JP7007795B2 - 有機膜の気相堆積 - Google Patents
有機膜の気相堆積 Download PDFInfo
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- JP7007795B2 JP7007795B2 JP2016197037A JP2016197037A JP7007795B2 JP 7007795 B2 JP7007795 B2 JP 7007795B2 JP 2016197037 A JP2016197037 A JP 2016197037A JP 2016197037 A JP2016197037 A JP 2016197037A JP 7007795 B2 JP7007795 B2 JP 7007795B2
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Images
Classifications
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- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D1/00—Processes for applying liquids or other fluent materials
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- C—CHEMISTRY; METALLURGY
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45523—Pulsed gas flow or change of composition over time
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
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- H01L21/02118—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer carbon based polymeric organic or inorganic material, e.g. polyimides, poly cyclobutene or PVC
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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
- H01L21/02263—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase
- H01L21/02271—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase deposition by decomposition or reaction of gaseous or vapour phase compounds, i.e. chemical vapour deposition
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- 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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- H01L21/0228—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase deposition by decomposition or reaction of gaseous or vapour phase compounds, i.e. chemical vapour deposition deposition by cyclic CVD, e.g. ALD, ALE, pulsed CVD
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- H01L21/02107—Forming insulating materials on a substrate
- 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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Description
本出願は、2015年10月9日出願の米国特許出願第14/879,962号の一部継続出願である。
本発明は、気相堆積によって有機薄膜を形成する方法に関する。
図5A~5Dは、気化器から基板への負の温度差を用いるもの(図5Aおよび5B)と気化器から基板への正の温度差を用いるもの(図5Cおよび5D)との同様な逐次堆積プロセスを比較する実験の結果を示す。すべての実験は、ASM International,N.V.(Almere、オランダ)によって提供されるPULSAR 3000(商標)beta ALDツールの中で300mmウエハを使用した。負の温度差は、正の差を有するプロセスと比べて3倍を超える成長速度で膜を堆積し、はるかに高い厚さ均一性を有する膜を作り出した。
トレンチをパターン形成したウエハの上で行った別の負の温度差実験において、PMDAとDAHとを逐次プロセスにおいて反応させてトレンチパターンを有する基板の上にポリイミド膜を堆積した。トレンチは40および50nmの可変ピッチと25~35nmの開口とを有した。第一の反応体PMDAを150℃の温度で気化し、PMDAガスラインを153℃に維持し、基板を127℃に維持した。第二の反応体DAHを45℃に保った。450sccmのライン流量を用い、PMDAおよびDAHに11/8.066秒および4.68/9秒のパルス/パージ長さをそれぞれ用いた。得られた膜をトンネル電子顕微鏡法(TEM)によって分析した。20サイクル後、TEM画像は、膜がトレンチ底部区域で厚くなり、トレンチの側壁で薄くなることを示した。同じパラメータを用いて成長した平らなウエハ上の膜厚は7nmであり、いくつかのトレンチの底部の上の膜厚は約11nmであり、いくつかのトレンチの側部の上の膜厚は約4nmであった。したがって、成長は、トレンチの底部区域でより速く進み、ボトムアップ充填を示した。60回の堆積サイクル後、TEM分析は、ポリイミドによるトレンチの継ぎ目のないボトムアップギャップ充填を示した。上面は、比較的滑らかであり、ある程度の自己平坦化挙動を示した。
別の負の温度差実験において、逐次堆積プロセスにおいてPMDAとDAHとを反応させてトレンチパターンを有する基板の上にポリイミド膜を堆積した。さまざまな時間のパージ長さを用いた。一つの膜においてはPMDAに8.066秒、DAHに9.0秒のパージ長さを用い、別の膜においてはPMDAとDAHとのそれぞれに15秒のパージ長さを用い、別の膜においてはPMDAとDAHとのそれぞれに25秒のパージ長さを用いた。得られた膜をTEMによって分析した。パージ長さは、ギャップ充填性能に確かに影響を及ぼすようであった。しかし、短いパージほど構造体の上に平坦な膜が得られた。したがってパージ長さは、膜の最終形態を調整する因子として用いることができる。
別の負の差実験において、異なる温度における二種類の別々の交互および逐次堆積プロセスにおいてPMDAとDAHとを反応させた。第一の実験において、PMDAを150℃で気化し、基板を127℃に維持した。第二の実験において、PMDAを180℃で気化し、基板を160℃に維持した。第一の実験において堆積した膜は主としてポリアミック酸であり、第二の実験において堆積した膜は主としてポリイミドであった。堆積温度は、反応体がPMDAおよびDAHであるとき、堆積される膜の組成に影響を及ぼすようである。低い堆積温度ほどポリアミック酸の比率が大きくなるようであり、高い堆積温度ほどポリイミドの比率が大きくなるようであった。
別の負の温度差実験において、堆積したポリアミック酸膜をアニールしてポリイミドを形成した。PMDAとDAHとを反応させるとき低い堆積温度ほどポリアミック酸が大きな比率で堆積する。FTIR分光法によってポリイミドへの変換を確認した。異なる温度でアニールした4種類のポリアミック酸膜についてのデータは、次の通りである。
別の負の温度差実験において、さまざまな温度で有機膜を堆積した。分光電位測定法(SE)およびX線反射率(XRR)を用いて厚さを分析し、厚さを測定した。密度およびRMS粗さも測定した。4種類の膜についてのデータは、次の通りである。
別の負の温度差実験において、ポリアミック酸からポリイミドなどのエッチング耐性がより高い高分子への変換を確認するために、水を用いて堆積膜をエッチングした。ポリアミック酸は水溶性であり、水によってエッチングすることができる。それに対して、ポリイミドは水溶性でなく、水によってエッチングすることができない。第一の膜は127℃で堆積し、したがって大部分がポリアミック酸であった。第二の膜は160℃で堆積し、したがって大部分がポリイミドであった。第三の膜は127℃で堆積し、続いてアルゴンプラズマで処理して堆積したポリアミック酸をポリイミドへ変換した。膜の厚さを水への暴露の前後に測定し、水によるエッチングの程度を定量するため比較した。以下のデータは、127℃で堆積したポリアミック酸膜が水によってエッチングされ、160℃で堆積したポリイミド膜と、127℃で堆積し、続いて硬化してポリイミドを形成したポリアミック酸膜とが水によってエッチングされなかったことを示す。
トレンチをパターン形成したウエハの上で行った別の負の温度差実験において、逐次プロセスにおいて1,4-フェニレンジイソシアナート(PDIC)とDAHとを反応させてトレンチパターンを有する基板上にポリウレア膜を堆積した。トレンチは、40および50nmの可変ピッチと25~35nmの開口とを有した。第一の反応体PDICを75℃の温度で気化し、PDICガスラインを85℃に維持し、基板を40℃に維持した。第二の反応体DAHを45℃に保った。450sccmのライン流量を用い、PDICおよびDAHに3/2秒および8/7秒のパルス/パージ長さをそれぞれ用いた。得られた膜をトンネル電子顕微鏡法(TEM)によって分析した。50サイクル後、TEM画像は、膜がトレンチ底部区域で厚くなり、トレンチの側壁で薄くなることを示した(図6A)。同じパラメータを用いて成長した平らなウエハ上の膜厚は7nmであり、いくつかのトレンチの底部の上の膜厚は約10nmであり、いくつかのトレンチの側部の上の膜厚は約3nmであった。したがって、成長は、トレンチの底部区域でより速く進み、ボトムアップ充填を示した。215回の堆積サイクル後、TEM分析(図6B)は、ポリウレアによるトレンチの継ぎ目のないボトムアップギャップ充填を示した。三次元フィーチャのアスペクト比は小さくなり、ある程度の自己平坦化挙動を示した。
Claims (30)
- 有機膜堆積のための装置であって、
有機反応体を気化して反応体蒸気を形成するように構成された容器と、
基板を収容し、前記容器と選択的に流体連通するように構成された反応空間と、
前記容器の中の前記反応体を温度A以上に維持し、
前記基板を前記温度Aより低い温度Bに維持し、
前記容器内の圧力と前記反応空間内の圧力との間で圧力の差を維持し、
ここで、前記容器内の圧力を前記反応空間内の圧力よりも高く、ここで、圧力の差が80Torr未満で、
前記圧力の差を維持しながら、前記反応体蒸気を前記容器から前記基板へ輸送し、前記基板の上に有機膜を堆積する
ように構成された制御システムと、
を備える、装置。 - 前記有機膜は、高分子を含む、請求項1に記載の装置。
- 前記容器は、室温および大気圧で固体を収容する、請求項1に記載の装置。
- 前記容器は、ピロメリット酸二無水物(PMDA)を収容する、請求項1に記載の装置。
- 前記制御システムは、ケルビンで表わした温度Bに対する温度Aの比を1より大きく、1.25より小さく維持するようにさらに構成された、請求項1に記載の装置。
- 前記制御システムは、前記温度Bを前記温度Aより5℃から50℃低く維持するようにさらに構成された、請求項1に記載の装置。
- 前記容器を前記反応空間へ流体接続するガスラインをさらに含み、前記制御システムは、前記ガスラインを温度Cに維持するようにさらに構成され、前記温度Cは、前記温度Aより高い、請求項1に記載の装置。
- 前記反応空間に接続された出口ラインおよび不活性ガス供給源をさらに備え、前記制御システムは、前記反応体蒸気および第二の反応体の蒸気の供給の間に余分な反応体蒸気および副生成物を除去するようにさらに構成され、
前記制御システムは、逐次堆積プロセスにおいて前記反応体蒸気と交互に第二の反応体の蒸気を前記基板へ輸送するようにさらに構成された、請求項1に記載の装置。 - 有機膜を気相堆積するための方法であって、
気化器の中で第一の有機反応体を温度Aで気化して第一の反応体の蒸気を形成するステップと、
反応空間の中で基板を前記温度Aより低い温度Bで前記第一の反応体の蒸気に曝露するステップと、
前記気化器内の圧力と前記反応空間内の圧力との間で圧力の差を維持するステップと、
ここで、前記気化器内の圧力を前記反応空間内の圧力よりも高く、ここで、圧力の差が80Torr未満で、
前記圧力の差を維持しながら、前記基板の上に前記有機膜を堆積するステップと、
を含む方法。 - 前記有機膜は、高分子を含む、請求項9に記載の方法。
- 前記高分子は、ポリイミドを含む、請求項10に記載の方法。
- 前記有機膜は、ポリアミック酸を含み、前記ポリアミック酸膜をポリイミド膜へ変換するステップをさらに含む、請求項9に記載の方法。
- 前記第一の反応体は、室温および大気圧で固体である、請求項9に記載の方法。
- 前記第一の反応体は、酸二無水物である、請求項9に記載の方法。
- ケルビンで表わした温度Bに対する温度Aの比は、1より大きく、1.15より小さい、請求項9に記載の方法。
- 前記温度Bは、前記温度Aより5℃から50℃の間だけ低い、請求項9に記載の方法。
- 前記基板は、平面でないトポグラフィーを含み、前記有機膜を堆積するステップは、前記基板の下部フィーチャの上に第一の厚さを形成するステップと、前記基板の上部領域区域の上に第二の厚さを堆積するステップとを含み、前記第一の厚さは、前記第二の厚さより大きく、
前記基板を曝露するステップは、前記基板の上に前記第一の反応体の化学種を自己制限的に吸着するステップを含み、前記方法は、
余分な前記第一の反応体を前記基板との接触から除くステップと、
前記第一の反応体の蒸気と第二の反応体とが実質的に混合しないように、前記基板を前記第二の反応体に曝露するステップと、
余分な前記第二の反応体を前記基板との接触から除くステップと、
をさらに含む、請求項9に記載の方法。 - 基板の上の三次元構造体のアスペクト比を小さくするための方法であって、
第一の反応体を気化して第一の反応体の蒸気を形成するステップと、
反応空間の中で基板を前記第一の反応体の蒸気に曝露するステップであって、前記基板は、三次元構造を有するトポグラフィーを含む、ステップと、
有機膜がコンフォーマルでない層であって、堆積するにつれて前記有機膜が前記基板の上の前記三次元構造体のアスペクト比を小さくするように、前記トポグラフィーの上部フィーチャと比較して前記トポグラフィーの下部フィーチャの上で前記基板の上に優先的に堆積するステップであって、前記堆積は、前記基板を前記第一の反応体の蒸気に曝露することを含む、ステップと、
を含む方法。 - 前記気化は、温度Aで行われ、前記基板は堆積時、温度Bであり、ケルビンで表わした温度Bに対する温度Aの比は、1から1.15の間である、請求項18に記載の方法。
- 前記温度Bは、前記温度Aより5℃から50℃の間だけ低い、請求項19に記載の方法。
- 前記堆積するステップは、
前記基板を第二の反応体の蒸気に曝露して前記基板の上の前記第一の反応体の蒸気の化学種と反応させるステップと、
前記基板を前記第一の反応体の蒸気に曝露するステップと前記基板を前記第二の反応体の蒸気に曝露するステップとを交互に逐次的に繰り返すステップと、
をさらに含む、請求項18に記載の方法。 - 気化温度Aと基板温度Bとを、B<Aとなるように制御するステップをさらに含む、請求項18に記載の方法。
- 前記有機膜を堆積するステップは、ポリアミック酸膜を堆積するステップを含み、前記ポリアミック酸膜をポリイミド膜へ変換するステップをさらに含む、請求項22に記載の方法。
- 前記第一の反応体は、有機反応体であり、前記曝露するステップは、前記反応空間を画定する反応器の側方を通って延在する加熱されたガスラインを通して前記第一の反応体の蒸気を、前記反応空間内の前記基板の上のガス分配ブロックへ供給するステップを含む、請求項18に記載の方法。
- 前記ガス分配ブロックは、前記反応空間に到達するまでの前記第一の反応体の蒸気と第二の反応体の蒸気とのために別々の流路を維持する、請求項24に記載の方法。
- 気化器の中で第一の反応体を気化して第一の反応体の蒸気を形成するステップと、
反応空間の中で基板を前記第一の反応体の蒸気と第二の反応体の蒸気とに曝露するステップと、ここで、前記基板温度は、前記曝露するステップの間、130℃未満の温度に維持されて、
前記第一の反応体の蒸気と前記第二の反応体の蒸気からのポリアミック酸膜を前記基板の上に堆積するステップと、ここで、堆積したポリアミック酸膜は大部分がポリアミック酸を含む、
を含む、有機膜を形成する方法。 - 前記ポリアミック酸膜をポリイミドへ変換するステップをさらに含む、請求項26に記載の方法。
- 前記第一の反応体は、ピロメリット酸二無水物(PMDA)を含む酸二無水物を含む、請求項26に記載の方法。
- 前記第二の反応体は、1,6-ジアミノヘキサン(DAH)を含むジアミンを含む、請求項28に記載の方法。
- 前記制御システムが、逐次堆積プロセスにおいて前記反応体の蒸気と交互に第二の反応体の蒸気を前記基板に輸送することによって前記有機膜を堆積するように構成される、請求項1に記載の装置。
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