TWI487756B - 高溫熱退火製程 - Google Patents
高溫熱退火製程 Download PDFInfo
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- TWI487756B TWI487756B TW102124867A TW102124867A TWI487756B TW I487756 B TWI487756 B TW I487756B TW 102124867 A TW102124867 A TW 102124867A TW 102124867 A TW102124867 A TW 102124867A TW I487756 B TWI487756 B TW I487756B
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- Prior art keywords
- poly
- styrene
- film
- substrate
- block
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- 238000000034 method Methods 0.000 title claims description 65
- 238000000137 annealing Methods 0.000 title claims description 19
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- 239000000203 mixture Substances 0.000 claims description 123
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- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims description 11
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- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 6
- RDOXTESZEPMUJZ-UHFFFAOYSA-N anisole Chemical compound COC1=CC=CC=C1 RDOXTESZEPMUJZ-UHFFFAOYSA-N 0.000 claims description 6
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Classifications
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- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
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- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
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- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
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- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
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- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
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- C23C18/125—Process of deposition of the inorganic material
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Description
本發明係關於自組裝嵌段共聚物之領域。特別地,本發明係有關沉積於基板表面上之聚(苯乙烯)-嵌-聚(矽氧烷)嵌段共聚物膜組成物的具體熱退火製程。
某些由兩種或更多種端至端結合之不同均聚物組成的嵌段共聚物係已知為自組裝為具有10奈米(nm)至50nm之典型維度的週期性微域。因為使用光學微影術於奈米規格維度(尤其是次45nm)進行圖案化之昂貴性及難度,使用此等微域以圖案化表面之可能性業經愈來愈受到關注。
惟,控制該等嵌段共聚物微域於基板上之橫向佈置為持續存在之挑戰。先前,此問題業經使用經微影預定義之形貌性及/或化學性圖案化該基板而解決。先前之研究業經表明,基板之化學性圖案化後係定向層狀形式之自組裝嵌段共聚物微域,獲得接近彼等化學預設圖案的週期性。其他研究業經顯示,藉由控制形貌性預設圖案之底部及側壁上之嵌段共聚物的表面潤濕特性,於形貌性預設圖案後可定向該層狀。該層狀係形成維度比基板預設圖
案小之線/空間圖案,將該形貌性預設圖案細分為更高頻次之線圖案;亦即,具有更小節距之線圖案。嵌段共聚物圖案化之一個限制為,於用於形貌性及/或化學性指導預設圖案之該預設圖案表面上到處形成該等圖案的傾向。
目前,縮小給定之基板上多種特徵(如,場效應電晶體之閘)之尺寸的能力係受限於用於曝光光阻劑之光的波長(亦即,193nm)。此等限制對於製造具有<50nm之臨界維度(CD)之特徵造成顯著困難。於自組裝製程中,使用傳統之嵌段共聚物於取向控制及長範圍有序存在難點。此外,此等嵌段共聚物往往對後續加工步驟提供不適當之抗蝕刻性。
聚(苯乙烯)與聚(二甲基矽氧烷)之二嵌段共聚物對於使用定向自組裝技術之奈米規格維度(尤其是次45nm)圖案化的應用提供支持。惟,該技藝中傳統智慧為,於此等操作中使用聚(苯乙烯)-嵌-聚(二甲基矽氧烷)嵌段共聚物不能有效地熱退火。據此,彼等該技藝中者業經研發了多種用於加工聚(苯乙烯)-嵌-聚(二甲基矽氧烷)嵌段共聚物的替代技術。
舉例而言,於美國專利第2011/0272381號中,Millward等人揭露了加工二嵌段共聚物膜如聚(苯乙烯)-嵌-聚(二甲基矽氧烷)之溶劑退火方法。
儘管如此,對於加工用於定向自組裝應用之聚(苯乙烯)-嵌-聚(矽氧烷)二嵌段共聚物組成物的替代方法仍有需求。
本發明係提供一種加工基板之方法,係包含:提供具有表面之基板;提供共聚物組成物,係包含:聚(苯乙烯)-嵌-聚(矽氧烷)嵌段共聚物成分,其中,該聚(苯乙烯)-嵌-聚(矽氧烷)嵌段共聚物成分之數量平均分子量為5至1,000公斤(kg)/莫耳(mol);以及,抗氧化劑;將該共聚物組成物之膜施用至該基板之表面;視需要地,烘烤該膜;藉由在氣氛下將該膜於275至350℃加熱1秒至4小時之時間而將該膜退火;以及,處理該經退火之膜,以自該經退火之膜移除聚(苯乙烯)並將該經退火之膜中的聚(矽氧烷)轉化為SiOx
。
本發明係提供一種加工基板之方法,係包含:提供具有表面之基板;提供共聚物組成物,係包含:聚(苯乙烯)-嵌-聚(矽氧烷)嵌段共聚物成分,其中,該聚(苯乙烯)-嵌-聚(矽氧烷)嵌段共聚物成分之數量平均分子量為5至1,000kg/莫耳;以及,抗氧化劑,其中,該抗氧化劑係選自下列所組成之群組:含有至少一個2,6-二-第三丁基苯酚部分(moiety)之抗氧化劑;含有至少一個根據下式之部分的抗氧化劑:
含有至少一個根據下式之部分的抗氧化劑:
含有至少一個根據下式之部分的抗氧化劑:;以及,
其混合物;將該共聚物組成物之膜施用至該基板之表面;視需要地,烘烤該膜;藉由在氣氛下,將該膜於275至350℃加熱1秒至4小時之時間而將該膜退火;以及處理該經退火之膜,以自該經退火之膜移除聚(苯乙烯),並將該經退火之膜中的聚(矽氧烷)轉化為SiOx
。
本發明係提供一種加工基板之方法,係包含:提供具有表面之基板;提供共聚物組成物,係包含:聚(苯乙烯)-嵌-聚(矽氧烷)嵌段共聚物成分,其中,該聚(苯乙烯)-嵌-聚(矽氧烷)嵌段共聚物成分之數量平均分子量為5至1,000kg/mol;以及抗氧化劑,其中,該抗氧化劑係選自下列所組成之群組: ;;及其
混合物;將該共聚物組成物之膜施用至該基板之表面;視需要地,烘烤該膜;藉由在氣氛下將該膜於275至350℃加熱1秒至4小時之時間而將該膜退火;以及處理該經退火之膜,以自該經退火之膜移除聚(苯乙烯),並將該經退火之膜中的聚(矽氧烷)轉化為SiOx
。
本發明係提供根據本發明之方法加工的基板。
本發明係提供業經根據本發明之方法加工的基板,其中,該基板之表面係包含次微影性SiOx
特徵。
第1圖係根據比較例F1製備之產物膜之自上而下之掃描式電子顯微(SEM)影像的示意圖。
第2圖係根據實施例7製備之產物膜之自上而下之掃描式電子顯微(SEM)影像的示意圖。
第3圖係根據實施例8製備之產物膜之自上而下之掃描式電子顯微(SEM)影像的示意圖。
本發明係提供一種於構建需要顯微蝕刻或微圖案化表面之裝置(如,微電子、微感測器及生物晶片)的構建中,形成在後續之圖案轉移加工中可用於微影術之線和空間特徵的方法。本發明之方法係提供,創製具有可被相對於使用傳統微影手段創製於基板上之引導圖案之整數因數除盡之節距維度的圖案。形成此等具有較小維度如可使用傳統微影技術製造者之二分之一或四分之一,高解析圖案的能力,舉例而言,使得全新的半導體晶片之設計及製造技術成為可能。
本文及後附申請專利範圍中使用之術語「PSt-b-PSi嵌段共聚物」係聚(苯乙烯)-嵌段-聚(矽氧烷)二嵌段共聚物的縮寫。
本文及後附申請專利範圍中使用之關於本
發明之嵌段共聚物的術語「MN
」係根據在實施例中使用之方法測定之該嵌段共聚物成分之數量平均分子量(以公克(g)/莫耳(mol)計)。
本文及後附申請專利範圍中使用之關於在本發明之共聚物組成物使用之PSt-b-PSi摻合物的術語「MN-摻合物
」或「摻合物數量平均分子量」係該PSt-b-PSi摻合物中所包括之PSt-b-PSi嵌段共聚物之數量平均分子量的加權平均。
本文及後附申請專利範圍中使用之關於本發明之嵌段共聚物的術語「MW
」係根據在實施例中使用之方法測定之該嵌段共聚物成分之重量平均分子量(以g/mol計)。
本文及後附申請專利範圍中使用之關於在本發明之共聚物組成物使用之PSt-b-PSi摻合物的術語「MW-摻合物
」或「摻合物重量平均分子量」係該PSt-b-PSi摻合物中所包括之PSt-b-PSi嵌段共聚物之重量平均分子量的加權平均。
本文及後附申請專利範圍中使用之關於本發明之嵌段共聚物成分的術語「PD」係該嵌段共聚物成分之多分散性,根據下述等式計算之:
本文及後附申請專利範圍中使用之術語「平均分子量」,關於(a)作為單一PSt-b-PSi嵌段共聚物
之PSt-b-PSi嵌段共聚物成分,係意指該PSt-b-PSi嵌段共聚物之數量平均分子量(MN
);對於(b)作為兩種或更多種不同PSt-b-PSi嵌段共聚物之摻合物的不同PSt-b-PSi嵌段共聚物成分,係意指該摻合物中該兩種或更多種PSt-b-PSi嵌段共聚物之數量平均分子量(MN
)的加權平均。
本文及後附申請專利範圍中使用之關於PSt-b-PSi嵌段共聚物之術語「WfPSt
」係該嵌段共聚物成分中之該聚(苯乙烯)嵌段的重量百分比。
本文及後附申請專利範圍中使用之關於在本發明之共聚物組成物中使用之PSt-b-PSi摻合物的術語「WfPSt-摻合物
」或「摻合物聚(苯乙烯)重量分率」,係該PSt-b-PSi摻合物中包括之PSt-b-PSi嵌段共聚物中該聚(苯乙烯)嵌段的重量百分比之加權平均。
本文及後附申請專利範圍中使用之關於本發明之PSt-b-PSi嵌段共聚物的術語「WfPSi
」係該嵌段共聚物中該聚(矽氧烷)嵌段的重量百分比。
本文及後附申請專利範圍中使用之關於在本發明之共聚物組成物中使用之PSt-b-PSi摻合物的術語「WfPSi-摻合物
」或「摻合物聚(矽氧烷)重量分率」,係該PSt-b-PSi摻合物中包括之PSt-b-PSi嵌段共聚物中該聚(矽氧烷)嵌段的重量百分比之加權平均。
嵌段共聚物係自兩種或更多種相異之單體合成,且顯現兩種或更多種化學性相異但仍彼此共價鍵結之聚合性鏈片段的聚合物。二嵌段共聚物係自兩種相異之
單體(如,A與B)衍生之特定類別的嵌段共聚物,且其係具有包含共價鍵結至B殘基之聚合性嵌段之A殘基之聚合性嵌段的結構(如,AAAAA-BBBBB)。
於本發明之方法中使用之共聚物組成物係包含聚(苯乙烯)-嵌-聚(矽氧烷)嵌段共聚物成分;以及抗氧化劑;其中,該聚(苯乙烯)-嵌-聚(矽氧烷)嵌段共聚物成分係選自下列所組成之群組:(a)單一PSt-b-PSi嵌段共聚物;及(b)至少兩種相異之PSt-b-PSi嵌段共聚物的摻合物。
當於本發明之方法中使用之聚(苯乙烯)-嵌-聚(矽氧烷)嵌段共聚物成分為單一PSt-b-PSi嵌段共聚物時,所使用之PSt-b-PSi嵌段共聚物較佳係顯現5至1,000kg/mol(較佳為25至1,000kg/mol;更佳為30至1,000kg/mol;再更佳為30至100kg/mol;最佳為30至60kg/mol)的數量平均分子量(MN
);以及1至3(較佳為1至2;最佳為1至1.2)之多分散性(PD)。於本發明之方法中使用之聚(苯乙烯)-嵌-聚(矽氧烷)嵌段共聚物成分較佳係經選擇以顯現0.34至0.64(較佳為0.47至0.50)之聚(矽氧烷)重量分率(WfPSi
)。於本發明之方法中使用之聚(苯乙烯)-嵌-聚(矽氧烷)嵌段共聚物成分較佳係經選擇以顯現0.19至0.33(較佳為0.21至0.28;最佳為0.22至0.25)之聚(矽氧烷)重量分率(WfPSi
)。藉由本文所提供之教示,具有該技藝通常知識者將能夠使用本發明之方法沉積此包含單一PSt-b-PSi嵌段共聚物的共聚物組成物,其中,透過選擇及控制膜沉積條件,舉例而言:(a)該基板之表面能(亦即,以插置材質預
處理該基板之表面)、(b)所沉積之共聚物組成物膜的厚度、(c)所沉積之共聚物組成物的烘烤輪廓(亦即,烘烤溫度及烘烤時間)及(d)所沉積之共聚物組成物的退火輪廓(亦即,退火溫度及退火時間),在所沉積之共聚物組成物中的筒狀聚(矽氧烷)域將自組裝,以將其本身以其對稱軸平行於該基板之表面、垂直於該基板之表面、或前兩者之組合的方式定向。
當於本發明之方法中使用之聚(苯乙烯)-嵌-聚(矽氧烷)嵌段共聚物成分為至少兩種相異之PSt-b-PSi嵌段共聚物之摻合物時,該至少兩種相異之PSt-b-PSi嵌段共聚物較佳係選自具有1至1,000kg/mol(較佳為1至100kg/mol;最佳為5至60kg/mol)之數量平均分子量(MN
);以及,1至3(較佳為1至2;最佳為1至1.2)之多分散性(PD)的PSt-b-PSi嵌段共聚物。所使用之至少兩種相異之PSt-b-PSi嵌段共聚物之摻合物較佳係顯現5至1,000kg/mol(較佳為25至1,000kg/mol;更佳為30至1,000kg/mol;再更佳為30至100;最佳為30至60kg/mol)的摻合物數量平均分子量(MN-摻合物
)。所使用之至少兩種相異之PSt-b-PSi嵌段共聚物之摻合物較佳係顯現0.34至0.64(較佳為0.47至0.50)之摻合物聚(矽氧烷)重量分率(WfPSi-摻合物
)。所使用之至少兩種相異之PSt-b-PSi嵌段共聚物之摻合物較佳係顯示0.19至0.33(較佳為0.21至0.28;最佳為0.22至0.25)之摻合物聚(矽氧烷)重量分率(WfPSi-摻合物
)。較佳之聚(苯乙烯)-嵌-聚(矽氧烷)嵌段共聚物成分係包含至少兩種
相異之PSt-b-PSi嵌段共聚物的摻合物。當以當量分子量(亦即,MN-單一PSt-b-PSi
=MN-摻合物
)及當量聚(二甲基矽氧烷)重量分率(亦即,WfPSi-單一PSt-b-PSi
=WfPSi-摻合物
)為基準相比較時,包含PSt-b-PSi嵌段共聚物摻合物之共聚物組成物係提供較單一PSt-b-PSi嵌段共聚物組成物顯著之值,因為在用以於含矽基板上形成週期性奈米結構(如線/空間圖案)之對準自組裝應用中,該摻合物系統欲以顯現更快之退火輪廓及更低之缺陷(以當量分子量/PSi重量分率為基準而比較)。藉由本文所提供之教示,具有該技藝通常知識者將能夠使用本發明之方法沉積此包含PSt-b-PSi嵌段共聚物摻合物的共聚物組成物,其中,透過選擇及控制膜沉積條件,舉例而言:(a)該基板之表面能(亦即,以插置材質預處理該基板之表面)、(b)所沉積之共聚物組成物膜的厚度、(c)所沉積之共聚物組成物的烘烤輪廓(亦即,烘烤溫度及烘烤時間)及(d)所沉積之共聚物組成物的退火輪廓(亦即,退火溫度及退火時間),在所沉積之共聚物組成物中的筒狀聚(矽氧烷)域將自組裝,以將其本身以其對稱軸平行於該基板之表面、垂直於該基板之表面、或前兩者之組合的方式。
於本發明之方法中使用之聚(苯乙烯)-嵌-聚(矽氧烷)嵌段共聚物組成物較佳係具有聚(苯乙烯)嵌段,其中,該聚(苯乙烯)嵌段係包括來自苯乙烯、氘代苯乙烯、苯乙烯嵌段修飾單體及氘代苯乙烯嵌段修飾單體之至少一者的殘基。更佳地,其中,該聚(苯乙烯)嵌段係包括總計0至100wt%(較佳為0至15wt%;更佳為0.001至
15wt%)之苯乙烯嵌段修飾單體衍生單元及氘代苯乙烯嵌段修飾單體衍生單元。
該苯乙烯嵌段單體較佳係選自下列所組成之群組:羥基苯乙烯(如,4-羥基苯乙烯;3-羥基苯乙烯;2-羥基苯乙烯;2-甲基-4-羥基苯乙烯;2-第三丁基-4-羥基苯乙烯;3-甲基-4-羥基苯乙烯;2-氟-4-羥基苯乙烯;2-氯-4-羥基苯乙烯;3,4-二羥基苯乙烯;3,5-二羥基苯乙烯;3,4,5-三羥基苯乙烯;3,5-二甲基-4-羥基苯乙烯;3,5-第三丁基-4-羥基苯乙烯);矽氧基苯乙烯(如,4-三甲基矽氧基苯乙烯;及3,5-二甲基-4-三甲基矽氧基苯乙烯);以及4-乙醯氧基苯乙烯(如,3,5-二甲基-4-乙醯氧基苯乙烯;3,5-二溴-4-乙醯氧基苯乙烯;3,5-二氯-4-乙醯氧基苯乙烯);及其組合。該苯乙烯嵌段單體更佳係選自下列所組成之群組:4-羥基苯乙烯;3-羥基苯乙烯;2-羥基苯乙烯;2-甲基-4-羥基苯乙烯;2-第三丁基-4-羥基苯乙烯;3-甲基-4-羥基苯乙烯;2-氟-4-羥基苯乙烯;2-氯-4-羥基苯乙烯;3,4-二羥基苯乙烯;3,5-二羥基苯乙烯;3,4,5-三羥基苯乙烯;3,5-二甲基-4-羥基苯乙烯;3,5-第三丁基-4-羥基苯乙烯;及其組合。該苯乙烯嵌段修飾單體最佳係選自下列所組成之群組:4-羥基苯乙烯;3-羥基苯乙烯;2-羥基苯乙烯;及其組合。
該氘代苯乙烯嵌段單體較佳係選自下列所組成之群組:氘代羥基苯乙烯(如,氘代4-羥基苯乙烯;氘代3-羥基苯乙烯;氘代2-羥基苯乙烯;氘代2-甲基-4-羥基
苯乙烯;氘代2-第三丁基-4-羥基苯乙烯;氘代3-甲基-4-羥基苯乙烯;氘代2-氟-4-羥基苯乙烯;氘代2-氯-4-羥基苯乙烯;氘代3,4-二羥基苯乙烯;氘代3,5-二羥基苯乙烯;氘代3,4,5-三羥基苯乙烯;氘代3,5-二甲基-4-羥基苯乙烯;氘代3,5-第三丁基-4-羥基苯乙烯);氘代矽氧基苯乙烯(如,氘代4-三甲基矽氧基苯乙烯;及氘代3,5-二甲基-4-三甲基矽氧基苯乙烯);氘代4-乙醯氧基苯乙烯(如,氘代3,5-二甲基-4-乙醯氧基苯乙烯;氘代3,5-二溴-4-乙醯氧基苯乙烯;及氘代3,5-二氯-4-乙醯氧基苯乙烯);及其組合。該氘代苯乙烯嵌段單體更佳係選自下列所組成之群組:氘代4-羥基苯乙烯;氘代3-羥基苯乙烯;氘代2-羥基苯乙烯;氘代2-甲基-4-羥基苯乙烯;氘代2-第三丁基-4-羥基苯乙烯;氘代3-甲基-4-羥基苯乙烯;氘代2-氟-4-羥基苯乙烯;氘代2-氯-4-羥基苯乙烯;氘代3,4-二羥基苯乙烯;氘代3,5-二羥基苯乙烯;氘代3,4,5-三羥基苯乙烯;氘代3,5-二甲基-4-羥基苯乙烯;氘代3,5-第三丁基-4-羥基苯乙烯;及其組合。該氘代苯乙烯嵌段修飾單體最佳係選自下列所組成之群組:氘代4-羥基苯乙烯;氘代3-羥基苯乙烯;氘代2-羥基苯乙烯;及其組合。
於本發明之方法中使用之聚(苯乙烯)-嵌-聚(矽氧烷)嵌段共聚物組成物較佳係具有聚(矽氧烷)嵌段,其中,該聚(矽氧烷)嵌段係包括來自矽氧烷單體及氘代矽氧烷單體之至少一者的殘基。更佳地,其中,該聚(矽氧烷)嵌段係包括>75wt%(更佳為>90wt%;最佳為>95
wt%)之二甲基矽氧烷衍生單元。
該矽氧烷單體較佳係選自下列所組成之單體:芳基(芳基)矽氧烷(如,苯基(苯基)矽氧烷);芳基(烷基)矽氧烷(如,苯基(甲基)矽氧烷);烷基(烷基)矽氧烷(如,二甲基矽氧烷;甲基(乙基)矽氧烷);鹵化烷基(烷基)矽氧烷(如,三氟丙基(甲基)矽氧烷);烷基矽氧烷;及其組合。該矽氧烷單體更佳係選自下列所組成之群組:苯基(甲基)矽氧烷、二甲基矽氧烷、甲基(乙基)矽氧烷、三氟丙基(甲基)矽氧烷、及其組合。該矽氧烷單體最佳係二甲基矽氧烷。
該氘代矽氧烷單體較佳係選自下列所組成之群組:氘代芳基(芳基)矽氧烷(如,氘代苯基(苯基)矽氧烷);氘代芳基(烷基)矽氧烷(如,氘代苯基(甲基)矽氧烷);氘代烷基(烷基)矽氧烷(如,氘代二甲基矽氧烷;氘代甲基(乙基)矽氧烷);氘代鹵化烷基(烷基)矽氧烷(如,氘代三氟丙基(甲基)矽氧烷);氘代烷基矽氧烷;及其組合。該氘代矽氧烷單體更佳係選自下列所組成之群組:氘代苯基(甲基)矽氧烷、氘代二甲基矽氧烷、氘代甲基(乙基)矽氧烷、氘代三氟丙基(甲基)矽氧烷、及其組合。該氘代矽氧烷單體最佳係氘代二甲基矽氧烷。
於本發明之方法中使用之共聚物組成物係含有抗氧化劑。於本發明之方法中使用之共聚物組成物較佳係含有>2wt%(以該PSt-b-PSi嵌段共聚物成分之重量為基準計)抗氧化劑。於本發明之方法中使用之共聚物組成物更佳係含有>2至10wt%(以該PSt-b-PSi嵌段共聚物成分
之重量為基準計)抗氧化劑。於本發明之方法中使用之共聚物組成物最佳係含有5至10wt%(以該PSt-b-PSi嵌段共聚物成分之重量為基準計)抗氧化劑。
於本發明之方法中使用之共聚物組成物中所含有的抗氧化劑可係選自一級抗氧化劑及二級抗氧化劑。該抗氧化劑較佳係選自下列所組成之群組:含有至少一個(較佳為至少兩個;更佳為至少三個;最佳為三個至四個)2,6-二-第三丁基苯酚部分之抗氧化劑;含有至少一個(較佳為至少兩個;更佳為至少三個;最佳為三個至四個)根據下式之部分的抗氧化劑:
含有至少一個(較佳為至少兩個;最佳為兩個)根據下式之部分的抗氧化劑:
含有至少一個(較佳為至少兩個;最佳為兩個)根據下式之部分的抗氧化劑:;及其混合物。該抗氧化劑更佳係選自下列所組成之群組: ;;及其混合物。該抗氧化劑再更佳係選自下列所組成之群組:、以及與一種或多種其他抗氧化劑之混合物。該抗氧化劑最佳係
於本發明之方法中使用之共聚物組成物中含有的抗氧化劑(或抗氧化劑之混合物)較佳係具有358g/mol之平均分子量。於本發明之方法中使用之共聚物組成物中含有的抗氧化劑(或抗氧化劑之混合物)更佳係具有600g/mol之平均分子量。於本發明之方法中使用之共聚物組成物中使用的抗氧化劑(或抗氧化劑之混合物)最佳係具有1,000g/mol之平均分子量。
於本發明之方法中含有之共聚物組成物中使用的抗氧化劑(或抗氧化劑之混合物)較佳係在760mm Hg(101.3kPa)測量到具有>400℃之平均沸點。於本發明之方法中含有之共聚物組成物中使用的抗氧化劑(或抗氧化劑之混合物)更佳係在760mm Hg(101.3kPa)測量到具有>500℃之平均沸點。於本發明之方法中含有之共聚物組
成物中使用的抗氧化劑(或抗氧化劑之混合物)再更佳係在760mm Hg(101.3kPa)測量到具有>700℃之平均沸點。於本發明之方法中含有之共聚物組成物中使用的抗氧化劑(或抗氧化劑之混合物)又更佳係在760mm Hg(101.3kPa)測量到具有>800℃之平均沸點。於本發明之方法中含有之共聚物組成物中使用的抗氧化劑(或抗氧化劑之混合物)最佳係在760mm Hg(101.3kPa)測具有>1,000℃之平均沸點。
於本發明之方法中使用之共聚物組成物係視需要復包含溶劑。適合於在共聚物組成物中使用之溶劑係包括能將聚(苯乙烯)-嵌-聚(矽氧烷)嵌段共聚物成分分散為藉由動態光散射量測之流體動力學直徑低於50nm之顆粒或聚集體。所使用之溶劑較佳係選自丙二醇單甲醚醋酸酯(PGMEA)、丙酸乙氧基乙酯、苯甲醚、乳酸乙酯、2-庚酮、環己酮、醋酸戊酯、γ-丁內酯(GBL)、N-甲基吡咯烷酮(NMP)及甲苯。所使用之溶劑更佳係選自丙二醇單甲醚醋酸酯(PGMEA)及甲苯。所使用之溶劑最佳係甲苯。
於本發明之方法中使用之共聚物組成物係視需要復包含佐劑。佐劑係包括額外之聚合物(包括均聚物及隨機共聚物);界面活性劑;光酸產生劑;熱酸產生劑;粹滅劑;硬化劑;黏著促進劑;溶解速率修飾劑;光固化劑;光敏化劑;酸增幅劑;塑化劑;取向控製劑;及交聯劑。用於本發明之共聚物組成物中的較佳佐劑係包括界面活性劑。
所使用之基板係任何包括具有可塗覆本發明之方法中之該共聚物組成物之表面的基板。較佳之基板係包括分層基板。較佳之基板係包括含矽之基板(如,玻璃;二氧化矽;氮化矽;氮氧化矽;含矽之半導體基板如矽晶圓、矽晶圓碎片、絕緣基板上矽、藍寶石基板上矽、於基礎半導體基底上之矽磊晶層、矽-鍺基板);塑膠;金屬(如,銅、釕、金、鉑、鋁、鈦及合金);氮化鈦;及非含矽之半導體性基板(如,非含矽之晶圓碎片、非含矽之晶圓、鍺、砷化鎵及磷化銦)。最佳之基板係含矽之基板。
視需要地,於本發明之方法中,於施用該共聚物組成物之前,以插置材質預處理待塗覆該共聚物組成物之基板的表面。該預處理材質較佳係作為類似於插置於該基板之表面與該共聚物組成物之間的繫層(tying layer),以提升該聚(苯乙烯)-嵌-聚(矽氧烷)嵌段共聚物成分與該基板之間的黏著性。該插置材質較佳係形成選自成像層及取向控制層之層。
適用於本發明之方法中的成像層係包括,舉例而言,可被圖案化或選擇性活化之任何類型材質。此等材質係包括,舉例而言,聚合物刷及矽烷與矽氧烷化合物之自組裝單層。
適用於本發明之方法中的取向控制層係包括中性及非中性取向控制層。亦即,該取向控制層可形成介於該基板與共聚物組成物之間的介面,其係優先藉由該聚(苯乙烯)嵌段或該聚(矽氧烷)嵌段之一者潤濕,亦即,非
中性取向控制層。中性取向控制層係指形成介於基板與該共聚物組成物之間的介面,其係藉由該聚(苯乙烯)嵌段與該聚(矽氧烷)嵌段同等潤濕。
於本發明之方法中,較佳係於沉積該共聚物組成物之前,預處理該基板以促進該共聚物組成物中之該聚(苯乙烯)-嵌-聚(矽氧烷)嵌段共聚物成分的引導性自組裝。具體地,該預處理可促進一種或兩種用於嵌段共聚物膜之引導性自組裝的傳統方法,亦即,製圖磊晶(graphoepitaxy)及化學磊晶。於製圖磊晶中,該基板之表面係以該基板之表面上的形貌特徵(如,溝槽、孔)進行預圖案化,其係操作以導向將該共聚物組成物之該聚(苯乙烯)-嵌-聚(矽氧烷)嵌段共聚物成分中之該聚(苯乙烯)與該聚(矽氧烷)嵌段的自組織。
於化學磊晶中,該基板之表面係以顯現組成性圖案之膜處理之,其中,該組成性圖案之多個部分與該聚(苯乙烯)嵌段及該聚(矽氧烷)嵌段之間的親和性相異。該化學親和性差異係操作以促進該共聚物組成物之聚(苯乙烯)-嵌-聚(矽氧烷)嵌段共聚物成分的定向自組裝。
於本發明之方法中,該插置層較佳係使用選自旋塗、浸塗、輥塗、噴塗及層壓之方法(最佳係旋塗)而形成於該基板上。將該插置層形成材質施用至該基板之表面上之後,視需要進一步處理該材質以移除任何殘留之溶劑。較佳係於升高之溫度(如,70至340℃)將該插置層烘烤至少10秒至5分鐘,以自該插置層移除任何殘留之溶
劑。經烘烤之插置層較佳係使用能自該基板之表面移除任何未結合之插置層之殘質的溶劑沖洗,隨後,於升高之溫度(如,70至340℃)再次烘烤至少10秒至5分鐘以移除任何殘留之溶劑。
於本發明之方法中,將包含該聚(苯乙烯)-嵌-聚(矽氧烷)嵌段共聚物成分及抗氧化劑之共聚物組成物的膜施用至基板之表面較佳係包含,使用選自旋塗、浸塗、輥塗、噴塗及層壓之方法(最佳係旋塗)將該共聚物組成物沉積於該基板之表面上。將該共聚物組成物膜施用至該基板之後,視需要進一步處理該膜以移除任何殘留之溶劑。較佳係於升高之溫度(如,70至340℃)烘烤該膜至少10秒至5分鐘,以自所沉積之共聚物組成物移除任何殘留之溶劑。
於本發明之方法中,隨後,係藉由在275至350℃(更佳為300至350℃;最佳為320至350℃),於氣氛下,將所沉積之共聚物組成物膜加熱1秒至4小時(較佳為2秒至1小時;更佳為30秒至1小時;最佳為90秒至1小時)之時間,以使得該聚(苯乙烯)-嵌-聚(矽氧烷)嵌段共聚物成分能夠自組裝於該基板之表面上。所沉積之膜較佳係於選自空氣、氮氣及氬氣之氣氛下退火。所沉積之膜較佳係於具有氧濃度150ppm(更佳為10ppm;再更佳為7.5ppm;又更佳為6.5ppm;最佳為4ppm)之氣氛下退火。所沉積之膜更佳係於具有氧濃度150ppm(更佳為10ppm;再更佳為7.5ppm;又更佳為6.5ppm;最
佳為4ppm)之氮或氬氣氛下退火。所沉積之膜最佳係於具有氧濃度100ppm(較佳為7.5ppm;更佳為6.5ppm;最佳為4ppm)之氮或氬氣氛下退火。
於本發明之方法中,經退火之膜係經處理以移除該經退火之膜中的聚(苯乙烯)嵌段,且將該經退火之膜中的聚(矽氧烷)嵌段轉化為SiOx
,提供具有複數孔洞(如,垂直於該基板之表面的溝槽;或複數個其對稱軸垂直於該基板之表面的筒狀SiOx
柱)之產物膜。該處理係包含:將該膜暴露於使該膜中之聚(苯乙烯)嵌段相對於該膜中之聚(矽氧烷)嵌段顯現區別之反應性的條件,以促進自經退火之膜移除聚(苯乙烯)域且促進將該聚(矽氧烷)域轉化為SiOx
。該處理較佳係包含:視需要地,將經退火之膜暴露於含鹵素之電漿(如,CF4
),以移除在經退火之膜之表面上形成的任何潤濕層;之後,將該經退火之膜暴露於反應性電漿或反應性離子蝕刻大氣,以移除聚(苯乙烯)域並將聚(矽氧烷)域轉化為SiOx
。該處理最佳係包含:將經退火之膜暴露於含鹵素之電漿,以移除在該經退火之膜上形成之任何潤濕層;以及,隨後將該經退火之膜暴露於反應性電漿或反應性離子蝕刻大氣,其中,該大氣係包含由低壓離子化氧氧化性氣體(較佳係O2
)構成之電漿;其中,該經退火之膜中的聚(苯乙烯)域被移除,且該經退火之膜中的聚(矽氧烷)域被轉化為SiOx
。
本發明之某些態樣將於下述實施例中詳述之。
於本文之實施例中,下述材質係於使用之前穿行通過充填有活化A-2級氧化鋁的柱,亦即,四氫呋喃(99.9%純度,購自Aldrich)、苯乙烯(購自Aldrich)及環己烷(HPLC級,購自Fischer)。於本文之實施例中所使用之其他全部材質係可商購之材質且係直接使用。
於本文之實施例中所報導之膜厚度係使用NanoSpec/AFT 2100膜厚度量測工具量測之。該等膜之厚度係自穿行通過繞射光柵之白光的干擾而測定。使用名為「Polyimide on Silicon」之標準程式來分析成分波長(380至780nm),以測定該膜之厚度。該聚(苯乙烯)-嵌-聚(矽氧烷)嵌段共聚物組成物與刷層之厚度係作為一層聚合物層而一起量測。所報導之膜厚度係該嵌段共聚物組成物與該刷層之厚度的組合厚度。
於該等實施例中報導之數量平均分子量(MN
)及多分散性值係藉由凝膠滲透色層分析(GPC)於配備安捷倫(Agilent)1100系列折射率及MiniDAWN光散射偵檢器(Wyatt Technology Co.)之Agilent 1100系列LC系統上量測之。樣本係以約1mg/mL之濃度溶解於HPLC級四氫呋喃(THF)中,並通過0.20微米(μm)針筒過濾器過濾,再注射通過兩根PLGel 300x7.5mm Mixed C柱(5mm,Polymer Laboratories,Inc.)。維持1mL/min之流速及35℃之溫度。該等柱係經窄分子量PS標準品(EasiCal PS-2,Polymer Laboratories,Inc.)校準。
於該等實施例中述及之質子核磁共振(1
H
NMR)譜結果係於Varian INOVA 400MHz NMR光譜儀上測得。使用氘代四氫呋喃(THF)。使用10秒之延遲時間以確保用於定量積分之質子的完全放鬆(relaxation)。化學位移係報導相對於四甲基矽烷。
於氮氣氛下,將環己烷(1,500g)加入2公升玻璃反應器中。隨後,通過套管將苯乙烯(50.34g)加入該反應器中。隨後將該反應器之內容物加熱至40℃。隨後,將於環己烷中稀釋為0.32M濃度的第二丁基鋰(19.18g)通過套管快速加入該反應器中,造成該反應器之內容物變為黃色。將該反應器之內容物攪拌30分鐘。隨後,將該反應器之內容物冷卻至30℃。隨後,將環氧乙烷(0.73g)轉移至該反應器中。將該反應器之內容物攪拌15分鐘。隨後,將20mL之於甲醇中的HCl之1.4M溶液加入該反應物中。隨後,藉由以500mL聚合物溶液與1,250mL異丙醇的比在異丙醇中沉澱,而分離該反應器中之聚合物。隨後,過濾所得沉澱並於60℃之真空烘箱中乾燥過夜,獲得42g之羥基封端之聚(苯乙烯)刷產物。該羥基封端之聚(苯乙烯)刷產物係顯現數量平均分子量(MN)為7.4kg/mol,且多分散性(PD)為1.07。
於氬氣氛下,將環己烷(90mL)及苯乙烯(17.1g)加入500mL圓底反應器中。隨後,通過套管將0.7
mL劑於環己烷中之第二丁基鋰之1.4M溶液快速加入該反應器中,造成該反應器之內容物變為橙黃色。令該反應器之內容物攪拌30分鐘。隨後,將小部分該反應器之內容物自該反應器抽入含有無水甲醇之小圓底燒瓶中,進行所形成之聚(苯乙烯)嵌段的凝膠滲透色層分析。之後,將2,2,5,5-四甲基二矽呋喃(472mg)加入該反應器中。橙色開始緩慢變淡,且於1小時之後,該反應器之內容物係淡黃色。隨後,將10.5g之新鮮昇華之六甲基環三矽氧烷轉移至該反應器中。令該反應器內容物反應1.5小時,直至該反應器之內容物無色。隨後,將乾燥四氫呋喃(90mL)加入該反應器中,令該反應再進行3.25小時。隨後,將氯三甲基矽烷(1mL)加入該反應器中以粹滅反應。藉由在500mL甲醇中沉澱並過濾,而分離產物。以額外之甲醇洗滌之後,將該聚合物再次溶解於150mL二氯甲烷中,以去離子水洗滌三次,隨後,於500mL甲醇中沉澱。隨後,將該聚合物過濾,並於70℃真空烘箱中乾燥過夜,得到20.5g產物。該聚(苯乙烯)-嵌-聚(矽氧烷)嵌段共聚物產物係顯現數量平均分子量(MN
)為24kg/mol;多分散性(PD)為1.01以及28wt%聚(矽氧烷)含量(藉由1
H NMR確定)。
於比較例S1及實施例3至5之每一例中,藉由將根據實施例2製備之PSt-b-PSi嵌段共聚物溶解於丙二醇甲醚醋酸酯(可自陶氏化學公司(The Dow Chemical Company)購得之Dowanol®
PMA)中而製備固體濃度為1.6
wt%的基底旋塗溶液,用於膜沉積。將表1中標註之抗氧化劑加入該基底旋塗溶液中,以於最終旋塗溶液中給出所標註之濃度。
將根據實施例1製備之羥基封端之聚(苯乙烯)刷於甲苯之1.5wt%(固體)溶液,藉由以3,000rpm將該溶液於具有天然氧化層之矽基板的表面上旋塗1分鐘而修飾該表面。隨後,將該基板於設定為150℃之熱板上
放置1分鐘。隨後,將該基板於氮氣氛下於設定為250℃之熱板上放置20分鐘,以退火所沉積之刷層。隨後,藉由首先將該基板於甲苯中浸泡1分鐘再隨後以3,000rpm旋轉乾燥1分鐘而以甲苯沖洗該基板,以移除任何之未附著之聚合物。隨後,將該基板於設定為110℃之熱板上烘烤1分鐘。
使用0.2μm Whatman針筒過濾器,將根據比較例S1、實施例3及實施例4製備之每一旋塗溶液以手過濾。於比較例F1、實施例7至8中,經過濾之來自比較例S1及實施例3至4的旋塗溶液係分別以2,500rpm將該等旋塗溶液旋塗於個別之根據實施例6製備的聚(苯乙烯)刷基板上。隨後,將該等基板於設定為150℃之熱板上放置1分鐘。隨後,將該等基板於含有10ppm氧之氮氣下於設定為340℃之熱板上放置表2中標註之退火時間,以將所沉積之膜退火。
PDM表面潤濕層係在氣氛-膜介面處形成於每一經退火之膜上。隨後,使用PlasmaTherm 790i RIE處理,使用連續反應性離子蝕刻(RIE)步驟經退火之膜,以顯露所沉積之膜的嵌段共聚物形貌。首先,使用短CF4電漿(10毫托(mT),50瓦(W))RIE處理(電漿安定化後8秒)以擊穿該聚(二甲基矽氧烷)之表面潤濕層。隨後,採用O2電漿(6mT,90W)RIE處理(電漿安定化後25秒)以移除聚(苯乙烯),並將PDMS轉化為SiOx。
隨後,使用Zeiss/Leo Gemini 982掃描式電子顯微鏡檢查經電漿處理之膜。使用雙側碳膠帶將該等測試樣本安裝於SEM樣本臺上,並於分析前藉由鼓吹氮氣而清潔之。以50,000x放大收集每一測試樣本之影像。根據比較例F1及實施例7至8製備之產物膜的自上而下之SEM影像係分別顯示於第1圖至第3圖中。根據比較例F1及實施例7至8之每一例製備的產物膜係各自顯現具有27nm之節距L0
的指紋圖案。
Claims (11)
- 一種加工基板之方法,係包含:提供具有表面之基板;提供共聚物組成物,係包含:聚(苯乙烯)-嵌-聚(矽氧烷)嵌段共聚物成分,其中,該聚(苯乙烯)-嵌-聚(矽氧烷)嵌段共聚物成分之數量平均分子量為5至1,000公斤/莫耳(kg/mol);以及抗氧化劑;將該共聚物組成物之膜施用至該基板之該表面;藉由在氣氛下,將該膜於275至350℃加熱1秒至4小時之期間而將該膜退火;以及處理該經退火之膜,以自該經退火之膜移除該聚(苯乙烯)嵌段,並將該經退火之膜中的該聚(矽氧烷)嵌段轉化為SiOx 。
- 如申請專利範圍第1項所述之方法,復包含:於該施用膜步驟後且於該將膜退火步驟前,烘烤該膜。
- 如申請專利範圍第1或2項所述之方法,其中,該抗氧化劑係選自下列所組成之群組:含有至少一個2,6-二-第三丁基苯酚部分之抗氧化劑;含有至少一個根據下式之部分的抗氧化劑:
- 如申請專利範圍第1或2項所述之方法,其中,該抗氧化劑係選自下列所組成之群組:
- 如申請專利範圍第3項所述之方法,其中,所提供之該聚(苯乙烯)-嵌-聚(矽氧烷)嵌段共聚物成分係具有25至1,000公斤/莫耳之數量平均分子量(MN );1至3之多分散性(PD);以及0.19至0.33之聚(矽氧烷)重量分率(WfPSi )之單一之聚(苯乙烯)-嵌-聚(矽氧烷)二嵌段共聚物。
- 如申請專利範圍第5項所述之方法,其中,所提供之該共聚物組成物復包含溶劑,其中,該溶劑係選自下列所組成之群組:丙二醇單甲醚醋酸酯(PGMEA)、丙酸乙氧基乙酯、苯甲醚、乳酸乙酯、2-庚酮、環己酮、醋酸戊酯、γ-丁內酯(GBL)、N-甲基吡咯烷酮(NMP)及甲苯。
- 如申請專利範圍第3項所述之方法,其中,該聚(苯乙烯)-嵌-聚(矽氧烷)嵌段共聚物成分係至少兩種相異之聚(苯乙烯)-嵌-聚(矽氧烷)嵌段共聚物的摻合物;其中,該至少兩種相異之聚(苯乙烯)-嵌-聚(矽氧 烷)嵌段共聚物係選自具有1至1,000公斤/莫耳之數量平均分子量(MN )及1至3之多分散性(PD)的聚(苯乙烯)-嵌-聚(矽氧烷)嵌段共聚物之群組;以及其中,該摻合物係顯現25至1,000公斤/莫耳之摻合物數量平均分子量(MN-摻合物 )。
- 如申請專利範圍第7項所述之方法,其中,該摻合物係顯現0.19至0.33之摻合物聚(矽氧烷)重量分率(WfPSi-摻合物 )。
- 如申請專利範圍第8項所述之方法,其中,所提供之該共聚物組成物復包含溶劑,其中,該溶劑係選自下列所組成之群組:丙二醇單甲醚醋酸酯(PGMEA)、丙酸乙氧基乙酯、苯甲醚、乳酸乙酯、2-庚酮、環己酮、醋酸戊酯、γ-丁內酯(GBL)、N-甲基吡咯烷酮(NMP)及甲苯。
- 如申請專利範圍第1項所述之方法,其中,該氣氛係具有100ppm氧之氮氣氛。
- 一種基板,係由如申請專利範圍第1或2項所述之方法加工。
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