JP7112793B2 - 成膜方法及び成膜装置 - Google Patents
成膜方法及び成膜装置 Download PDFInfo
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- JP7112793B2 JP7112793B2 JP2021554934A JP2021554934A JP7112793B2 JP 7112793 B2 JP7112793 B2 JP 7112793B2 JP 2021554934 A JP2021554934 A JP 2021554934A JP 2021554934 A JP2021554934 A JP 2021554934A JP 7112793 B2 JP7112793 B2 JP 7112793B2
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- 238000000034 method Methods 0.000 title claims description 114
- 239000007789 gas Substances 0.000 claims description 119
- 238000006243 chemical reaction Methods 0.000 claims description 86
- 239000012495 reaction gas Substances 0.000 claims description 58
- 239000002994 raw material Substances 0.000 claims description 36
- 230000004913 activation Effects 0.000 claims description 13
- 230000015572 biosynthetic process Effects 0.000 claims description 12
- 238000009616 inductively coupled plasma Methods 0.000 claims description 6
- 230000003213 activating effect Effects 0.000 claims description 5
- 125000002524 organometallic group Chemical group 0.000 claims description 5
- 238000005121 nitriding Methods 0.000 claims description 4
- 230000001590 oxidative effect Effects 0.000 claims description 3
- 238000000231 atomic layer deposition Methods 0.000 description 68
- 238000005229 chemical vapour deposition Methods 0.000 description 56
- GIRKRMUMWJFNRI-UHFFFAOYSA-N tris(dimethylamino)silicon Chemical compound CN(C)[Si](N(C)C)N(C)C GIRKRMUMWJFNRI-UHFFFAOYSA-N 0.000 description 11
- 238000010926 purge Methods 0.000 description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 9
- 239000006227 byproduct Substances 0.000 description 5
- 230000006698 induction Effects 0.000 description 5
- 239000011261 inert gas Substances 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 229910052814 silicon oxide Inorganic materials 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 239000011148 porous material Substances 0.000 description 3
- 235000012239 silicon dioxide Nutrition 0.000 description 3
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
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- 239000000376 reactant Substances 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- MNWRORMXBIWXCI-UHFFFAOYSA-N tetrakis(dimethylamido)titanium Chemical compound CN(C)[Ti](N(C)C)(N(C)C)N(C)C MNWRORMXBIWXCI-UHFFFAOYSA-N 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- JLTRXTDYQLMHGR-UHFFFAOYSA-N trimethylaluminium Chemical compound C[Al](C)C JLTRXTDYQLMHGR-UHFFFAOYSA-N 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
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Description
成膜対象にCVD膜とALD膜とを成膜する成膜方法であって、
前記ALD膜を成膜するALDプロセスでは、
成膜対象が配置された反応容器を、第1供給管を介して導入される原料ガスで充満させる第1工程と、
前記第1工程後に、前記反応容器の気相中の前記原料ガスを排気する第2工程と、
前記第2工程後に、第2供給管内で誘導結合プラズマにより活性化されて前記第2供給管を介して導入される反応ガスで、前記反応容器を充満させる第3工程と、
前記第3工程後に、前記反応ガスを前記反応容器から排気する第4工程と、
を含むALDサイクルが複数回繰り返し実施され、
前記CVD膜を成膜するCVDプロセスでは、前記ALDサイクルが少なくとも1回実施され、かつ、前記第2工程の排気は、前記反応容器の気相中に前記原料ガスを残存させたまま終了させる成膜方法に関する。
成膜対象が配置される反応容器と、
原料ガスを前記反応容器に供給する第1供給管と、
前記反応容器と接続され、反応ガスが供給される第2供給管と、
前記第2供給部管内の前記反応ガスを誘導結合プラズマにより活性化する反応ガス活性化装置と、
前記反応容器内を排気する排気部と、
CVDプロセスとALDプロセスとを制御する制御部と、
を有し、
前記制御部は、
前記ALDプロセスでは、
前記成膜対象が配置された前記反応容器に前記第1供給管を介して前記原料ガスを導入する第1工程と、
前記第1工程後に、前記排気部により前記原料ガスを前記反応容器から排気する第2工程と、
前記第2工程後に、前記第2供給管内で前記反応ガス活性化装置により活性化された前記反応ガスを、前記第2供給管を介して前記反応容器に導入する第3工程と、
前記第3工程後に、前記反応ガスを前記反応容器から排気する第4工程と、
を含むALDサイクルを複数回繰り返し実施させ、
前記CVDプロセスでは、前記ALDサイクルを少なくとも1回実施させ、かつ、前記第2工程は、前記反応容器の気相中に前記原料ガスを残存させたまま終了させる成膜装置に関する。
図1は、実施形態に係る成膜装置を示す。図1において、成膜装置10は、例えば石英製の反応容器20を有する。反応容器20は、原料ガス導入口30と、反応ガス導入口40と、排気口50とを有する。反応容器20内には成膜対象1を例えば載置して支持する支持部60が設けられる。
図3に示すように、多孔質体1を成膜するために、先ずCVD膜4を形成し、その後、CVD膜4上にALD膜5を形成する。CVD膜4が多孔質体1の孔1Aを埋め、緻密なALD膜5が、密度が疎であり例えばバリア性の乏しいCVD膜4を被覆することができる。それにより、多孔質体1の表面を、例えば疎水性または親水性等の特性を有する表面に改質することができる。
説明の便宜上、先ず、ALDプロセスを説明する。ALDプロセスは、第1工程~第4工程を1サイクルとするALDサイクルを、ALD膜5の膜厚が得られるまで繰り返し実施される。
ALDサイクルを実施するにあたり、先ず、排気ポンプ310により反応容器20内が真空引きされ、反応容器20内が例えば10-4Paに設定される。次に、ALDサイクルの第1工程として、第1バルブ120を開状態として原料ガスTDMASが反応容器20内に供給され、第1バルブ120が閉鎖される。それにより、反応容器20内は比較的低い圧力例えば1~10Paにて原料ガスで充満される。ALDサイクルの第1工程で、支持部60上の成膜対象1の表面にTDMASが吸着される。
第1工程の開始後のT1A時間経過後、ALDサイクルの第2工程として、反応容器20内に例えばパージガスが導入され、反応容器20内の気相中の原料ガスTDMASは排気され、反応容器20内がパージガスに置換される。この排気時間をT2Aとする。
次に、ALDサイクルの第3工程として、反応ガス活性化装置210で活性化された反応ガスであるOHラジカル(OH*)が、第2バルブ230を開状態とすることで反応容器20内に導入される。その後、第2バルブ230が閉鎖されて、反応容器20内は比較的低い圧力にて反応ガスで充満される。その結果、成膜対象1の表面では、TDMASがOHラジカル(OH*)と反応する。具体的には、TDMASがOHラジカル(OH*)により酸化されて、シリコン酸化膜SiO2が生成される。それにより、成膜対象1の表面はシリコン酸化膜により被覆される。また、シリコン酸化膜上にはヒドロキシ基(-OH)が形成される。このヒドロキシ基(-OH)上には、有機金属ガスは室温でも飽和吸着が可能である。よって、成膜中に成膜対象1を強制加熱する必要がない。
第3工程の開始後のT3A時間経過後、ALDサイクルの第4工程として、反応容器20内に例えばパージガスが導入され、反応容器20内の気相中の活性化反応ガスは排気され、反応容器20内がパージガスに置換される。第4工程の排気時間T4Aは、例えば第2工程の排気時間T2Aと等しくすることができる。
図5に示すように、CVDプロセスもALDサイクルと同様に第1工程~第4工程を有する。第1工程の時間をT1C、第2工程の時間をT2C、第3工程の時間をT3C及び第4工程の時間をT4Cとすると、例えば、T1C=T2A、T2C<T2A、T3C=T3A及びT4C=T4Aに設定される。つまり、CVDプロセスでは、第2工程の時間T2CがALDサイクルの第2工程の時間T2Aよりも短く設定される点を除いて、ALDサイクルと等しく設定することができる。
Claims (5)
- 成膜対象にCVD膜とALD膜とを成膜する成膜方法であって、
前記ALD膜を成膜するALDプロセスでは、
成膜対象が配置された反応容器を、第1供給管を介して導入される原料ガスで充満させる第1工程と、
前記第1工程後に、前記反応容器の気相中の前記原料ガスを排気する第2工程と、
前記第2工程後に、第2供給管内で誘導結合プラズマにより活性化されて前記第2供給管を介して導入される反応ガスで、前記反応容器を充満させる第3工程と、
前記第3工程後に、前記反応ガスを前記反応容器から排気する第4工程と、
を含むALDサイクルが複数回繰り返し実施され、
前記CVD膜を成膜するCVDプロセスでは、前記ALDサイクルが少なくとも1回実施され、
前記ALDプロセス及び前記CVDプロセスでは、前記第1工程の時間は実質的に等しく設定され、
前記CVDプロセスでの前記第2工程の時間は、前記ALDプロセスでの前記第2工程の時間よりも短く設定されて、前記第2工程の排気は、前記反応容器の気相中に前記原料ガスを残存させたまま終了させる成膜方法。 - 成膜対象にCVD膜とALD膜とを成膜する成膜方法であって、
前記ALD膜を成膜するALDプロセスでは、
成膜対象が配置された反応容器を、第1供給管を介して導入される原料ガスで充満させる第1工程と、
前記第1工程後に、前記反応容器の気相中の前記原料ガスを排気する第2工程と、
前記第2工程後に、第2供給管内で誘導結合プラズマにより活性化されて前記第2供給管を介して導入される反応ガスで、前記反応容器を充満させる第3工程と、
前記第3工程後に、前記反応ガスを前記反応容器から排気する第4工程と、
を含むALDサイクルが複数回繰り返し実施され、
前記CVD膜を成膜するCVDプロセスでは、前記ALDサイクルが少なくとも1回実施され、かつ、前記第2工程の排気は、前記反応容器の気相中に前記原料ガスを残存させたまま終了させ、
前記成膜対象は多孔質体であり、成膜される面に開口する孔を有し、
前記CVDプロセスの実施により前記CVD膜によって前記開口を塞ぎ、その後、前記ALDプロセスの実施により前記CVD膜上に前記ALD膜を成膜する成膜方法。 - 請求項1または2において、
前記原料ガスは有機金属ガスであり、
前記反応ガスは酸化ガスである成膜方法。 - 請求項1または2において、
前記原料ガスは有機金属ガスであり、
前記反応ガスは窒化ガスである成膜方法。 - 成膜対象が配置される反応容器と、
原料ガスを前記反応容器に供給する第1供給管と、
前記反応容器と接続され、反応ガスが供給される第2供給管と、
前記第2供給部管内の前記反応ガスを誘導結合プラズマにより活性化する反応ガス活性化装置と、
前記反応容器内を排気する排気部と、
CVDプロセスとALDプロセスとを制御する制御部と、
を有し、
前記制御部は、
前記ALDプロセスでは、
前記成膜対象が配置された前記反応容器に前記第1供給管を介して前記原料ガスを導入する第1工程と、
前記第1工程後に、前記排気部により前記原料ガスを前記反応容器から排気する第2工程と、
前記第2工程後に、前記第2供給管内で前記反応ガス活性化装置により活性化された前記反応ガスを、前記第2供給管を介して前記反応容器に導入する第3工程と、
前記第3工程後に、前記反応ガスを前記反応容器から排気する第4工程と、
を含むALDサイクルを複数回繰り返し実施させ、
前記CVDプロセスでは、前記ALDサイクルを少なくとも1回実施させ、
前記ALDプロセス及び前記CVDプロセスでは、前記第1工程の時間は実質的に等しく設定され、
前記CVDプロセスでの前記第2工程の時間は、前記ALDプロセスでの前記第2工程の時間よりも短く設定されて、前記第2工程の排気は、前記反応容器の気相中に前記原料ガスを残存させたまま終了させる成膜装置。
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