manufacturing the same |
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