JP2005342975A - Transparent barrier film - Google Patents
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Abstract
【課題】酸素バリア性や水蒸気バリア性に優れかつ高透明性を合わせ持つ、エレクトロニクス素子用の透明バリアフィルムを提供すること。
【解決手段】透明プラスチックフィルムの少なくとも片面に窒化珪素膜が成膜されている透明バリアフィルムであって、該窒化珪素膜の元素比がＮ／Ｓｉ＝０．８〜１．４の範囲であり、膜密度が２．１〜３．０ｇ／ｃｍ3 の範囲にあること。透明バリアフィルムの酸素透過度が０．１ｃｃ／ｍ2 ・ｄａｙ以下であり、水蒸気透過度が０．１ｇ／ｍ2 ・ｄａｙ以下であること。
【選択図】なしDisclosed is a transparent barrier film for an electronic device having excellent oxygen barrier properties and water vapor barrier properties and high transparency.
A transparent barrier film having a silicon nitride film formed on at least one surface of a transparent plastic film, wherein the element ratio of the silicon nitride film is in a range of N / Si = 0.8 to 1.4. The film density is in the range of 2.1 to 3.0 g / cm 3 . The oxygen permeability of the transparent barrier film is 0.1 cc / m 2 · day or less, and the water vapor permeability is 0.1 g / m 2 · day or less.
[Selection figure] None
Description
本発明は、液晶素子（ＬＣＤ）、エレクトロルミネッセンス素子（ＥＬ）等に代表されるエレクトロニクス素子用のバリア性を付与した透明バリアフィルムに関するものである。 The present invention relates to a transparent barrier film provided with a barrier property for an electronic device represented by a liquid crystal device (LCD), an electroluminescence device (EL) and the like.
自己発光体である有機ＥＬ素子は、低消費電力、高い応答速度、高視野角等の多くの利点からブラウン管や液晶素子に変わるフラットパネルディスプレイとして注目されている。有機ＥＬ素子は、一般に透明基板上に陽極、有機発光層、陰極を積層し有機ＥＬ素子が形成され、両電極間に電圧を印加することにより有機発光層で発光が生じるものである。 An organic EL element that is a self-luminous element has attracted attention as a flat panel display that is replaced by a cathode ray tube or a liquid crystal element because of many advantages such as low power consumption, high response speed, and high viewing angle. In general, an organic EL element is formed by laminating an anode, an organic light emitting layer, and a cathode on a transparent substrate, and light is emitted from the organic light emitting layer by applying a voltage between the electrodes.
しかしながら、有機ＥＬ素子は非常に酸素や水分に弱いことが知られており、このような有機ＥＬ素子は大気中に暴露した状態で放置すると、酸素、水蒸気の有機ＥＬ素子内への進入による劣化が引き起こされることが知られている。特に陰極層に用いられる仕事関数の低いアルカリ金属、またはアルカリ土類金属は水分により酸化されやすく、酸化されることにより電子の注入が阻害されダークスポットと呼ばれる非発光領域が発生し時間の経過と共に拡大する。この陰極層保護のために必要な水蒸気透過度は、１×１０-6ｇ／ｍ2 ・ｄａｙともいわれている。 However, it is known that organic EL elements are very sensitive to oxygen and moisture. When such organic EL elements are left exposed to the atmosphere, deterioration due to the entry of oxygen and water vapor into the organic EL elements. Is known to be caused. In particular, alkali metals or alkaline earth metals with a low work function used for the cathode layer are easily oxidized by moisture, and when they are oxidized, electron injection is inhibited and a non-light emitting region called a dark spot is generated over time. Expanding. The water vapor permeability necessary for protecting the cathode layer is also said to be 1 × 10 −6 g / m 2 · day.
また、可撓性を有する有機ＥＬディスプレイとして、バリア膜を形成した透明プラスチックフィルム上に有機ＥＬ素子を形成することも盛んに研究されている（特許文献１、非特許文献１参照）。一般的にプラスチックフィルムは、水、酸素のバリア性に乏しいため、有機ＥＬ素子の長寿命化のためにはプラスチックフィルムへのバリア性の付与が不可欠である。 In addition, as an organic EL display having flexibility, formation of an organic EL element on a transparent plastic film on which a barrier film is formed has been actively studied (see Patent Document 1 and Non-Patent Document 1). In general, a plastic film is poor in water and oxygen barrier properties, and therefore it is indispensable to provide barrier properties to the plastic film in order to extend the life of the organic EL element.
この様なガスバリアの劣性を補う方法として、透明プラスチックフィルム上にバリア層を設ける検討が盛んになされている。このバリア層は、主に透明性の高い珪素、アルミニウムなどの金属酸化物や、金属窒化物があげられ、スパッタリング法、イオンプレーティング法、真空蒸着法、ＣＶＤ法などにより形成される。更に、ディスプレイ作製時における種々な工程中での耐熱性、耐薬品性、耐アルカリ性、耐酸性等が要求され、また様々な環境下での高いバリア性を維持することが要求される。 As a method for compensating for such inferiority of the gas barrier, studies for providing a barrier layer on a transparent plastic film have been actively conducted. This barrier layer is mainly made of highly transparent metal oxides such as silicon and aluminum, and metal nitrides, and is formed by sputtering, ion plating, vacuum deposition, CVD, or the like. Furthermore, heat resistance, chemical resistance, alkali resistance, acid resistance, and the like in various processes at the time of manufacturing a display are required, and high barrier properties under various environments are required to be maintained.
窒化珪素膜はバリア性、透明性が高いことが知られているが、成膜方法によっては着色してしまったり（非特許文献１参照）、成膜条件によっては高温、高湿下に放置すると酸化されてしまうことが知られている。ディスプレイの前面板に用いるためには膜の着色は好ましいものではなく、また、酸化されてしまい物性が変化してしまうような膜では高い信頼性が得られない。
本発明は、上記のような問題点を解決するためのものであり、その課題とするところは、酸素バリア性や水蒸気バリア性に優れ、かつ高透明性を合わせ持つ、透明バリアフィルムを提供することにある。 The present invention is for solving the above-mentioned problems, and the object of the present invention is to provide a transparent barrier film having excellent oxygen barrier properties and water vapor barrier properties, and having high transparency. There is.
本発明は、透明プラスチックフィルムの少なくとも片面に窒化珪素膜が成膜されている透明バリアフィルムであって、該窒化珪素膜の元素比がＮ／Ｓｉ＝０．８〜１．４の範囲であり、膜密度が２．１〜３．０ｇ／ｃｍ3 の範囲にあることを特徴とする透明バリアフィルムである。 The present invention is a transparent barrier film in which a silicon nitride film is formed on at least one surface of a transparent plastic film, and the element ratio of the silicon nitride film is in the range of N / Si = 0.8 to 1.4. The transparent barrier film is characterized in that the film density is in the range of 2.1 to 3.0 g / cm 3 .
また、本発明は、請求項１に記載される透明バリアフィルムの酸素透過度が０．１ｃｃ／ｍ2 ・ｄａｙ以下であり、水蒸気透過度が０．１ｇ／ｍ2 ・ｄａｙ以下であることを特徴とする透明バリアフィルムである。 In the present invention, the transparent barrier film described in claim 1 has an oxygen permeability of 0.1 cc / m 2 · day or less and a water vapor permeability of 0.1 g / m 2 · day or less. It is the transparent barrier film characterized.
これまで示してきたように、本発明は、透明プラスチックフィルムの少なくとも片面に窒化珪素膜が成膜されている透明バリアフィルムであって，該窒化珪素膜の元素比がＮ／Ｓｉ＝０．８〜１．４の範囲であり、膜密度が２．１〜３．０ｇ／ｃｍ3 の範囲にあるので、窒化珪素膜が非常に緻密で、かつ応力の少ない構造を取るため、極めて高いバリア性を示す透明バリアフィルムとなる。 As described above, the present invention is a transparent barrier film in which a silicon nitride film is formed on at least one surface of a transparent plastic film, and the element ratio of the silicon nitride film is N / Si = 0.8. Since the film density is in the range of ~ 1.4 and the film density is in the range of 2.1 to 3.0 g / cm 3 , the silicon nitride film has a very dense and low-stress structure, so it has an extremely high barrier property It becomes the transparent barrier film which shows.
以下本発明を詳細に説明する。
本発明に用いられる透明プラスチックフィルムは、バリア層の透明性を生かすために透明なフィルムが好ましい。例えば、ポリエチレンテレフタレート（ＰＥＴ）、ポリエチレンナフタレート（ＰＥＮ）などのポリエステルフィルム、ポリカーボネートフィルム（ＰＣ）、ポリエーテルスルフォン（ＰＥＳ）、ポリカーボネートフィルム、ポリアリレートフィルム、ポリエチレンやポリプロピレンなどのポリオレフィンフィルムや、環状シクロオレフィンを含むシクロオレフィンフィルム、ポリスチレンフィルム、ポリアミドフィルム、ポリ塩化ビニルフィルム、ポリアクリルニトリルフィルム、ポリイミドフィルム等が用いられる。
The present invention will be described in detail below.
The transparent plastic film used in the present invention is preferably a transparent film in order to make use of the transparency of the barrier layer. For example, polyester films such as polyethylene terephthalate (PET) and polyethylene naphthalate (PEN), polycarbonate films (PC), polyether sulfone (PES), polycarbonate films, polyarylate films, polyolefin films such as polyethylene and polypropylene, and cyclic cyclo A cycloolefin film containing olefin, a polystyrene film, a polyamide film, a polyvinyl chloride film, a polyacrylonitrile film, a polyimide film, or the like is used.
延伸、未延伸のどちらでも良く、また機械的強度や寸法安定性を有するものが良い。これらをフィルム状に加工して用いられる。二軸方向に任意に延伸されていても問題ない。また、この基材の表面に、周知の種々の添加剤や安定剤、例えば、帯電防止剤、紫外線防止剤、可塑剤、滑剤などが使用されていても良く、薄膜との密着性を良くするために、前処理としてコロナ処理、低温プラズマ処理、イオンボンバード処理を施しておいても良く、さらに薬品処理、溶剤処理などを施しても良い。 Either stretched or unstretched, and those having mechanical strength and dimensional stability are preferred. These are processed into a film and used. There is no problem even if the film is arbitrarily stretched in the biaxial direction. In addition, various known additives and stabilizers such as antistatic agents, ultraviolet inhibitors, plasticizers, lubricants and the like may be used on the surface of the base material to improve the adhesion to the thin film. Therefore, corona treatment, low temperature plasma treatment, ion bombardment treatment may be performed as pretreatment, and chemical treatment, solvent treatment, etc. may be performed.
本発明の窒化珪素膜は、高いバリア性を有するバリア層として用いられるものであり、窒化珪素膜の元素比がＮ／Ｓｉ＝０．８〜１．４の範囲であり、膜密度が２．１〜３．０ｇ／ｃｍ3 の範囲にあることが好ましい。この範囲を外れると、窒化珪素膜の膜組成が崩れ、膜の緻密さが低下しバリア性の劣化や、湿度による膜の酸化劣化が起こり好ましくない。 The silicon nitride film of the present invention is used as a barrier layer having high barrier properties, the element ratio of the silicon nitride film is in the range of N / Si = 0.8 to 1.4, and the film density is 2. It is preferably in the range of 1 to 3.0 g / cm 3 . Outside this range, the film composition of the silicon nitride film is destroyed, the film density is lowered, and the barrier property is deteriorated and the film is oxidized and deteriorated due to humidity.
このような窒化珪素膜の成膜方法としては，公知の真空蒸着法により形成することができるが、その他の薄膜形成方法である、プラズマＣＶＤ法、触媒化学気相堆積法（Ｃａｔ−ＣＶＤ）、スパッタリング法、イオンプレーティング法により成膜される。本発明で得られるような高い透明性とバリア性を兼ね備える窒化珪素膜を得るためには、プラズマＣＶＤ法、触媒化学気相堆積法、スパッタリング法が適していると考えられる。 As a method for forming such a silicon nitride film, it can be formed by a known vacuum vapor deposition method, but other thin film formation methods such as plasma CVD method, catalytic chemical vapor deposition method (Cat-CVD), The film is formed by sputtering or ion plating. In order to obtain a silicon nitride film having both high transparency and barrier properties as obtained in the present invention, it is considered that plasma CVD, catalytic chemical vapor deposition, and sputtering are suitable.
窒化珪素膜の厚みは５〜１０００ｎｍ、より好ましくは１００〜３００ｎｍの範囲で最適化されるものと考えられる。窒化珪素膜の膜厚が５ｎｍ以下であると高いバリア性が得
られず、またバリア層の厚みが１０００ｎｍを超えるとフィルムのフレキシブル性、透明性を損なうおそれがある。さらに、応力の制御が困難になり、窒化珪素膜にクラックが入りやすくバリア性が低下する恐れがある。
It is considered that the thickness of the silicon nitride film is optimized within a range of 5 to 1000 nm, more preferably 100 to 300 nm. If the thickness of the silicon nitride film is 5 nm or less, high barrier properties cannot be obtained, and if the thickness of the barrier layer exceeds 1000 nm, the flexibility and transparency of the film may be impaired. Furthermore, it becomes difficult to control the stress, and the silicon nitride film is liable to crack and the barrier property may be lowered.
また、窒化珪素膜の膜組成は光電子分光法（ＸＰＳ）により測定が可能であり、具体的な装置としては、（株）島津製作所製：ＥＳＣＡ３２００が挙げられる。また、膜密度についてはＸ線反射率法により測定が可能であり、具体的な測定装置としては、理学電機（株）製：ＡＴＸ−Ｇが挙げられる。 The film composition of the silicon nitride film can be measured by photoelectron spectroscopy (XPS), and a specific apparatus is ESCA3200 manufactured by Shimadzu Corporation. The film density can be measured by the X-ray reflectivity method, and a specific measuring apparatus includes ATX-G manufactured by Rigaku Corporation.
本発明における窒化珪素膜の膜組成は、酸素、および炭素が含まれていても膜密度が、２．１〜３．０ｇ／ｃｍ3 の範囲に入っている限りは何ら問題は無いと考えられる。上記の様な方法で透明プラスチックフィルムを用いて真空成膜法にて窒化珪素膜を付けようとした場合、透明プラスチックフィルム中に含まれる水分や、酸素によって混入してしまう場合が考えられる。
よって、窒化珪素膜中に含まれる酸素組成は制御されているものでは無く、透明プラスチックフィルムの種類、成膜前の脱ガス条件や、成膜中の条件によって変化していくものである。そういった条件の中でも酸素組成比は低いことが好ましい。また、同一条件で窒化珪素膜を脱ガスのないシリコンウエハーに成膜した場合、赤外線吸収法（ＩＲ）によるＳｉ−Ｏ関するピークはほとんど観測されない。
The film composition of the silicon nitride film in the present invention is considered to have no problem as long as the film density is in the range of 2.1 to 3.0 g / cm 3 even if oxygen and carbon are included. . When an attempt is made to attach a silicon nitride film by a vacuum film formation method using a transparent plastic film by the method as described above, it may be mixed by moisture contained in the transparent plastic film or oxygen.
Therefore, the oxygen composition contained in the silicon nitride film is not controlled and changes depending on the type of transparent plastic film, degassing conditions before film formation, and conditions during film formation. Among these conditions, the oxygen composition ratio is preferably low. In addition, when a silicon nitride film is formed on a silicon wafer without degassing under the same conditions, a peak related to Si—O by infrared absorption (IR) is hardly observed.
本発明におけるバリア性とは、酸素透過度（ＪＩＳ Ｋ７１２６のＢ法（等圧法））、および、水蒸気透過度（ＪＩＳ Ｋ７１２９のＢ法（赤外センサー法））を指す。酸素透過度の測定は、ＭＯＣＯＮ社製：ＯＸＴＲＡＮ ２／２１を用いて、温度２５℃、湿度７５％ＲＨの環境下でゼロ点を測定した後の測定値を指す。また、水蒸気透過度の測定は、ＭＯＣＯＮ社製：ＰＥＲＭＡＴＲＡＮ−Ｗ ３／３２を用いて、温度４０℃、湿度９０％ＲＨの環境下での測定値を指す。 The barrier property in the present invention refers to oxygen permeability (JIS K7126 method B (isobaric method)) and water vapor permeability (JIS K7129 method B (infrared sensor method)). The measurement of oxygen permeability refers to the measurement value after measuring the zero point in an environment of temperature 25 ° C. and humidity 75% RH using OXTRAN 2/21 manufactured by MOCON. Moreover, the measurement of water-vapor permeability refers to the measured value in the environment of temperature 40 degreeC and humidity 90% RH using MOCON: PERMATRAN-W 3/32.
本発明の窒化珪素膜によれば膜中の組成、および膜密度を規定することにより窒化珪素膜が緻密な構造、および高いバリア性を得ることが出来、また温度６０℃、湿度９０％ＲＨの環境下に５００時間保存した後の窒化珪素膜の組成を規定することにより高い信頼性を得ることが可能である。 According to the silicon nitride film of the present invention, by defining the composition and film density in the film, the silicon nitride film can have a dense structure and high barrier properties, and has a temperature of 60 ° C. and a humidity of 90% RH. High reliability can be obtained by defining the composition of the silicon nitride film after storage for 500 hours in the environment.
次に実施例を示し本発明をさらに詳細に説明する。 EXAMPLES Next, an Example is shown and this invention is demonstrated further in detail.
（透明プラスチックフィルム上への窒化珪素膜の成膜）
透明プラスチックフィルムとして、ポリエーテルスルホン（ＰＥＳ）フィルム（住友ベークライト（株）製：ＰＥＳフィルム ＵＣＰＥＳ、厚み２００μｍ）を用いて、ロードロックを介して平行平板方式のプラズマＣＶＤ装置内のサンプルホルダーへと導入し、５×１０-7Ｔｏｒｒにまで排気を行った。続いて、サンプルホルダーを１５０℃にまで加熱し、１時間放置することにより脱ガスを行った。
(Deposition of silicon nitride film on transparent plastic film)
Using a polyethersulfone (PES) film (manufactured by Sumitomo Bakelite Co., Ltd .: PES film UCPES, thickness 200 μm) as a transparent plastic film, introduced into a sample holder in a parallel plate type plasma CVD apparatus via a load lock. Then, the exhaust was performed up to 5 × 10 −7 Torr. Subsequently, the sample holder was heated to 150 ° C. and left for 1 hour for degassing.
次に、サンプルホルダー温度を１５０℃に保ったまま、ＳｉＨ4 、ＮＨ3 、Ｈ2 をそれぞれ１０、２０、４００ｓｃｃｍ導入し、コンダクタンスバルブによりチャンバー内の圧力を１０Ｐａに保ち、１３．５６ＭＨｚの高周波電源を用い、投入電力を３００Ｗで透明プラスチックフィルム上に１００ｎｍの窒化珪素膜を形成し透明バリアフィルムを得た。 Next, while maintaining the sample holder temperature at 150 ° C., SiH 4 , NH 3 , and H 2 were introduced at 10, 20, and 400 sccm, respectively, and the pressure in the chamber was maintained at 10 Pa by a conductance valve, and a 13.56 MHz high frequency power source A 100 nm silicon nitride film was formed on the transparent plastic film at an input power of 300 W to obtain a transparent barrier film.
次に、実施例１においてＳｉＨ4 流量を４ｓｃｃｍにした以外は実施例１と同様にして窒化珪素膜を形成し透明バリアフィルムを得た。 Next, a silicon nitride film was formed in the same manner as in Example 1 except that the SiH 4 flow rate was changed to 4 sccm in Example 1 to obtain a transparent barrier film.
次に、実施例１においてＳｉＨ4 流量を１４ｓｃｃｍにした以外は実施例１と同様にして窒化珪素膜を形成し透明バリアフィルムを得た。 Next, a silicon nitride film was formed in the same manner as in Example 1 except that the SiH 4 flow rate was changed to 14 sccm in Example 1 to obtain a transparent barrier film.
次に、実施例１と比較するための実施例４においては、ＳｉＨ4 流量を２０ｓｃｃｍにした以外は実施例１と同様にして窒化珪素膜を形成し透明バリアフィルムを得た。 Next, in Example 4 for comparison with Example 1, a silicon nitride film was formed in the same manner as in Example 1 except that the SiH 4 flow rate was changed to 20 sccm to obtain a transparent barrier film.
次に、実施例１と比較するための実施例５においては、ＳｉＨ4 流量を２ｓｃｃｍ、ＮＨ3 流量を４０ｓｃｃｍにした以外は実施例１と同様にして窒化珪素膜を形成し透明バリアフィルムを得た。 Next, in Example 5 for comparison with Example 1, a silicon nitride film was formed in the same manner as in Example 1 except that the SiH 4 flow rate was 2 sccm and the NH 3 flow rate was 40 sccm to obtain a transparent barrier film. It was.
（窒化珪素膜の組成の測定）
得られた窒化珪素膜の組成の分析は、（株）島津製作所製：ＥＳＣＡ３２００を用いて測定を行った。Ｘ線源にはＭｇα線を使用し、電圧５ｋＶ、電流３０ｍＡに設定した。また、アナライザー透過エネルギーは１０ｅＶとし、光電子の取り込みは０．１ｅＶステップで１ポイントの収拾時間は１００ｍｓとした。
また、膜の深さ方向の情報を得るために、熱陰極型エッチングイオン銃を用いて６０秒のエッチングを１０回行い、デプスプロファイルを得た。窒化珪素膜中の組成比はＳｉ、Ｎ、Ｏピーク面積に、各元素の感度補正係数（Ｓｉ：０．２８８、Ｏ：１．０８２、Ｃ：０．２９３）を用いて補正を行いデプスプロファイルの平均を膜組成とした。
(Measurement of composition of silicon nitride film)
The composition of the obtained silicon nitride film was analyzed using ESCA3200 manufactured by Shimadzu Corporation. Mgα rays were used as the X-ray source, and the voltage was set to 5 kV and the current was set to 30 mA. The analyzer transmission energy was 10 eV, the photoelectron uptake was 0.1 eV, and the collection time for one point was 100 ms.
Further, in order to obtain information in the depth direction of the film, etching was performed 10 times for 60 seconds using a hot cathode type etching ion gun to obtain a depth profile. The composition ratio in the silicon nitride film is corrected by using the sensitivity correction coefficients (Si: 0.288, O: 1.082, C: 0.293) of each element for the Si, N, and O peak areas. Was the film composition.
（窒化珪素膜の膜密度の測定）
得られた窒化珪素膜の密度の分析は、（株）理学電機製：ＡＴＸ−Ｇを用いて測定を行った。Ｘ線源にＣｕＫα線を用い、光学系には、Ｇｅ（１１１）非対称ビーム圧縮光学系を用いた。また、測定条件としてスキャン速度０．１０゜／ｍｉｎ、サンプリング幅０．００２゜、走査範囲２θ＝０．２〜５゜の範囲で測定を行った。得られたデータより付属の解析ソフトを用いて、臨界角付近のフィッティングを行い膜密度を求めた。
(Measurement of silicon nitride film density)
The analysis of the density of the obtained silicon nitride film was performed by using ATX-G manufactured by Rigaku Corporation. A CuKα ray was used as the X-ray source, and a Ge (111) asymmetric beam compression optical system was used as the optical system. Further, the measurement was performed under the conditions of a scanning speed of 0.10 ° / min, a sampling width of 0.002 °, and a scanning range 2θ = 0.2 to 5 °. From the obtained data, using the attached analysis software, fitting near the critical angle was performed to obtain the film density.
（透明バリアフィルムのバリア性の評価）
酸素透過度は、ＭＯＣＯＮ社製：ＯＸＴＲＡＮ ２／２１を用いて、温度２５℃、湿度７５％ＲＨの環境下でゼロ点を測定した後の測定値を用いた。
水蒸気透過度は、ＭＯＣＯＮ社製：ＰＥＲＭＡＴＲＡＮ−Ｗ ３／３２を用いて、温度４０℃、湿度９０％ＲＨの環境下での測定値を用いた。
(Evaluation of barrier properties of transparent barrier film)
The measured value after measuring the zero point in an environment of temperature 25 ° C. and humidity 75% RH was used for oxygen permeability using OXTRAN 2/21 manufactured by MOCON.
For the water vapor transmission rate, a measurement value in an environment of a temperature of 40 ° C. and a humidity of 90% RH was used by using PERMATRAN-W 3/32 manufactured by MOCON.
実施例１〜５について、上記に示すとおり測定したデータを表１に示す。 The data measured for Examples 1-5 as shown above are shown in Table 1.
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| WO2007111098A1 (en) * | 2006-03-24 | 2007-10-04 | Konica Minolta Medical & Graphic, Inc. | Transparent barrier sheet and method for producing same |
| WO2007111074A1 (en) * | 2006-03-24 | 2007-10-04 | Konica Minolta Medical & Graphic, Inc. | Transparent barrier sheet and method for producing transparent barrier sheet |
| WO2007111075A1 (en) * | 2006-03-24 | 2007-10-04 | Konica Minolta Medical & Graphic, Inc. | Transparent barrier sheet and method for producing transparent barrier sheet |
| WO2009001924A1 (en) | 2007-06-27 | 2008-12-31 | Ulvac, Inc. | Resin substrate |
| JP2009031611A (en) * | 2007-07-27 | 2009-02-12 | Ulvac Japan Ltd | Resin substrate |
| JP2009133000A (en) * | 2007-10-30 | 2009-06-18 | Fujifilm Corp | Silicon nitride film, gas barrier film and thin film element using the same |
| JP2010059528A (en) * | 2008-09-08 | 2010-03-18 | Fujifilm Corp | Method for producing gas barrier film |
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| US20140183498A1 (en) * | 2012-12-31 | 2014-07-03 | Saint-Gobain Performance Plastics Corporation | Thin Film Silicon Nitride Barrier Layers On Flexible Substrate |
| WO2019065020A1 (en) * | 2017-09-27 | 2019-04-04 | 富士フイルム株式会社 | Gas barrier film |
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