JP2020512693A - 表面処理方法およびそのための組成物 - Google Patents
表面処理方法およびそのための組成物 Download PDFInfo
- Publication number
- JP2020512693A JP2020512693A JP2019552589A JP2019552589A JP2020512693A JP 2020512693 A JP2020512693 A JP 2020512693A JP 2019552589 A JP2019552589 A JP 2019552589A JP 2019552589 A JP2019552589 A JP 2019552589A JP 2020512693 A JP2020512693 A JP 2020512693A
- Authority
- JP
- Japan
- Prior art keywords
- surface treatment
- composition
- treatment composition
- weight
- trimethylsilyl
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
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- 238000000034 method Methods 0.000 title claims abstract description 57
- 238000004381 surface treatment Methods 0.000 title claims description 76
- 239000004065 semiconductor Substances 0.000 claims abstract description 30
- 239000002335 surface treatment layer Substances 0.000 claims abstract description 20
- 238000004140 cleaning Methods 0.000 claims abstract description 17
- 239000000758 substrate Substances 0.000 claims description 40
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 38
- 239000012756 surface treatment agent Substances 0.000 claims description 31
- 239000000010 aprotic solvent Substances 0.000 claims description 30
- 150000001875 compounds Chemical class 0.000 claims description 26
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical group C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 claims description 17
- -1 glycol dialkyl ether Chemical class 0.000 claims description 15
- 239000010410 layer Substances 0.000 claims description 15
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- 239000003054 catalyst Substances 0.000 claims description 12
- 239000002904 solvent Substances 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 11
- 239000003960 organic solvent Substances 0.000 claims description 11
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 10
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 10
- 150000002596 lactones Chemical class 0.000 claims description 10
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 claims description 9
- YEJRWHAVMIAJKC-UHFFFAOYSA-N 4-Butyrolactone Chemical group O=C1CCCO1 YEJRWHAVMIAJKC-UHFFFAOYSA-N 0.000 claims description 8
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- 150000004945 aromatic hydrocarbons Chemical class 0.000 claims description 7
- ZSMNRKGGHXLZEC-UHFFFAOYSA-N n,n-bis(trimethylsilyl)methanamine Chemical compound C[Si](C)(C)N(C)[Si](C)(C)C ZSMNRKGGHXLZEC-UHFFFAOYSA-N 0.000 claims description 7
- 125000000026 trimethylsilyl group Chemical group [H]C([H])([H])[Si]([*])(C([H])([H])[H])C([H])([H])[H] 0.000 claims description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
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- 150000005215 alkyl ethers Chemical class 0.000 claims description 4
- QULMGWCCKILBTO-UHFFFAOYSA-N n-[dimethylamino(dimethyl)silyl]-n-methylmethanamine Chemical group CN(C)[Si](C)(C)N(C)C QULMGWCCKILBTO-UHFFFAOYSA-N 0.000 claims description 4
- FBADCSUQBLLAHW-UHFFFAOYSA-N 4-trimethylsilyloxypent-3-en-2-one Chemical compound CC(=O)C=C(C)O[Si](C)(C)C FBADCSUQBLLAHW-UHFFFAOYSA-N 0.000 claims description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- LGRFSURHDFAFJT-UHFFFAOYSA-N Phthalic anhydride Natural products C1=CC=C2C(=O)OC(=O)C2=C1 LGRFSURHDFAFJT-UHFFFAOYSA-N 0.000 claims description 3
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- POPACFLNWGUDSR-UHFFFAOYSA-N methoxy(trimethyl)silane Chemical compound CO[Si](C)(C)C POPACFLNWGUDSR-UHFFFAOYSA-N 0.000 claims description 3
- CWXWPIUMYLZIME-UHFFFAOYSA-N n-[dimethyl(2-phenylethyl)silyl]-n-methylmethanamine Chemical compound CN(C)[Si](C)(C)CCC1=CC=CC=C1 CWXWPIUMYLZIME-UHFFFAOYSA-N 0.000 claims description 3
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- 125000003354 benzotriazolyl group Chemical group N1N=NC2=C1C=CC=C2* 0.000 claims 2
- VMZOBROUFBEGAR-UHFFFAOYSA-N tris(trimethylsilyl) phosphite Chemical compound C[Si](C)(C)OP(O[Si](C)(C)C)O[Si](C)(C)C VMZOBROUFBEGAR-UHFFFAOYSA-N 0.000 claims 2
- 238000004519 manufacturing process Methods 0.000 abstract description 6
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- 150000004760 silicates Chemical class 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 150000003460 sulfonic acids Chemical class 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- MZLGASXMSKOWSE-UHFFFAOYSA-N tantalum nitride Chemical compound [Ta]#N MZLGASXMSKOWSE-UHFFFAOYSA-N 0.000 description 1
- 125000005207 tetraalkylammonium group Chemical group 0.000 description 1
- ZCWKIFAQRXNZCH-UHFFFAOYSA-M tetramethylazanium;perchlorate Chemical compound C[N+](C)(C)C.[O-]Cl(=O)(=O)=O ZCWKIFAQRXNZCH-UHFFFAOYSA-M 0.000 description 1
- 150000003536 tetrazoles Chemical class 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- QJMMCGKXBZVAEI-UHFFFAOYSA-N tris(trimethylsilyl) phosphate Chemical compound C[Si](C)(C)OP(=O)(O[Si](C)(C)C)O[Si](C)(C)C QJMMCGKXBZVAEI-UHFFFAOYSA-N 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 238000009281 ultraviolet germicidal irradiation Methods 0.000 description 1
- AQLJVWUFPCUVLO-UHFFFAOYSA-N urea hydrogen peroxide Chemical compound OO.NC(N)=O AQLJVWUFPCUVLO-UHFFFAOYSA-N 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
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- H01L21/02225—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer
- H01L21/0226—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process
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- H01L21/02296—Forming insulating materials on a substrate characterised by the treatment performed before or after the formation of the layer
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- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
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Abstract
Description
本出願は2018年1月16日に出願された米国仮出願第62/617,688号および2017年3月24日に出願された米国仮出願第62/476,182号の優先権を主張し、これらの両方は、参照によりその全体が本明細書に組み込まれる。
いくつかの実施形態では、本開示が表面処理方法に関する。このような方法は例えば、基板(例えば、半導体基板)の表面(例えば、パターンを有する表面)を、少なくとも1種類(例えば、2種類、3種類、または4種類)の非プロトン性溶媒および少なくとも1種類(例えば、2種類、3種類、または4種類)の表面処理剤を含む表面処理組成物と接触させることによって実施することができる。表面処理剤は、Si含有化合物とすることができる。一般に、表面処理組成物は表面が少なくとも約50度の水接触角を有するように、表面上に表面処理層(例えば、疎水性単分子層)を形成する。
a)任意選択で、表面を水性洗浄剤と接触させる;
b)任意選択で、表面を第1のすすぎ溶液と接触させる;
c)表面処理組成物であって、表面処理組成物は少なくとも1種類の非プロトン性溶媒および少なくとも1種類の表面処理剤を含み、少なくとも1種類の表面処理剤はSi含有化合物を含み、表面処理組成物は表面が少なくとも約50度の水接触角を有するように、表面上に表面処理層を形成する;
d)任意選択で、表面を第2のすすぎ溶液と接触させる;
e)表面を乾燥させる
f)必要に応じて、表面処理層を除去して、清浄化されパターン化された表面を形成する。
そのような実施形態では、パターンが最大で約20nmの寸法を有するフィーチャを含むことができる。
表面処理溶液(すなわち、処方1〜101)は、成分を室温で混合することによって調製した。処方1〜101の組成を以下の表1に要約する。表1に列挙される全てのパーセンテージは別段の指示がない限り、重量パーセンテージである。
1.SiO 2またはSiN 試験片を台の上に置く。
2.標本が針のすぐ下にくるまで、垂直ノブを時計回りに回転させることによって、ステージを上方に上昇させる。
3.1滴の脱イオン水を分注し、試料表面に軽く接触させ、次いで、液滴が針先端から分離するまで試料を下降させる。
4.ステージ調整のための横方向ノブを使用して、視野を横切る液滴を中心に置く。
5.ステージをガイドレールに沿って移動させることにより、視野の低下に焦点を合わせ、鮮明な画像を得る。
6.「AutoFAST」ボタンをクリックして画像をフリーズし、計算する。左右の接触角の2種類の数字が表示される。
7.手動で計算するには、マウスを使用して液滴の周囲に5つのマーカーを配置する。
8.メインメニューからドロップレットアイコンを選択し、接触角を計算する。
9.これにより、画像上に曲線フィットおよび接線が生成される。画面の左隅には2種類の数字が表示される。これらは左右の接触角である。
10.3箇所の基質の部位で上記の手順を繰り返し、得られた接触角を平均し、平均結果を表1に報告する。
2 「CA」は、接触角(度)を指す
3 「HMDS」は、ヘキサメチルジシラザンを指す
4 「PGMEA」は、プロピレングリコールメチルエーテルアセテートを指す
5 「PGME」は、プロピレングリコールメチルエーテルを指す
6 「HMDSO」は、ヘキサメチルジシロキサンを指す
7 「HMDSA」は、ヘプタメチルジシラザンを指す
8 「TMSDMA」は、N−(トリメチルシリル)ジメチルアミンを指す
9 「BDADMS」は、ビス(ジメチルアミノ)ジメチルシランを指す
表面処理溶液(すなわち、製剤102〜115)は、成分を室温で混合することによって調製した。製剤102〜115の組成を以下の表2に要約する。表2に列挙される全てのパーセンテージは別段の指示がない限り、重量パーセンテージである。
Claims (52)
- 基板の表面に配置されたパターンを有する半導体基板を処理する方法であって、
少なくとも1種類の非プロトン性溶媒および少なくとも1種類の表面処理剤を含む表面処理組成物と前記基板とを接触させることを含み、前記少なくとも1種類の表面処理剤はSi含有化合物を含み、
表面処理組成物は、表面が少なくとも約50度の水接触角を有するように表面上に表面処理層を形成し、前記パターンは最大で約20nmの寸法を有するフィーチャを含む、方法。 - 前記表面が、SiO2、SiN、TiN、SiOC、SiON、Si、SiGe、Ge、またはWを含む、請求項1に記載の方法。
- 前記少なくとも1種類の非プロトン性溶媒が、カーボネート溶媒、ラクトン、ケトン、芳香族炭化水素、シロキサン、グリコールジアルキルエーテル、グリコールアルキルエーテルアセテート、エステル、尿素、ラクタム、ジメチルスルホキシド、およびN−メチルピロリドンからなる群から選択される、請求項1に記載の方法。
- 前記少なくとも1種類の非プロトン性溶媒が、カーボネート溶媒を含む、請求項1に記載の方法。
- 前記カーボネート溶媒がプロピレンカーボネートである請求項4に記載の方法。
- 前記少なくとも1種類の非プロトン性溶媒がラクトンを含む、請求項1に記載の方法。
- ラクトンがガンマ−ブチロラクトンである請求項6に記載の方法。
- 前記少なくとも1種類の非プロトン性溶媒が、表面処理組成物の約90重量%〜約99.9重量%である請求項1に記載の方法。
- 前記Si含有化合物がジシラザンである請求項1に記載の方法。
- 前記ジシラザンが、ヘキサメチルジシラザン、ヘプタメチルジシラザン、N−メチルヘキサメチルジシラザン、1,3−ジフェニルテトラメチルジシラザン、または1,1,3,3−テトラフェニル−1,3−ジメチルジシラザンである請求項9に記載の方法。
- 前記Si含有化合物がトリメチルシリル基を含む、請求項1に記載の方法。
- 前記Si含有化合物が、N−(トリメチルシリル)ジメチルアミン、N−(トリメチルシリル)ジエチルアミン、4−トリメチルシリルオキシ−3−ペンテン−2−one、ビス−トリメチルシリルサルフェート、メトキシトリメチルシラン、N−アリル−N、N−ビス(トリメチルシリル)アミン、N−(トリメチルシリル)ジエチルアミン、N、N−ビス−トリメチルシリル尿素、またはトリス−トリメチルシリルホスファイトである請求項11に記載の方法。
- 前記Si含有化合物がアミノシランである請求項1に記載の方法。
- 前記アミノシランが、ビス(ジメチルアミノ)ジメチルシランまたはフェネチルジメチル(ジメチルアミノ)シランである請求項13に記載の方法。
- 前記少なくとも1種類の表面処理剤が、前記表面処理組成物の約0.5重量%〜約10重量%である請求項1に記載の方法。
- 前記表面処理組成物が触媒をさらに含む、請求項1に記載の方法。
- 前記触媒が、ベンゾトリアゾール、無水フタル酸、無水酢酸、メタンスルホン酸、硫酸、またはトリフルオロメタンスルホン酸である請求項16に記載の方法。
- 前記触媒が、前記表面処理組成物の約0.1重量%〜約1重量%である請求項16に記載の方法。
- 前記表面処理組成物が水をさらに含み、水が前記表面処理組成物の多くとも約2重量%である請求項1に記載の方法。
- 前記表面処理組成物が実質的に水を含まない、請求項1に記載の方法。
- 前記表面処理組成物が、表面が少なくとも約65度の水接触角を有するように表面上に表面処理層を形成する、請求項1に記載の方法。
- 前記表面を表面処理組成物と接触させる前に、前記表面を少なくとも1種類の水性洗浄溶液と接触させることをさらに含む、請求項1に記載の方法。
- 前記少なくとも1種類の水性洗浄溶液が、水、アルコール、水酸化アンモニウム水溶液、塩酸水溶液、過酸化水素水溶液、有機溶媒、またはそれらの組み合わせを含む、請求項22に記載の方法。
- 前記表面を前記少なくとも1種類の水性洗浄溶液と接触させた後であって、前記表面を前記表面処理組成物と接触させる前に、前記表面を第1のリンス溶液と接触させることをさらに含む、請求項22に記載の方法。
- 前記表面を前記表面処理組成物と接触させた後に、前記表面を第2のリンス溶液と接触させることをさらに含む、請求項1に記載の方法。
- 前記表面を乾燥させることをさらに含む、請求項1に記載の方法。
- 前記表面処理層を除去することをさらに含む、請求項1に記載の方法。
- 少なくとも1種類の非プロトン性溶媒、および少なくとも1種類の表面処理剤を含む表面処理組成物であって、前記表面処理剤はトリメチルシリル基、アミノシリル基、またはSi−H結合を含まないジシラザン基を含むSi含有化合物であり、表面処理組成物が、表面が少なくとも約50度の水接触角を有するように表面上に表面処理層を形成する、表面処理組成物。
- 前記少なくとも1種類の非プロトン性溶媒が、カーボネート溶媒、ラクトン、ケトン、芳香族炭化水素、シロキサン、グリコールジアルキルエーテル、グリコールアルキルエーテルアセテート、エステル、尿素、ラクタム、ジメチルスルホキシド、およびN−メチルピロリドンからなる群から選択される、請求項28に記載の組成物。
- 前記少なくとも1種類の非プロトン性溶媒がカーボネート溶媒を含む、請求項29に記載の組成物。
- 前記カーボネート溶媒がプロピレンカーボネートである請求項30に記載の組成物。
- 前記少なくとも1種類の非プロトン性溶媒がラクトンを含む、請求項28に記載の組成物。
- ラクトンがガンマ−ブチロラクトンである請求項32に記載の組成物。
- 前記少なくとも1種類の非プロトン性溶媒が、前記表面処理組成物の約90重量%〜約99.9重量%である請求項28に記載の組成物。
- 前記Si含有化合物がジシラザンである請求項28に記載の組成物。
- 前記ジシラザンが、ヘキサメチルジシラザン、ヘプタメチルジシラザン、N−メチルヘキサメチルジシラザン、1,3−ジフェニルテトラメチルジシラザン、または1,1,3,3−テトラフェニル−1,3−ジメチルジシラザンである請求項35に記載の組成物。
- 前記Si含有化合物がトリメチルシリル基を含む、請求項28に記載の組成物。
- 前記Si含有化合物が、N−(トリメチルシリル)ジメチルアミン、N−(トリメチルシリル)ジエチルアミン、4−トリメチルシリルオキシ−3−ペンテン−2−one、ビス−トリメチルシリルスルフェート、メトキシトリメチルシラン、N−アリル−N、N−ビス(トリメチルシリル)アミン、N−(トリメチルシリル)ジエチルアミン、N、N−ビス−トリメチルシリル尿素、またはトリス−トリメチルシリルホスファイトである請求項37に記載の組成物。
- 前記Si含有化合物がアミノシランである請求項28に記載の組成物。
- アミノシランがビス−ジメチルアミノジメチルシランまたはフェネチルジメチル(ジメチルアミノ)シランである請求項39に記載の組成物。
- 前記少なくとも1種類の表面処理剤が、前記表面処理組成物の約0.5重量%〜約10重量%である請求項28に記載の組成物。
- 触媒をさらに含む、請求項28に記載の組成物。
- 前記触媒が、ベンゾトリアゾール、無水フタル酸、無水酢酸、メタンスルホン酸、硫酸、またはトリフルオロメタンスルホン酸である請求項42に記載の組成物。
- 前記触媒が、前記表面処理組成物の約0.1重量%〜約1重量%である請求項42に記載の組成物。
- 前記表面処理組成物が水をさらに含み、水が表面処理組成物の多くとも約2重量%である請求項28に記載の組成物。
- 前記表面処理組成物が実質的に水を含まない、請求項28に記載の組成物。
- 前記表面処理組成物が、表面が少なくとも約65度の水接触角を有するように表面上に表面処理層を形成する、請求項28に記載の組成物。
- ラクトン、ケトン、芳香族炭化水素、シロキサン、グリコールジアルキルエーテル、グリコールアルキルエーテルアセテート、エステル、尿素、ラクタム、ジメチルスルホキシド、およびN−メチルピロリドンからなる群から選択される約90重量%〜約99.5重量%の少なくとも1種類の非プロトン性溶媒、および約0.5重量%〜約10重量%の少なくとも1種類の表面処理剤を含み、前記表面処理剤は、トリメチルシリル基、アミノシリル基、またはSi−H結合を含まないジシラザン基、を含むSi含有化合物である表面処理組成物。
- 触媒または水をさらに含む、請求項48に記載の組成物。
- プロピレンカーボネート、ヘキサメチルジシラザン、および任意に少なくとも1種類の共溶媒からなる表面処理組成物。
- ヘキサメチルジシラザンが組成物の約0.5重量%〜約10重量%である請求項50に記載の組成物。
- 前記少なくとも1種類の共溶媒が、水、シロキサン、または芳香族炭化水素を含む、請求項50に記載の組成物。
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