JP6597296B2 - 基板処理方法 - Google Patents
基板処理方法 Download PDFInfo
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- JP6597296B2 JP6597296B2 JP2015253439A JP2015253439A JP6597296B2 JP 6597296 B2 JP6597296 B2 JP 6597296B2 JP 2015253439 A JP2015253439 A JP 2015253439A JP 2015253439 A JP2015253439 A JP 2015253439A JP 6597296 B2 JP6597296 B2 JP 6597296B2
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- 239000000758 substrate Substances 0.000 title claims description 85
- 238000003672 processing method Methods 0.000 title claims description 9
- 239000007789 gas Substances 0.000 claims description 60
- 238000012545 processing Methods 0.000 claims description 41
- 238000005530 etching Methods 0.000 claims description 32
- 229910052731 fluorine Inorganic materials 0.000 claims description 23
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 22
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 22
- 238000010438 heat treatment Methods 0.000 claims description 21
- 238000009832 plasma treatment Methods 0.000 claims description 17
- 238000011282 treatment Methods 0.000 claims description 16
- 239000011261 inert gas Substances 0.000 claims description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 7
- 239000010703 silicon Substances 0.000 claims description 7
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 7
- 229910044991 metal oxide Inorganic materials 0.000 claims description 6
- 150000004706 metal oxides Chemical class 0.000 claims description 6
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 claims description 5
- 239000006227 byproduct Substances 0.000 claims description 5
- 239000011737 fluorine Substances 0.000 claims description 5
- 150000002366 halogen compounds Chemical class 0.000 claims description 5
- 150000002500 ions Chemical class 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 claims description 3
- 230000004913 activation Effects 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 claims description 2
- 238000007254 oxidation reaction Methods 0.000 claims description 2
- 230000001590 oxidative effect Effects 0.000 claims description 2
- 238000012360 testing method Methods 0.000 description 152
- 238000011156 evaluation Methods 0.000 description 129
- 229910004298 SiO 2 Inorganic materials 0.000 description 55
- 238000000137 annealing Methods 0.000 description 54
- 238000012546 transfer Methods 0.000 description 32
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 30
- 230000005684 electric field Effects 0.000 description 21
- 239000004065 semiconductor Substances 0.000 description 18
- 238000004519 manufacturing process Methods 0.000 description 17
- 229910052757 nitrogen Inorganic materials 0.000 description 14
- 238000000034 method Methods 0.000 description 13
- 238000005259 measurement Methods 0.000 description 12
- 230000008569 process Effects 0.000 description 12
- 230000015572 biosynthetic process Effects 0.000 description 11
- 229910052739 hydrogen Inorganic materials 0.000 description 11
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 10
- 238000003795 desorption Methods 0.000 description 10
- 238000001020 plasma etching Methods 0.000 description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 8
- 238000001228 spectrum Methods 0.000 description 8
- 230000015556 catabolic process Effects 0.000 description 7
- 239000001257 hydrogen Substances 0.000 description 7
- 229910052760 oxygen Inorganic materials 0.000 description 7
- 238000009616 inductively coupled plasma Methods 0.000 description 6
- 238000005040 ion trap Methods 0.000 description 6
- 230000006866 deterioration Effects 0.000 description 5
- 230000007246 mechanism Effects 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 150000002222 fluorine compounds Chemical class 0.000 description 4
- 229910052736 halogen Inorganic materials 0.000 description 4
- 150000002367 halogens Chemical class 0.000 description 4
- 238000011084 recovery Methods 0.000 description 4
- 235000012239 silicon dioxide Nutrition 0.000 description 4
- 229910001873 dinitrogen Inorganic materials 0.000 description 3
- 239000010453 quartz Substances 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 2
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 2
- 229910052794 bromium Inorganic materials 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000005240 physical vapour deposition Methods 0.000 description 2
- 230000032258 transport Effects 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
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910000449 hafnium oxide Inorganic materials 0.000 description 1
- WIHZLLGSGQNAGK-UHFFFAOYSA-N hafnium(4+);oxygen(2-) Chemical compound [O-2].[O-2].[Hf+4] WIHZLLGSGQNAGK-UHFFFAOYSA-N 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 150000002829 nitrogen 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
- 239000001301 oxygen Substances 0.000 description 1
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- 229920005591 polysilicon Polymers 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 229910001936 tantalum oxide 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
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
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Description
続いて、前記プラズマ処理により生じた副生成物を前記基板から昇華させて除去するために前記基板を加熱する工程と、
次いで、当該上層膜の除去によって前記プラズマに曝された前記酸化膜の前記上層膜が積層されていた側の表面が露出した状態で、プラズマによる活性化が行われていない不活性ガス雰囲気で前記基板を450℃以上に加熱する加熱処理工程と、
を備え、
前記プラズマ処理工程を行ってから前記加熱処理工程を行うまでに、当該基板の表面を酸化する酸化処理が行われず、
前記プラズマ処理工程は、前記プラズマを構成するイオンとラジカルとを分離し、前記ラジカルを前記基板に供給する工程を備えることを特徴とする。
続いて、本発明に関連して行われた評価試験について説明する。
評価試験1
評価試験1として、p型シリコン基板の表面に形成された犠牲酸化膜を剥離して洗浄した後、当該基板の表面を酸化し、SiO2膜を形成した。このSiO2膜の膜厚は5nm〜6nmである。その後、エッチングモジュール2においてこの基板、つまりSiO2膜を既述のプラズマに曝した後、既述のようにSiO2膜上へのAl膜の形成と、水素ガス雰囲気でのアニール処理とを順に行った。つまり、この評価試験1における基板の処理は、図4のフローチャートで説明した処理とは、N2ガス雰囲気におけるアニール処理が行われていないという点で異なっている。このように基板に一連の処理を行った後は、Al膜に電界を印加すると共に、この電界の強度を変化させて、SiO2膜のリーク電流の特性を調べた。また、対照試験1として、エッチングモジュール2おけるプラズマ処理を行わないことを除いては評価試験1と同様の基板の処理を行った後、SiO2膜について同様の測定を行ってリーク電流の特性を調べた。
評価試験2として評価試験1と略同様に基板に処理を行い、リーク電流を測定した。ただし、評価試験1における基板の処理との差異点として、この評価試験2における基板の処理では、基板をプラズマに曝した後、Al膜を形成する前に、発明の実施の形態で説明したようにN2ガス雰囲気でアニール処理を行った。このアニール処理における基板の加熱温度は600℃、処理時間は10分とした。
評価試験3として、評価試験2と略同様の基板の処理と、基板処理後の測定とを行った。ただし、この評価試験3における基板の処理は、複数の基板について行っており、N2ガス雰囲気におけるアニール処理に関しては、基板毎に異なる温度で処理を行った。具体的には300℃、400℃、500℃のいずれかの温度に基板を加熱してアニール処理を行った。この評価試験3のうち、アニール処理が300℃、400℃、500℃で行われた試験について夫々、評価試験3−1、評価試験3−2、評価試験3−3とする。このような差違を除いて、評価試験3は評価試験2と同様に行われた。従って、基板のアニール処理の時間は10分である。
評価試験4として、評価試験2と略同様の基板の処理と、基板処理後の測定とを行った。評価試験2との差異点を説明すると、この評価試験4ではN2ガス雰囲気でのアニール処理において、基板毎に異なる処理時間を設定して処理を行った。具体的には、アニールの処理時間を10分、15分または20分に設定した。この評価試験4において、アニール処理の時間が10分、15分、20分とされた試験を夫々評価試験4−1、評価試験4−2、評価試験4−3とする。また、この評価試験4のアニール処理では、各基板の加熱温度は500℃とした。
評価試験5では、評価試験2と略同様の基板の処理と、処理後の測定とを行ったが、N2ガス雰囲気でのアニール処理の時間は評価試験2よりも短く、7分とした。このアニール処理の時間を除いて、評価試験5の基板の処理は、評価試験2の基板の処理と同様である。従って、評価試験5のアニール処理の温度は600℃である。図11のグラフは、既述の各グラフと同様に縦軸、横軸にリーク電流、電界強度を夫々設定して、評価試験5の結果を示している。この図11中、評価試験5の結果を点線のグラフの波形で示している。また、図11では評価試験5の結果との比較するために、対照試験1の結果、評価試験2の結果を、実線のグラフの波形、一点鎖線のグラフの波形で夫々示している。
評価試験6として、評価試験1と同様に基板にSiO2膜の形成、プラズマ処理を順次行った。ただし、この評価試験6では、このプラズマ処理後におけるN2ガス雰囲気でのアニール処理、Al膜の形成及び水素ガス雰囲気でのアニール処理は行っていない。そして、プラズマ処理した基板について昇温脱離ガス分光法(TDS)による測定を行い、基板を加熱した際に脱離するガスの検出を行った。この評価試験6のTDSでは、測定中に基板の温度を変化させた。
評価試験7として、評価試験6と同様に処理を行った複数の基板に対してTDSによる測定を行い、M/z=19、即ちFについてのスペクトルを取得した。この評価試験7のTDSでは、測定毎に基板を加熱する温度を変更した。図13のグラフは、このTDSにおいて基板を夫々600℃、500℃で加熱したときに得られたFについてのスペクトルを、実線、波線で夫々示している。この図13のグラフの縦軸はFの信号強度を示し、横軸は基板の加熱を開始してからの経過時間(単位:秒)を示している。
評価試験8として、評価試験6、7と同様に基板にSiO2膜の形成、プラズマ処理を順次行った後、真空中でアニール処理を行った。この一連の処理は複数の基板について行い、基板毎に異なる温度で真空中でのアニール処理を行った。具体的に、600℃または500℃で当該アニール処理を行った。また、この一連の処理後に、各基板を大気雰囲気に24時間曝した後、TDSを行った。このTDSでは、評価試験6と同様に、測定中に基板の温度を変化させた。この評価試験8において、上記のアニール処理の温度を600℃、500℃とした試験を夫々、評価試験8−1、評価試験8−2とする。評価試験8−1、8−2共に、アニール処理の時間は10分である。
2 エッチングモジュール
4 窒素アニールモジュール
51 成膜モジュール
52 水素アニールモジュール
65 SiO2膜
66 SiN膜
Claims (6)
- ハロゲン化合物からなる処理ガスをプラズマ化して得たプラズマを用いて、シリコンあるいは金属の酸化膜が形成された基板をプラズマ処理し、前記酸化膜に積層された上層膜を除去するプラズマ処理工程と、
続いて、前記プラズマ処理により生じた副生成物を前記基板から昇華させて除去するために前記基板を加熱する工程と、
次いで、当該上層膜の除去によって前記プラズマに曝された前記酸化膜の前記上層膜が積層されていた側の表面が露出した状態で、プラズマによる活性化が行われていない不活性ガス雰囲気で前記基板を450℃以上に加熱する加熱処理工程と、
を備え、
前記プラズマ処理工程を行ってから前記加熱処理工程を行うまでに、当該基板の表面を酸化する酸化処理が行われず、
前記プラズマ処理工程は、前記プラズマを構成するイオンとラジカルとを分離し、前記ラジカルを前記基板に供給する工程を備えることを特徴とする基板処理方法。 - 前記加熱処理工程に続いて、前記酸化膜に積層されるように導電膜を形成する工程を行うことを特徴とする請求項1記載の基板処理方法。
- 前記ハロゲン化合物は、フッ素を含む化合物であることを特徴とする請求項1または2記載の基板処理方法。
- 前記プラズマ処理工程は、前記酸化膜に積層された上層膜を除去するエッチング工程であることを特徴とする請求項1ないし3のいずれか一つに記載の基板処理方法。
- 前記上層膜はシリコン窒化膜であることを特徴とする請求項1ないし4のいずれか一つに記載の基板処理方法。
- 前記酸化膜はトランジスタのゲート酸化膜である請求項4または5記載の基板処理方法。
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