JP7502644B2 - 基板、選択的膜堆積方法、有機物の堆積膜及び有機物 - Google Patents
基板、選択的膜堆積方法、有機物の堆積膜及び有機物 Download PDFInfo
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- JP7502644B2 JP7502644B2 JP2020565156A JP2020565156A JP7502644B2 JP 7502644 B2 JP7502644 B2 JP 7502644B2 JP 2020565156 A JP2020565156 A JP 2020565156A JP 2020565156 A JP2020565156 A JP 2020565156A JP 7502644 B2 JP7502644 B2 JP 7502644B2
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D1/00—Processes for applying liquids or other fluent materials
- B05D1/60—Deposition of organic layers from vapour phase
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D1/00—Processes for applying liquids or other fluent materials
- B05D1/62—Plasma-deposition of organic layers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/04—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to gases
- B05D3/0493—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to gases using vacuum
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
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Description
上記第二表面領域よりも上記第一表面領域に、下記一般式(1)で表される有機物の膜を選択的に堆積させることを特徴とする選択的膜堆積方法である。
上記第二表面領域よりも上記第一表面領域に、前述の一般式(1)で表される有機物の膜を選択的に堆積させることを特徴とする。
本開示の実施形態に係る選択的膜堆積方法では、第二表面領域よりも第一表面領域における水の接触角が10°以上大きいことが好ましく、20°以上大きいことがより好ましく、30°以上大きいことがさらに好ましい。
これにより、水の接触角が大きい第一表面領域には、水の接触角が小さい第二表面領域に比べて、有機物の膜が選択的に堆積していると判断可能である。
また、金属が露出した第一表面領域を得る方法としては、金属膜の表面の酸化膜を、HF等を含む溶液を用いて削除し、金属表面を露出する方法が挙げられる。上記酸化膜を機械的に削除してもよい。
非金属無機材料を含む第二表面領域は、上記非金属無機材料以外の化合物が含まれていてもよく、非金属無機材料のみを含んでいてもよいが、非金属無機材料のみを含み、非金属無機材料のみが表面に露出していることが望ましい。
本開示の実施の形態に係る湿式法では、上記した有機物と溶媒とを含む溶液に基板を暴露するが、その一例として、有機物と溶媒とを含む溶液に、第一表面領域と第二表面領域とを有する基板を浸漬することにより、上記溶液を上記基板の表面と接触させ、有機物の膜を、基板の第一表面領域に選択的に堆積させる膜堆積工程が挙げられる。上記溶液に基板を暴露するとは、基板の表面を溶液と接触させることをいう。従って、溶液に基板を暴露する方法として、浸漬法以外に、基板に溶液を滴下した後に高速回転させるスピンコート法や、溶液を基板に噴霧するスプレーコート法を用いることもでき、基板を溶液と接触させることが可能な方法であれば、これらの方法に限定されない。
本開示の実施の形態に係る乾式法では、有機物の気体を含む雰囲気に前記基板を暴露するが、具体的には、チャンバ内に基板を載置し、有機物を含む気体をチャンバ内に導入することにより、有機物を含む気体を基板の表面と接触させ、有機物の膜を、基板の第一表面領域に選択的に堆積させる膜堆積工程を行う。
本開示の実施形態に係る基板は、金属及び金属酸化物のうちの少なくとも1種を含む第一表面領域と、非金属無機材料を含む第二表面領域とが両方とも露出した構造を持つ基板であって、上記第一表面領域に下記一般式(1)で表される有機物の膜を有し、上記第二表面領域に上記有機物の膜を有しないか、上記第二表面領域上の上記有機物の膜の厚さt2が、上記第一表面領域上の上記有機物の膜の厚さt1よりも薄いことを特徴とする基板である。
イソプロピルアルコール(以下、IPAという)に1%のn-ドデシルアミンを溶解させ、有機物としてn-ドデシルアミンと溶媒とを含む溶液を調製した。
次に、この溶液にCu自然酸化膜を含有する基板を60秒浸漬させ、有機物の膜を堆積させた。溶液の温度は20~25℃であった。その後、20~25℃のIPAの液に60秒、2回浸漬させて、余分な有機物の除去を行い、続いて、20~25℃の窒素ガスを60秒間吹き付けて基板を乾燥させた。
基板上に形成された有機物の膜厚を原子間力顕微鏡(AFM)で測定したところ、3nmであった。また、X線光電子分光法(XPS)で元素組成を解析したところ、窒素の強いピークを確認した。
基板表面の金属酸化物の種類、有機物の種類、溶媒の種類、溶液濃度(有機物の濃度)などを、表1に示したように変更した以外は、実験例1-1と同様に実施し、評価を行った。その結果を表1に示す。
IPAに5%のn-ドデシルアミンを溶解させ、有機物としてn-ドデシルアミンと溶媒とを含む溶液を調製した。
次に、この溶液に非金属無機材料としてSi表面を含有する基板を60秒浸漬させ、有機物の膜を堆積させた。溶液の温度は20~25℃であった。その後、20~25℃のIPAの液に60秒、2回浸漬させて、余分な有機物の除去を行い、20~25℃の窒素ガスを60秒間吹き付けて基板を乾燥させた。
基板上に形成された有機物の膜厚をAFMで測定したところ、0nmであった。また、XPSで元素組成を解析したところ、窒素のピークは確認できなかった。
基板表面の非金属無機材料の種類、有機物の種類、溶媒の種類、溶液濃度(有機物の濃度)などを、表2に示したように変更した以外は、実験例2-1と同様に実施し、評価を行った。その結果を表2に示す。
Co自然酸化膜(Co酸化膜)含有基板は、シリコン基板上にコバルトの膜を蒸着により厚さ約100nmで成膜した後、大気中に暴露して得られた。
Si表面含有基板は、シリコン基板の自然酸化膜を除去して得られた。
SiO2表面含有基板は、シリコン基板上に二酸化シリコンの膜を化学的気相堆積法により厚さ約30nmで成膜して得られた。
SiN表面含有基板は、シリコン基板上にSi3N4の化学式で表される窒化シリコン膜を化学的気相堆積法により厚さ約30nmで成膜して得られた。
SiON表面含有基板は、シリコン基板上にSiN表面を形成させた後に酸化してSi4OxNy(xは3以上6以下、yは2以上4以下)の化学式で表される酸窒化シリコン膜を化学的気相堆積法により厚さ約10nmで成膜して得られた。
真空プロセスが可能なチャンバ内にCuO表面を含有する基板をセットし、チャンバ圧力を15Torr(2.0kPa 絶対圧)に設定した。次に、チャンバに接続したエチレンジアミンのシリンダーを保温する温度を20℃に設定してバルブを解放し、エチレンジアミンの気体をチャンバに供給し、CuO含有基板に気体のエチレンジアミンを接触させ、基板上に有機物の膜を堆積させた。なお、チャンバの温度は、シリンダーの温度と同じにし、エチレンジアミンの気体の温度は、基板に接触するまで、シリンダーを保温する温度と同じに保たれるようにした。有機物の膜の堆積後、チャンバ内を1Torr(0.13kPa)に減圧して余分な有機物を除去した。
基板上に形成された有機物の膜厚をAFMで測定したところ、8nmであった。また、XPSで元素組成を解析したところ、窒素の強いピークを確認した。
基板上の金属酸化物の種類、有機物の種類、シリンダーを保温する温度(有機物加熱温度)、チャンバ圧力(絶対圧力)などを表3に示したように変更した以外は、参考例3-1と同様に実施し、評価を行った。その結果を表3に示す。
真空プロセスが可能なチャンバ内に非金属無機材料としてSi表面を含有する基板をセットし、チャンバ圧力を15Torrに設定した。次に、チャンバに接続したエチレンジアミンのシリンダーを保温する温度を20℃に設定してバルブを解放し、Si表面含有基板に気体のエチレンジアミンを接触させた。有機物の膜の堆積後、チャンバ内を0.1Torrに減圧して余分な有機物を除去した。
基板上に形成された有機物の膜厚をAFMで測定したところ、0nmであった。また、XPSで元素組成を解析したところ、窒素のピークは確認できなかった。
基板上の非金属無機材料の種類、シリンダーを保温する温度(有機物加熱温度)、チャンバ圧力(絶対圧力)などを表4に示したように変更した以外は、参考例4-1と同様に実施し、評価を行った。その結果を表4に示す。
CoO表面含有基板は、蒸着によりシリコン基板上に酸化コバルトの膜を厚さ約100nmで成膜して得られた。
Si表面含有基板は、シリコン基板の自然酸化膜を除去して得られた。
SiO2表面含有基板は、化学的気相堆積法によりシリコン基板上に二酸化シリコンの膜を厚さ約30nmで成膜して得られた。
(溶液の調製)
溶媒としてイソプロピルアルコール(IPA)、有機物としてn-オクタデシルアミンを用い、該有機物の濃度が1質量%となるように混合溶解させ、有機物としてn-オクタデシルアミンと溶媒とを含む溶液を調製した。
膜厚100nmのコバルト膜を有するシリコン基板を30分間、UV/O3照射(ランプ:EUV200WS、ランプとの距離:10mm、UV照射により空気中の酸素からオゾンを発生させる)して表面を酸化し、表面に酸化コバルト(CoOx)を有する基板を得た。
上記基板を上記溶液に22℃で24時間浸漬させて、基板の表面処理を行い、基板の表面に有機物を堆積させた。その後、IPAに60秒、2回浸漬させて、窒素ガスを60秒間吹き付けて基板を乾燥させた。
(溶液の調製)
溶媒として表5に示す溶媒と有機物を用い、該有機物の濃度が表5に示した濃度となるように混合溶解させ、有機物と溶媒とを含む溶液を調製した。
(基板の準備)
実験例5-2~5-13では、実験例5-1と同様に表面に酸化コバルト(CoOx)を有する基板を準備した。
実験例5-14~5-26では、膜厚100nmのコバルト膜を有するシリコン基板を濃度0.5質量%のHF水溶液に22℃で1分間浸漬させて、表面の自然酸化膜を除去してコバルト膜(Co)を有する基板を得た。
実験例5-27では、膜厚100nmの銅膜を有するシリコン基板を30分間、UV/O3照射(ランプ:EUV200WS、ランプとの距離:10mm、UV照射により空気中の酸素からオゾンを発生させる)して表面を酸化し、表面に酸化銅(CuOx)を有する基板を得た。
実験例5-28では、膜厚100nmの銅膜を有するシリコン基板を濃度0.5質量%のHF水溶液に22℃で1分間浸漬させて、表面の自然酸化膜を除去して銅膜(Cu)を有する基板を得た。
上記処理により準備した基板を上記溶液に22℃で24時間浸漬させて、基板の表面処理を行い、基板の表面に有機物を堆積させた。その後、IPAに60秒、2回浸漬させて、窒素ガスを60秒間吹き付けて基板を乾燥させた。
有機物を含む溶液による表面処理を行った実験例5-1~5-28に係る基板表面上に純水約1μlを置き、22℃で水滴とウェハ表面とのなす角(接触角)を接触角計(協和界面科学株式会社製:DM-301)で測定した。その結果を表5に示す。
(溶液の調製)
溶媒として表6に示す溶媒と有機物を用い、該有機物の濃度が表6に示した濃度となるように混合溶解させ、有機物と溶媒とを含む溶液を調製した。
実験例6-1~6-8及び6-11~6-15では、膜厚100nmの酸化シリコン膜を有するシリコン基板を濃度0.5質量%のHF水溶液に22℃で1分間浸漬させて、表面を清浄し、表面が酸化シリコン(SiOx)の基板を得た。
実験例6-9では、膜厚30nmの窒化シリコン膜を有するシリコン基板を濃度0.5質量%のHF水溶液に22℃で1分間浸漬させて、表面の自然酸化膜を除去して表面が窒化シリコン(SiN)の基板を得た。
実験例6-10では、シリコン基板を濃度0.5質量%のHF水溶液に22℃で1分間浸漬させて、表面の自然酸化膜を除去して表面がシリコンの基板(Si基板)を得た。
上記の処理により得られた基板を上記溶液に22℃で24時間浸漬させて、基板の表面処理を行い、基板の表面に有機物を堆積させた。その後、IPAに60秒、2回浸漬させて、窒素ガスを60秒間吹き付けて基板を乾燥させた。
表面処理を施すことにより準備した実験例6-1~6-15に係る基板表面上に純水約1μlを置き、22℃で水滴とウェハ表面とのなす角(接触角)を接触角計(協和界面科学株式会社製:DM-301)で測定した。その結果を表6に示す。
(溶液の調製)
比較実験例1、3及び5では、表6に示すように、有機物を含まないIPA溶液を用いた。
比較実験例2、4及び6では、溶媒として表6に示すようにPGMEAを、有機物としてトリメチルシリルジメチルアミンを用い、該有機物の濃度が表6に示した濃度となるように混合溶解させ、有機物と溶媒とを含む溶液を調製した。なお、トリメチルシリルジメチルアミンは、本開示の有機物に該当しない。
比較実験例1~2では、実験例5-1と同様に表面に酸化コバルト(CoOx)を有する基板を準備し、比較実験例3~4では、実験例5-14と同様にしてコバルト膜(Co)を有する基板を準備し、比較実験例5~6では、実験例6-1と同様にして、表面が酸化シリコン(SiOx)の基板を準備した。
比較実験例1~6で準備した基板を上記溶液に22℃で24時間浸漬させて、基板の表面処理を行った。その後、IPAに60秒、2回浸漬させて、窒素ガスを60秒間吹き付けて基板を乾燥させた。
比較実験例1~6に係る基板表面上に純水約1μlを置き、22℃で水滴とウェハ表面とのなす角(接触角)を接触角計(協和界面科学株式会社製:DM-301)で測定した。その結果を表6に示す。
Claims (18)
- 金属及び金属酸化物のうちの少なくとも1種を含む第一表面領域と、非金属無機材料を含む第二表面領域とが両方とも露出した構造を持つ基板に対して、
前記第二表面領域よりも前記第一表面領域に、下記一般式(1)で表される有機物の膜を選択的に堆積させることを特徴とする選択的膜堆積方法。
- 第一表面領域上の有機物の膜の厚さt1と、第二表面領域上の有機物の膜の厚さt2との比(t1/t2)が5以上である、請求項1に記載の選択的膜堆積方法。
- 前記第二表面領域よりも前記第一表面領域に、前記一般式(1)で表される有機物の膜を選択的に堆積させる工程は、前記有機物の気体を含む雰囲気に前記基板を暴露する工程である、請求項1又は2に記載の選択的膜堆積方法。
- 前記有機物は、n-ブチルアミン、n-ペンチルアミン、n-ヘキシルアミン、n-ヘプチルアミン、n-オクチルアミン、シクロヘキシルアミン、アニリン及び2-アミノエタノールからなる群から選ばれた少なくとも一つである、請求項3に記載の選択的膜堆積方法。
- 前記有機物の気体を含む雰囲気の温度範囲は、0℃以上200℃以下である請求項3又は4に記載の選択的膜堆積方法。
- 前記有機物の気体を含む雰囲気の圧力範囲は、13Pa以上67kPa以下である請求項3~5のいずれか1項に記載の選択的膜堆積方法。
- 前記第二表面領域よりも前記第一表面領域に前記有機物の膜を選択的に堆積させる工程は、前記有機物と溶媒とを含む溶液に前記基板を暴露する工程である、請求項1又は2に記載の選択的膜堆積方法。
- 前記一般式(1)において、nが0であり、R2及びR3は、水素原子であり、R1は、炭素数1~30のヘテロ原子やハロゲン原子を有していてもよい直鎖状炭化水素基であることを特徴とする請求項7に記載の選択的膜堆積方法。
- 前記一般式(1)において、R1は、炭素数6~24のアルキル基であることを特徴とする請求項8に記載の選択的膜堆積方法。
- 前記有機物は、n-オクチルアミン、n-ノニルアミン、n-デシルアミン、n-ウンデシルアミン、n-ドデシルアミン、n-トリデシルアミン、n-テトラデシルアミン、n-ペンタデシルアミン、n-ヘキサデシルアミン、マルガリルアミン及びステアリルアミンからなる群から選ばれる少なくとも一つである請求項7~9のいずれか1項に記載の選択的膜堆積方法。
- 前記溶液に含まれる、前記一般式(1)で表される有機物の濃度が、前記有機物と前記溶媒の合計に対して0.01質量%以上20質量%以下である請求項7~10のいずれか1項に記載の選択的膜堆積方法。
- 前記溶液に使用する溶媒が、エステル類、エーテル類、ケトン類、アルコール系溶媒、及び多価アルコールの誘導体からなる群から選ばれる少なくとも一つを含む請求項7~11のいずれか1項に記載の選択的膜堆積方法。
- 前記溶液に使用する溶媒が、イソプロピルアルコール及びエタノールからなる群から選ばれる少なくとも一つである請求項12に記載の選択的膜堆積方法。
- 前記基板に対して、前記一般式(1)で表される有機物により選択的に膜を堆積させた後、前記基板を前記溶媒で洗浄する、請求項7~13のいずれか1項に記載の選択的膜堆積方法。
- 前記金属が、Cu、Co、Ru、Ni、Pt、Al、Ta、Ti及びHfからなる群より選ばれる少なくとも一つの金属であり、前記金属酸化物が、Cu、Co、Ru、Ni、Pt、Al、Ta、Ti及びHfからなる群より選ばれる少なくとも一つの金属の酸化物である、請求項1~14のいずれか1項に記載の選択的膜堆積方法。
- 前記非金属無機材料が、シリコン、シリコン酸化物、シリコン窒化物及びシリコン酸窒化物からなる群から選ばれる少なくとも一つである、請求項1~15のいずれか1項に記載の選択的膜堆積方法。
- 金属及び金属酸化物のうちの少なくとも1種を含む第一表面領域と、非金属無機材料を含む第二表面領域とが両方とも露出した構造を持つ基板であって、
前記第一表面領域に下記一般式(1)で表される有機物の膜を有し、
前記第二表面領域に前記有機物の膜を有しないか、前記第二表面領域上の前記有機物の膜の厚さt2が、前記第一表面領域上の前記有機物の膜の厚さt1よりも薄いことを特徴とする基板。
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