JP6226347B2 - 封止材フィルムの信頼寿命を評価する方法及び上記フィルムの信頼度評価装置 - Google Patents
封止材フィルムの信頼寿命を評価する方法及び上記フィルムの信頼度評価装置 Download PDFInfo
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- JP6226347B2 JP6226347B2 JP2016521210A JP2016521210A JP6226347B2 JP 6226347 B2 JP6226347 B2 JP 6226347B2 JP 2016521210 A JP2016521210 A JP 2016521210A JP 2016521210 A JP2016521210 A JP 2016521210A JP 6226347 B2 JP6226347 B2 JP 6226347B2
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Images
Classifications
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/84—Systems specially adapted for particular applications
- G01N21/88—Investigating the presence of flaws or contamination
- G01N21/95—Investigating the presence of flaws or contamination characterised by the material or shape of the object to be examined
- G01N21/958—Inspecting transparent materials or objects, e.g. windscreens
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- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
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- H—ELECTRICITY
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- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/10—Primary casings; Jackets or wrappings
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- H01M50/193—Organic material
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
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- H10K85/10—Organic polymers or oligomers
- H10K85/151—Copolymers
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Description
図1のように、水分吸収剤の含量によってヘイズ値が徐々に増加する傾向を示し、したがって、水分吸収剤の含量は、ヘイズの値を決定する主要因子になることができる。
D=k/Hz
図6に示されたように、本出願の上記信頼度測定装置は、光源11、積分球12及び測定部13を含む。
D=k/Hz
D=−αHz+β
Hz≧30%
DnSiQ(4−n)
(1)封止材フィルム形成用溶液の製造
水分吸着剤として平均粒径が5μmである焼成ドロマイト(calcined dolomite)100g及び溶剤としてMEKを固形分50重量%の濃度で投入し、ボールミリング作業を通じて水分吸収剤溶液を製造した。常温で反応器にシラン変性エポキシ樹脂(KSR−177、国都化学)200g及びフェノキシ樹脂(YP−50、東都化成)150gを投入し、メチルエチルケトンで希釈した。上記均質化された溶液に硬化剤であるイミダゾール(四国化成)4gを投入した後、1時間高速撹拌し、水分防止層溶液を製造した。上記溶液にあらかじめ準備した水分吸収剤溶液を焼成ドロマイトの含量が封止材フィルムのベース樹脂100重量部に対して10重量部となるように投入し、混合し、封止材フィルム形成用溶液を製造した。この時に使用されたエポキシ系ベース樹脂の硬化後の屈折率は、アッベ屈折計を通じて測定した場合、1.52であり、焼成ドロマイトの場合、1.8の屈折率を有するものと現われた。水分と反応時に焼成ドロマイトの水和反応によって屈折率が1.57に変わり、ベース樹脂屈折率と類似になった。
上記で準備しておいた封止材フィルム形成用溶液を離型PETの離型面に塗布し、110℃に10分間乾燥し、厚さが40μmである封止材フィルムを形成した後、25℃及び50%の相対湿度条件に露出しないように水分遮断用密封封筒に入れて保管した。
水分吸収剤の含量をベース樹脂100重量部に対して20重量部になるように投入したことを除いて実施例1と同一の方式で封止材フィルムを製造した。
水分吸収剤の含量をベース樹脂100重量部に対して30重量部になるように投入したことを除いて実施例1と同一の方式で封止材フィルムを製造した。
水分吸収剤の含量をベース樹脂100重量部に対して50重量部になるように投入したことを除いて実施例1と同一の方式で封止材フィルムを製造した。
平均粒径が100nmである水分吸収剤を投入したことを除いて実施例2と同一の方式で封止材フィルムを製造した。
製造されたフィルムを25℃及び50%の相対湿度条件に3時間露出させた後、水分遮断用密封用フィルムに入れて保管したことを除いて、実施例1と同一の方式で封止材フィルムを製造した。
製造されたフィルムを25℃及び50%の相対湿度条件に5時間露出させた後、水分遮断用密封用フィルムに入れて保管したことを除いて、実施例1と同一の方式で封止材フィルムを製造した。
製造されたフィルムを25℃及び50%の相対湿度条件に10時間露出させた後、水分遮断用密封用フィルムに入れて保管したことを除いて、実施例1と同一の方式で封止材フィルムを製造した。
水分吸収剤の含量をベース樹脂100重量部に対して5重量部になるように投入したことを除いて実施例1と同一の方式で封止材フィルムを製造した。
平均粒径が100nmである水分吸収剤を投入したことを除いて実施例1と同一の方式で封止材フィルムを製造した。
実施例で製造されたフィルムの粘度を25℃で130℃まで昇温しながら、点弾性測定器(Advanced Rheometric Expansion System、ARES)を利用して1Hzのfrequency及び5%のstrain条件で測定した。
実施例及び比較例で製造されたフィルムのヘイズを測定するために、別途の試験片を別に製造した。ヘイズの場合、厚さによっても変わるので、試験片フィルムの厚さをすべて40μmと同一に製造して評価した。硬化性製品の場合硬化剤がパウダー形態に分散している場合、硬化剤によって光が散乱されるため、このような影響を除去するために、離型フィルムの上で接着フィルムを硬化させて、硬化剤をすべてメルティングさせた後、水分吸着剤だけの影響性を有するヘイズを測定した。一方、硬化性フィルムではない場合には、そのままヘイズを評価した。ヘイズメーターは、日本電色社のNDH−5000を利用して測定し、測定規格は、JIS K7105にして測定し、製造された試験片を水分遮断用密封封筒から取り出した時点から、下記表1の25℃及び50%の相対湿度条件に露出時間経過後にヘイズ値を測定した。
実施例1〜7及び比較例1〜3の粘着フィルムを利用して6mmのベゼルを有する有機発光パネルを製造し、恒温恒湿チャンバで85℃の温度及び85%の相対湿度条件に1000時間放置した後、光学顕微鏡でダークスポットの生成有無を観察し、下記表1に示す。
1mm×50mm×50mmサイズ二つの板ガラスの間に実施例で製造された厚さ40μmのフィルムを40mm×40mmサイズに裁断して中央に位置させ、真空熱圧着し、硬化性粘着フィルムの場合、硬化させた。製造された粘着フィルムを85℃の温度及び85%の相対湿度の条件で0時間〜1200時間維持し、上記粘着フィルム最外郭端部から上記フィルムの中心部に水分が浸透し、透明化が起きた長さを光学顕微鏡を使用して測定した。
Claims (9)
- ベース樹脂及び水分吸収剤を含むフィルムのヘイズ(haze)を水分遮断用密封封筒から取り出した時点から、25℃及び50%の相対湿度の条件で1時間以内に測定し、上記測定されたヘイズ値の減少量を利用してフィルムの信頼寿命を評価する方法であって、
上記ヘイズ値の減少量が、下記一般式1を満足する、フィルムの信頼寿命を評価する方法:
上記フィルムのヘイズ値の減少量(%)は、上記フィルムを水分遮断用密封封筒から取り出した時点から、25℃及び50%の相対湿度の条件で1時間以内にヘイズメーターで測定した上記フィルムのヘイズ値の減少量(%)を示し、
mは、0超過であり、
Φは、ベース樹脂に対する水分吸収剤の含量を示し、
hは、フィルムの厚さを示し、
rは、水分吸収剤の平均粒径を示し、
n g は、水分吸収剤の屈折率を示し、
nは、ベース樹脂の屈折率を示す。 - 測定されたフィルムのヘイズ値が高いほど上記フィルムの信頼寿命が高いものと評価する、請求項1に記載の方法。
- フィルムが下記一般式3を満足する、請求項1に記載の方法:
[一般式3]
D=−α×Hz+β
上記一般式3で、
Hzは、上記フィルムを水分遮断用密封封筒から取り出した時点から、25℃及び50%の相対湿度の条件で1時間以内にヘイズメーターで測定した上記フィルムのヘイズ値(%)を示し、
Dは、2枚のガラス基板の間に上記フィルムをラミネートし、85℃の温度及び85%の相対湿度の条件で0〜1500時間維持した後に測定した上記フィルムの水分浸透距離(mm)を示し、
αは、0.01以上であり、
βは、1.0以上であり、Dより大きい。 - 2以上のフィルムのヘイズ値を比較して評価する、請求項1に記載の方法。
- 同一のサイズ及び同一種類の水分吸収剤を含むフィルムに対して同一の条件下で測定したヘイズ値を比較する、請求項4に記載の方法。
- 2以上のフィルムのヘイズ値及び上記ヘイズ値を有するフィルムを2枚のガラス基板の間にラミネートし、85℃の温度及び85%の相対湿度の条件で0〜1500時間維持した後に測定した上記フィルムの水分浸透距離を比較して評価する、請求項1に記載の方法。
- 85℃の温度及び85%の相対湿度の条件で同一の時間維持する条件の下で測定した水分浸透距離を比較する、請求項6に記載の方法。
- 試料フィルムに光を照射する光源と;
上記試料フィルムを透過する光を検出してヘイズを測定する積分球と;
上記積分球から測定されたヘイズ値の減少量を利用してフィルムの信頼度を測定する測定部と;
を含む、ベース樹脂及び水分吸収剤を含むフィルムの信頼度測定装置であって、
測定部は、
積分球から測定されたフィルムのヘイズ値を入力される入力部と;
上記入力されたヘイズ値からフィルムの信頼度を評価する評価部と;
上記評価結果を表示する表示部と;を含み、
評価部は、下記一般式1によってmを演算する演算部をさらに含む、フィルムの信頼度測定装置:
上記フィルムのヘイズ値の減少量(%)は、上記フィルムを水分遮断用密封封筒から取り出した時点から、25℃及び50%の相対湿度の条件で1時間以内にヘイズメーターで測定した上記フィルムのヘイズ値の減少量(%)を示し、
mは、0超過であり、
Φは、ベース樹脂に対する水分吸収剤の含量を示し、
hは、フィルムの厚さを示し、
rは、水分吸収剤の平均粒径を示し、
n g は、水分吸収剤の屈折率を示し、
nは、ベース樹脂の屈折率を示す。 - 試料フィルム内の水分吸収剤の含量、上記水分吸収剤の平均粒径、上記水分吸収剤の屈折率、上記試料フィルムの厚さ、上記試料フィルム内のベース樹脂の屈折率よりなる群から選択された1つ以上の値が上記入力部に追加に入力される、請求項8に記載の信頼度測定装置。
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CN105377966B (zh) | 2019-05-28 |
TWI548682B (zh) | 2016-09-11 |
US20160131599A1 (en) | 2016-05-12 |
KR101642568B1 (ko) | 2016-07-25 |
EP3012617A4 (en) | 2017-03-29 |
WO2014204256A2 (ko) | 2014-12-24 |
CN105377966A (zh) | 2016-03-02 |
EP3012617B1 (en) | 2021-04-21 |
CN105358963A (zh) | 2016-02-24 |
CN105358963B (zh) | 2018-10-12 |
KR20140147760A (ko) | 2014-12-30 |
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