JP2023505121A - 粘着剤層 - Google Patents
粘着剤層 Download PDFInfo
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- JP2023505121A JP2023505121A JP2022532566A JP2022532566A JP2023505121A JP 2023505121 A JP2023505121 A JP 2023505121A JP 2022532566 A JP2022532566 A JP 2022532566A JP 2022532566 A JP2022532566 A JP 2022532566A JP 2023505121 A JP2023505121 A JP 2023505121A
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- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 2
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- 150000002431 hydrogen Chemical class 0.000 description 2
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 2
- 230000001939 inductive effect Effects 0.000 description 2
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- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 2
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- UWFRVQVNYNPBEF-UHFFFAOYSA-N 1-(2,4-dimethylphenyl)propan-1-one Chemical compound CCC(=O)C1=CC=C(C)C=C1C UWFRVQVNYNPBEF-UHFFFAOYSA-N 0.000 description 1
- JWYVGKFDLWWQJX-UHFFFAOYSA-N 1-ethenylazepan-2-one Chemical compound C=CN1CCCCCC1=O JWYVGKFDLWWQJX-UHFFFAOYSA-N 0.000 description 1
- IVIDDMGBRCPGLJ-UHFFFAOYSA-N 2,3-bis(oxiran-2-ylmethoxy)propan-1-ol Chemical compound C1OC1COC(CO)COCC1CO1 IVIDDMGBRCPGLJ-UHFFFAOYSA-N 0.000 description 1
- JAHNSTQSQJOJLO-UHFFFAOYSA-N 2-(3-fluorophenyl)-1h-imidazole Chemical compound FC1=CC=CC(C=2NC=CN=2)=C1 JAHNSTQSQJOJLO-UHFFFAOYSA-N 0.000 description 1
- PFHOSZAOXCYAGJ-UHFFFAOYSA-N 2-[(2-cyano-4-methoxy-4-methylpentan-2-yl)diazenyl]-4-methoxy-2,4-dimethylpentanenitrile Chemical compound COC(C)(C)CC(C)(C#N)N=NC(C)(C#N)CC(C)(C)OC PFHOSZAOXCYAGJ-UHFFFAOYSA-N 0.000 description 1
- AUYVPDNKYBPWPQ-UHFFFAOYSA-N 2-[4-(4-bromobenzoyl)phenoxy]ethyl prop-2-enoate Chemical compound C1=CC(Br)=CC=C1C(=O)C1=CC=C(OCCOC(=O)C=C)C=C1 AUYVPDNKYBPWPQ-UHFFFAOYSA-N 0.000 description 1
- 125000006176 2-ethylbutyl group Chemical group [H]C([H])([H])C([H])([H])C([H])(C([H])([H])*)C([H])([H])C([H])([H])[H] 0.000 description 1
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- UPMLOUAZCHDJJD-UHFFFAOYSA-N 4,4'-Diphenylmethane Diisocyanate Chemical compound C1=CC(N=C=O)=CC=C1CC1=CC=C(N=C=O)C=C1 UPMLOUAZCHDJJD-UHFFFAOYSA-N 0.000 description 1
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- 230000001681 protective effect Effects 0.000 description 1
- 238000010526 radical polymerization reaction Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 238000007142 ring opening reaction Methods 0.000 description 1
- 125000002914 sec-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000005361 soda-lime glass Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 239000011135 tin Substances 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 description 1
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- 229950001353 tretamine Drugs 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
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Abstract
Description
DC60=100×(C60.1-C60.2)/C60.2
数式1でDC60はクリープ変形率の差であり、C60.1は前記第1領域の60℃でのクリープ変形率であり、C60.2は前記第2領域の60℃でのクリープ変形率である。
DCM20=100×(CM20.1-CM20.2)/CM20.2
数式3でDCM20はクリープ変形率の差であり、CM20.1は前記第1領域の-20℃でのクリープ変形率であり、CM20.2は前記第2領域の-20℃でのクリープ変形率である。
DM60=100×(M60.1-M60.2)/M60.2
数式5でMC60は貯蔵弾性率の差であり、M60.1は前記第1領域の60℃での貯蔵弾性率であり、M60.2は前記第2領域の60℃での貯蔵弾性率である。
DM30=100×(M30.1-M30.2)/M30.2
数式6でDM30は貯蔵弾性率の差であり、M30.1は前記第1領域の30℃での貯蔵弾性率であり、M30.2は前記第2領域の30℃での貯蔵弾性率である。
DM20=100×(M20.1-M20.2)/M20.2
数式7でDM20は貯蔵弾性率の差であり、M20.1は前記第1領域の-20℃での貯蔵弾性率であり、M20.2は前記第2領域の-20℃での貯蔵弾性率である。
DR60=100×(R60.1-R60.2)/R60.2
数式2でDR60は回復率の差であり、R60.1は前記第1領域の60℃での回復率であり、R60.2は前記第2領域の60℃での回復率である。
DRM20=100×(RM20.1-RM20.2)/RM20.2
数式4でDM20は回復率の差であり、RM20.1は前記第1領域の-20℃での回復率であり、RM20.2は前記第2領域の-20℃での回復率である。
DPG=100×(PG.1-PG.2)/PG.2
数式8でDPGは剥離力の差であり、PG.1は前記第1領域のガラスに対する剥離力であり、PG.2は前記第2領域のガラスに対する剥離力である。
DPI=100×(PI.1-PI.2)/PI.2
数式9でDPIは剥離力の差であり、PI.1は前記第1領域のポリイミドフィルムに対する剥離力であり、PI.2は前記第2領域のポリイミドフィルムに対する剥離力である。
貯蔵弾性率はARES G2(Advanced Rheometric Expansion System G2)(TA社)を使って評価した。厚さが約0.8mm程度である粘着剤層を直径が約8mm程度である円形に裁断して試片を製造した。前記粘着剤層は厚さが約25μm程度である粘着剤層を前記0.8mm程度の厚さとなるように重ねて製造した。直径が約8mmであるパラレルプレートフィクスチャ(parallel plate fixture)を使って前記試片に対して測定温度での貯蔵弾性率を評価した。前記評価時に評価条件は周波数1Hzおよびストレイン(strain)5%にした。
クリープ変形率(Creep)および回復率は次の方式で評価した。厚さが約0.8mm程度である粘着剤層を直径が約8mm程度である円形に裁断して試片を製造した。前記粘着剤層は厚さが約25μm程度である粘着剤層を前記0.8mm程度の厚さとなるように重ねて製造した。
変形量(単位:%)=100×(La-Li)/Li
数式AでLaは粘着剤層の変形方向(ストレスが加えられた方向)への変形後の長さ(単位:mm)であり、Liは粘着剤層の変形前の初期厚さ(単位:mm)である。
R%=100×(C-S)/C
数式BでR%は前記回復率であり、Cは前記クリープ変形率値(Creep、最大変形率)であり、Sは、前記約10,000Paのストレスを600秒の間試片に加えた後にストレスを除去し、再び600秒が経過した時点での試片の変形率(例えば、図9の20)である。
測定対象である粘着フィルム(離型フィルム/粘着剤層/基材フィルムの構造)を幅が約25mm程度であり、長さが約100mm程度である長方形に裁断して試片を製造した。引き続き離型フィルムを剥離し、粘着剤層をソーダライムガラス(soda lime glass)またはポリイミドフィルムにJIS Z 0237の規定により2kgのローラを使って付着し、常温で1日放置した。その後、TA(Texture Analyzer)装備(Stable Micro System社)を使って常温で180度の剥離角度および0.3m/minの剥離速度で粘着剤層を剥離して剥離力を測定した。
共重合体の融点およびガラス転移温度は、通常のDSC(Differential Scanning Calorimeter)装備を使った測定方法により測定した。装備としてはDSC-STAR3装備(Mettler Toledo社)を使った。試料(共重合体)約10mgを専用パン(pan)に密封し、昇温条件を10℃/minにして吸熱および発熱量を温度に応じて確認して融点などを測定した。
共重合体の重量平均分子量(Mw)は、GPC(Gel Permeation Chromatograph)を使って測定し、測定条件は下記の通りである。重量平均分子量測定時に検量線の製作には標準ポリスチレン(Aglient system(製))を使って測定結果を換算した。
測定機:Aglient GPC(Aglient 1200 series、U.S.)
コラム:PL Mixed B 2個連結
コラム温度:40℃
溶離液:THF(Tetrahydrofuran)
流速:1.0μL/min
濃度:~1mg/mL(100μl injection)
ダイナミックフォールディングテストは、図10に示されたような試片を製造して遂行した。図10に示された試片のように、両面にハードコーティング層100が形成された厚さ約50μm程度であるポリイミドフィルム200、粘着剤層300、偏光板400、粘着剤層300およびディスプレイパネル500を順次積層して製造された積層体を、横の長さが約7.8cmであり、縦の長さが約17cm程度である長方形の形態に裁断して試片を製造した。引き続き図11に示された通り、前記試片を5mm間隔の平行板の間に挟んで折り畳むフォールディングを25℃で20万回繰り返し、サンプルを回収した後にサンプルでの気泡の発生、浮き/剥離の発生およびハードコーティング層のクラックの発生などの不良を肉眼で観察した。前記不良のうち一つでも発生した場合をNGとして評価し、前記不良がすべて発生していない場合をPASSとして評価した。
2-エチルヘキシルアクリレート(2-EHA)、ラウリルアクリレート(LA)、4-ヒドロキシブチルアクリレート(HBA)および4-ベンゾイルフェニルメタクリレート(BPMA)を50:40:10:0.05の重量比率(2-EHA:LA:HBA:BPMA)で反応器内の溶媒であるエチルアセテートに投入し、ラジカル開始剤(2,2´-Azobis(4-methoxy-2,4-dimethylvaleronitrile))を約500ppm追加した後に約50℃で約8時間の間重合反応させて重合物(共重合体(A))を製造した。
製造例1の共重合体(重合物)(A)100重量部対比約0.3重量部のイソシアネート架橋剤(xylylene diisocyanate)を配合して粘着剤組成物を製造した。前記製造された粘着剤組成物を基材フィルム(PET(poly(ethylene terephthalate))のフィルム上にコンマコーター(comma coater)で塗布し、130℃で約3分程度維持して厚さが約25μm程度である粘着剤層を形成した。
製造例1の共重合体(重合物)(A)の代わりに製造例2の共重合体(重合物)(B)を使ったことを除いては実施形態1と同一にして粘着剤層を形成した。
製造例1の共重合体(重合物)(A)の代わりに製造例3の共重合体(重合物)(C)を使ったことを除いては実施形態1と同一にして粘着剤層を形成した。
製造例1の共重合体(重合物)(A)の代わりに製造例4の共重合体(重合物)(D)を使ったことを除いては実施形態1と同一にして粘着剤層を形成した。
製造例1の共重合体(重合物)(A)の代わりに製造例5の共重合体(重合物)(E)を使ったことを除いては実施形態1と同一にして粘着剤層を形成した。
実施形態および比較例の粘着剤層に対して紫外線を照射した場合、および照射していない場合におけるクリープ変形率および回復率をそれぞれ評価し、その結果を下記の表2および表3に記載した。
実施形態および比較例の粘着剤層に対して紫外線を照射した場合、および照射していない場合における貯蔵弾性率および剥離力をそれぞれ評価し、その結果を下記の表5および表6に記載した。前記で紫外線の照射は、試験例1の場合と同一に遂行した。下記で貯蔵弾性率の単位はPaである。
各実施形態の粘着剤層にマスクを媒介とした紫外線照射によって図2に示されたような第1領域1000および第2領域2000を形成し、前述した方式でダイナミックフォールディングテストを遂行した。ダイナミックフォールディングテストでフォールディング軸3000は第2領域2000の中心部と図2のように重複するようにした。その結果、実施形態の粘着剤層の場合はいずれも反復的なフォールディング後に不良が発生せず、フォールディング後にフォールディング跡も観察されなかった。
Claims (13)
- 第1領域および第2領域を含み、
前記第1領域および前記第2領域の下記の数式5による貯蔵弾性率の差の絶対値が10%以上であり、下記の数式8による剥離力の差の絶対値が40%以下である粘着剤層:
[数式5]
DM60=100×(M60.1-M60.2)/M60.2
[数式8]
DPG=100×(PG.1-PG.2)/PG.2
数式5および8でMC60は貯蔵弾性率の差であり、M60.1は前記第1領域の60℃での貯蔵弾性率であり、M60.2は前記第2領域の60℃での貯蔵弾性率であり、DPGは剥離力の差であり、PG.1は前記第1領域のガラスに対する剥離力であり、PG.2は前記第2領域のガラスに対する剥離力である。 - 前記第2領域の60℃での貯蔵弾性率が50,000Pa以下である、請求項1に記載の粘着剤層。
- 前記第1領域および前記第2領域の下記の数式6による貯蔵弾性率の差の絶対値は3%以上である、請求項1または2に記載の粘着剤層:
[数式6]
DM30=100×(M30.1-M30.2)/M30.2
数式6でDM30は貯蔵弾性率の差であり、M30.1は前記第1領域の30℃での貯蔵弾性率であり、M30.2は前記第2領域の30℃での貯蔵弾性率である。 - 前記第2領域の30℃での貯蔵弾性率が50,000Pa以下である、請求項3に記載の粘着剤層。
- 前記第1領域および前記第2領域の下記の数式7による貯蔵弾性率の差の絶対値は1%以上である、請求項1から4のいずれか一項に記載の粘着剤層:
[数式7]
DM20=100×(M20.1-M20.2)/M20.2
数式7でDM20は貯蔵弾性率の差であり、M20.1は前記第1領域の-20℃での貯蔵弾性率であり、M20.2は前記第2領域の-20℃での貯蔵弾性率である。 - 前記第2領域の-20℃での貯蔵弾性率が500,000Pa以下である、請求項5に記載の粘着剤層。
- 前記第1領域のガラスに対する常温剥離力が500gf/inch以上である、請求項1から6のいずれか一項に記載の粘着剤層。
- 前記第1領域および前記第2領域の下記の数式9による剥離力の差の絶対値が50%以下である、請求項1から7のいずれか一項に記載の粘着剤層:
[数式9]
DPI=100×(PI.1-PI.2)/PI.2
数式9でDPIは剥離力の差であり、PI.1は前記第1領域のポリイミドフィルムに対する剥離力であり、PI.2は前記第2領域のポリイミドフィルムに対する剥離力である。 - 前記第1領域のポリイミドフィルムに対する常温剥離力が500gf/inch以上である、請求項8に記載の粘着剤層。
- 結晶性アクリル共重合体を含む、請求項1から9のいずれか一項に記載の粘着剤層。
- 融点が-20℃以下であるアクリル共重合体を含む、請求項1から9のいずれか一項に記載の粘着剤層。
- 基材フィルム;および前記基材フィルムの一面または両面に形成された請求項1から11のいずれか一項に記載の粘着剤層を含む、粘着フィルム。
- 光学フィルム;および前記光学フィルムの一面または両面に形成された請求項1から11のいずれか一項に記載の粘着剤層を含む光学積層体。
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