JP6782695B2 - 誘導自己集合体施与のためのケイ素含有ブロックコポリマー - Google Patents
誘導自己集合体施与のためのケイ素含有ブロックコポリマー Download PDFInfo
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- C08F299/00—Macromolecular compounds obtained by interreacting polymers involving only carbon-to-carbon unsaturated bond reactions, in the absence of non-macromolecular monomers
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Description
i)ブロックコポリマー組成物を基材上にコーティングしフィルムを形成するステップ;
ii)ブロックコポリマーフィルムにフローベーク(flow bake)を施用して溶剤を除去し及び任意選択に、基材中に任意のトポグラフィを共形的にコーティングするステップ;
iii)アニールベークを施用して、ブロックコポリマーの自己集合に影響を及ぼすステップ;及び
iv)自己集合したポリマー構造を現像してパターンアレイを形成するステップ、
を含む。
20.14gのPS−b−PtBMA(PSブロックのMnは29290g/モル(GPC)、PtBMAのMnはNMRで見積もって6000g/モル、PDIは1.04であった)を、磁気攪拌棒及び冷水凝縮器を備えた500mlのフラスコ中で320gの1,4−ジオキサン中に溶解した。この溶液に、ジオキサン中の4M HCl60ml及び脱イオン(DI)水15gを加えた。このフラスコを90℃の油浴中に浸漬し、そしてフーリエ変換赤外(FTIR)スペクトルが1366cm−1でtert−ブチル基CHピークを示さなくなるまでこの温度で加水分解を行った。反応溶液を室温まで放冷し、そして攪拌しながらDI水中にゆっくりと注ぎ入れた。生じた白色のポリマーを濾過して単離し、そしてDI水及びメタノールで徹底的に洗浄した。最後に、重量が一定になるまでポリマーを真空中で乾燥して17gのPS−b−PMAAを得た。
上記で調製した12gのPS−b−PMAAを、磁石棒を含む250mlフラスコ中で、110gの1,4−ジオキサン及び36gのTHF中に溶解した。この溶液に、30gのメタノール中に溶解した6gのテトラメチルアンモニウム5水和物を加えた。混合物を7時間室温で攪拌した後、13gのヨウ化アリルを加えた。この反応混合物を2日間室温で攪拌した。生じたヨウ化テトラメチルアンモニウムを濾別した。この濾液を攪拌しながらメタノール中に注ぎ入れた。生じたポリマーを濾過して単離し、そしてメタノールで徹底的に洗浄した。真空中で乾燥した後、11.2gのPS−b−PAMAが得られた。このポリマーは、34484g/モルのMw、33091g/モルのMn及び1.04のPDIを有していた。
上述のように調製した2.3gのPS−b−PAMAをトルエン中に溶解して、10重量%の溶液を調製した。トルエン中5重量%のドデカンチオール3.25g及びトリス(トリメチルシリル)シラン11.6gを加えた。氷浴中で混合物を0℃に冷却した後に、ヘキサン中1Mのトリエチルボラン3.2gを、2時間かけて少しづつ加えた。添加後、氷浴を取り除き、反応混合物を室温で一晩攪拌した。この混合物を攪拌しながらメタノール中に注ぎ入れた。生じたポリマーを濾過して単離しそしてメタノールで徹底的に洗浄した。このポリマーをTHF中に溶解し、そしてDI水中に析出することによって精製した。最後に、ポリマーを、重量が一定となるまで、50℃の減圧炉中で乾燥した。2.5gのSiBCPが得られた。このポリマーは、38032g/モルのMw、36280g/モルのMn及び1.04のPDIを有していた。
上述のように製造したSiBCPをPGMEA中に溶解して、1.3重量%の溶液を調製した。この溶液を、0.2μmPTFEマイクロフィルタに通して濾過した。この溶液を、2200のrpmで30秒間、6インチケイ素ウェハ上にスピンキャストして28nmの薄いフィルムを得、そしてSiBCPフィルムを5分間、空気中で130℃でアニールした。このフィルムを、15秒間のCF3プラズマエッチングに付して上面Si湿潤層を除去し、次いで20秒間のO2プラズマでエッチングしてPSを除去した(エッチャー: MARCHエッチャー、Nordson Corp.)。自己集合ラインパターンを、NanoSEMで観察したところ、SiBCPが熱的にアニール可能であり、ラインパターンについては基材に対して並行なBCPシリンダ状フィンガープリント構造を形成したことを示した。というのも、基材に対して垂直なBCPシリンダ状構造はランダムホールのパターンを生成したであろうからである。
Claims (16)
- R1が水素であり、R2が水素またはC1〜C4アルキルであり、R3がC1〜C4アルキルまたはC1〜C4フルオロアルキルであり、R4、R5、R6、R7、R8、R9、R10、R11、及びR12がそれぞれメチルであり、そしてnが2〜6である、請求項1に記載の組成物。
- R1が水素であり、R2が水素であり、R3がC1〜C4アルキルであり、そしてR4、R5、R6、R7、R8、R9、R10、R11及びR12がそれぞれメチルであり、そしてnは2〜6である、請求項1または2に記載の組成物。
- R1が水素であり、R2が水素であり、R3がメチルであり、そしてR4、R5、R6、R7、R8、R9、R10、R11及びR12がそれぞれメチルであり、そしてnが3である、請求項1〜3のいずれか一つに記載の組成物。
- ブロックコポリマーが、1.2〜0.8の範囲の、繰り返し単位(2)に対する繰り返し単位(1)のモル比を有する、請求項1〜4のいずれか一つに記載の組成物。
- ブロックコポリマーが、5.3〜8.0の範囲の、繰り返し単位(2)に対する繰り返し単位(1)のモル比を有する、請求項1〜4のいずれか一つに記載の組成物。
- ブロックコポリマーが、7.3〜6.0の範囲の、繰り返し単位(2)に対する繰り返し単位(1)のモル比を有する、請求項1〜4のいずれか一つに記載の組成物。
- 溶剤中でのブロックコポリマーの濃度が全組成物の0.5〜5重量%である、請求項1〜7のいずれか一つに記載の組成物。
- 溶剤が、1,2−プロパンジオールC1〜C4アルキルエーテルC1〜C4アルキルカルボキシレート、C1〜C4アルキルC1〜C4アルキルカルボキシレート及びこれらの混合物から選ばれる群から選択される、請求項1〜8のいずれか一つに記載の組成物。
- 5.3〜8.0の範囲の、繰り返し単位(2)に対する繰り返し単位(1)のモル比を有する、請求項10に記載のブロックコポリマー。
- 7.3〜6.0の範囲の、繰り返し単位(2)に対する繰り返し単位(1)のモル比を有する、請求項10または11に記載のブロックコポリマー。
- 1.2〜0.8の、繰り返し単位(2)に対する繰り返し単位(1)のモル比を有する、請求項10に記載のブロックコポリマー。
- R1が水素であり、R2が水素またはC1〜C4アルキルであり、R3がC1〜C4アルキルまたはC1〜C4フルオロアルキルであり、そしてR4、R5、R6、R7、R8、R9、R10、R11及びR12がそれぞれメチルであり、そしてnが2〜6である、請求項10〜13のいずれか一つに記載のブロックコポリマー。
- R1が水素であり、R2が水素またはC1〜C4アルキルであり、R3がC1〜C4アルキルまたはC1〜C4フルオロアルキルであり、R4、R5、R6、R7、R8、R9、R10、R11、及びR12がそれぞれメチルであり、そしてnが3〜6である、請求項10〜14のいずれか一つに記載のブロックコポリマー。
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US14/527,939 US9505945B2 (en) | 2014-10-30 | 2014-10-30 | Silicon containing block copolymers for direct self-assembly application |
US14/527,939 | 2014-10-30 | ||
PCT/EP2015/074980 WO2016066684A1 (en) | 2014-10-30 | 2015-10-28 | Silicon containing block copolymers for direct self-assembly application |
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US9738765B2 (en) * | 2015-02-19 | 2017-08-22 | International Business Machines Corporation | Hybrid topographical and chemical pre-patterns for directed self-assembly of block copolymers |
CN109906237B (zh) * | 2016-11-30 | 2021-08-03 | 株式会社Lg化学 | 嵌段共聚物 |
KR102096272B1 (ko) * | 2016-11-30 | 2020-04-02 | 주식회사 엘지화학 | 블록 공중합체 |
KR102267528B1 (ko) | 2016-12-21 | 2021-06-22 | 리지필드 액퀴지션 | 블록 공중합체의 자기-조립을 위한 신규한 조성물 및 방법 |
JP7076701B2 (ja) * | 2018-03-05 | 2022-05-30 | 東京応化工業株式会社 | ブロック共重合体及びその製造方法、ならびに相分離構造を含む構造体の製造方法 |
FR3089982A1 (fr) * | 2018-12-12 | 2020-06-19 | Arkema France | Procédé de fabrication d’un copolymère à blocs contenant du silicium |
KR20240008940A (ko) | 2021-05-18 | 2024-01-19 | 메르크 파텐트 게엠베하 | Ps-b-pmma형 블록 공중합체의 유도 자기 조립의 패턴화를 위한 개선된 건식 에칭 능력을 가진 소수성 가교성 피닝 하층 |
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WO1988009527A2 (en) * | 1987-05-21 | 1988-12-01 | Hughes Aircraft Company | Silicon-containing negative resist material, and process for its use in patterning substrates |
US5985524A (en) * | 1997-03-28 | 1999-11-16 | International Business Machines Incorporated | Process for using bilayer photoresist |
US6210856B1 (en) * | 1999-01-27 | 2001-04-03 | International Business Machines Corporation | Resist composition and process of forming a patterned resist layer on a substrate |
JP3963623B2 (ja) * | 1999-12-09 | 2007-08-22 | 富士フイルム株式会社 | ポジ型フォトレジスト組成物 |
JP3858968B2 (ja) * | 2000-01-06 | 2006-12-20 | 信越化学工業株式会社 | トリス(トリメチルシリル)シリルエチルエステルの製造方法 |
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JP2020033566A (ja) | 2020-03-05 |
WO2016066684A1 (en) | 2016-05-06 |
IL250995A0 (en) | 2017-04-30 |
TWI677526B (zh) | 2019-11-21 |
SG11201701937RA (en) | 2017-04-27 |
EP3212714B1 (en) | 2019-03-06 |
KR102226229B1 (ko) | 2021-03-10 |
JP6810782B2 (ja) | 2021-01-06 |
CN107075057B (zh) | 2019-02-15 |
JP2018502936A (ja) | 2018-02-01 |
TW201619278A (zh) | 2016-06-01 |
US9505945B2 (en) | 2016-11-29 |
US20160122579A1 (en) | 2016-05-05 |
EP3212714A1 (en) | 2017-09-06 |
CN107075057A (zh) | 2017-08-18 |
KR20170081206A (ko) | 2017-07-11 |
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