JP6749090B2 - ハロゲン系ガスを用いる処理装置における処理方法 - Google Patents
ハロゲン系ガスを用いる処理装置における処理方法 Download PDFInfo
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- JP6749090B2 JP6749090B2 JP2015222244A JP2015222244A JP6749090B2 JP 6749090 B2 JP6749090 B2 JP 6749090B2 JP 2015222244 A JP2015222244 A JP 2015222244A JP 2015222244 A JP2015222244 A JP 2015222244A JP 6749090 B2 JP6749090 B2 JP 6749090B2
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- 229910052736 halogen Inorganic materials 0.000 title claims description 54
- 150000002367 halogens Chemical class 0.000 title claims description 54
- 238000012545 processing Methods 0.000 title claims description 43
- 238000003672 processing method Methods 0.000 title claims description 37
- 239000007789 gas Substances 0.000 claims description 190
- 238000010926 purge Methods 0.000 claims description 47
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims description 37
- 229910001882 dioxygen Inorganic materials 0.000 claims description 37
- 238000000034 method Methods 0.000 claims description 26
- 230000008569 process Effects 0.000 claims description 24
- 239000011651 chromium Substances 0.000 claims description 20
- 229910001220 stainless steel Inorganic materials 0.000 claims description 19
- 239000010935 stainless steel Substances 0.000 claims description 19
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 17
- 239000001301 oxygen Substances 0.000 claims description 17
- 229910052760 oxygen Inorganic materials 0.000 claims description 17
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 8
- 229910052804 chromium Inorganic materials 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 7
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 7
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 claims description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N argon Substances [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 238000004544 sputter deposition Methods 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 2
- 239000000460 chlorine Substances 0.000 description 45
- 238000002161 passivation Methods 0.000 description 40
- 238000005260 corrosion Methods 0.000 description 30
- 230000007797 corrosion Effects 0.000 description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 26
- 229910001868 water Inorganic materials 0.000 description 26
- 235000012431 wafers Nutrition 0.000 description 19
- 238000001020 plasma etching Methods 0.000 description 18
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 16
- 238000005530 etching Methods 0.000 description 13
- 230000000694 effects Effects 0.000 description 9
- 150000002500 ions Chemical class 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 8
- 238000011109 contamination Methods 0.000 description 8
- 229910052751 metal Inorganic materials 0.000 description 8
- 239000002184 metal Substances 0.000 description 8
- 229910019923 CrOx Inorganic materials 0.000 description 7
- 230000007246 mechanism Effects 0.000 description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 229910052801 chlorine Inorganic materials 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- QSWDMMVNRMROPK-UHFFFAOYSA-K chromium(3+) trichloride Chemical compound [Cl-].[Cl-].[Cl-].[Cr+3] QSWDMMVNRMROPK-UHFFFAOYSA-K 0.000 description 5
- 239000004065 semiconductor Substances 0.000 description 5
- 239000000758 substrate Substances 0.000 description 5
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 4
- 229910021555 Chromium Chloride Inorganic materials 0.000 description 4
- 239000007795 chemical reaction product Substances 0.000 description 4
- 230000001629 suppression Effects 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 230000005684 electric field Effects 0.000 description 3
- 239000011261 inert gas Substances 0.000 description 3
- 230000005764 inhibitory process Effects 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 238000012423 maintenance Methods 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000009832 plasma treatment Methods 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- QWPPOHNGKGFGJK-UHFFFAOYSA-N hypochlorous acid Chemical compound ClO QWPPOHNGKGFGJK-UHFFFAOYSA-N 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 2
- 238000010405 reoxidation reaction Methods 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 229910015189 FeOx Inorganic materials 0.000 description 1
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-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
- 239000007864 aqueous solution Substances 0.000 description 1
- -1 argon ions Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 229910000423 chromium oxide Inorganic materials 0.000 description 1
- 238000005536 corrosion prevention Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
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- 239000000047 product Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000005011 time of flight secondary ion mass spectroscopy Methods 0.000 description 1
- 238000009489 vacuum treatment Methods 0.000 description 1
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- H01J37/32—Gas-filled discharge tubes
- H01J37/32431—Constructional details of the reactor
- H01J37/32798—Further details of plasma apparatus not provided for in groups H01J37/3244 - H01J37/32788; special provisions for cleaning or maintenance of the apparatus
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- 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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- 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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- 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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- 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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- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
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Description
ステンレス鋼は、成分として含有するクロム(Cr)が空気中の酸素と結合することにより、表面に不動態膜(Cr2O3)が形成されている。この不動態膜は安定な物質であり、ハロゲン系ガスに対しても高い耐食性を有している。しかし、水分が存在する環境下ではハロゲン系ガスと反応して腐食が生じることが判明した。例えば、ハロゲンとして塩素(Cl)を用いた場合、大気開放した際の水分が多い環境では、水と塩素が反応して生じた塩酸によって不動態膜が破壊され、塩化クロム(CrCl3)が多く生成されて、ステンレス鋼の表面から剥離または揮発し、パーティクルやガス分子となってメタル汚染を引き起こす。
最初に、本発明の実施形態の処理方法に用いることができる処理装置の一例について説明する。図1はそのような処理装置の概略構成を示す断面図である。
このようなプラズマエッチングを複数枚のウエハについて繰り返して行うと、チャンバ2内や排気装置12等には反応生成物が付着するため、定期的にチャンバ2を大気開放し蓋部2bを開けてチャンバ2内等をメンテナンスする。
本実施形態は、このような問題を解決するものである。
上述したように、ガス供給配管10はステンレス鋼(SUS)製であり、表面に不動態膜が形成されているため高い耐食性を有しているが、水分を含む環境下ではハロゲン系ガスであるCl2ガスと水(H2O)と不動態膜(CrOx)との間では、一例として以下の(1)式および(2)式の反応が生じ、不動態膜が腐食される。
Cl2+H2O ⇔ HCl+HClO ・・・(1)
CrOx+HCl ⇔ CrClx+H2O ・・・(2)
すなわち、塩素ガス(Cl2)と水(H2O)とが反応して塩酸(HCl)が生じ、塩酸が不動態膜(CrOx)と反応して塩化クロム(CrClx)を生成する。
次に、本発明の第2の実施形態に係る処理方法について説明する。
図5は、本発明の第2の実施形態に係る処理方法を示すフロー図である。本実施形態では、第1の実施形態と同様、処理装置1により上記のようなプラズマエッチング処理を1回または複数回行い(ステップ11)、その後酸素ガス等でパージする代わりに、ガス供給配管10内およびチャンバ内をO2プラズマに曝してO2プラズマ処理を行い(ステップ12)、その後チャンバ2の大気開放を行う(ステップ13)。O2プラズマ処理は、ガス供給配管10を介してチャンバ2内に酸素ガスを供給しつつ、高周波電源7から載置台4に高周波電力を供給することにより行うことができる。他の機構でO2プラズマを生成した後、O2プラズマをガス供給配管10を介してチャンバ2内に導入するリモートプラズマであってもよい。
次に、本発明の第3の実施形態に係る処理方法について説明する。
図7は、本発明の第3の実施形態に係る処理方法を示すフロー図である。本実施形態では、第1の実施形態と同様、処理装置1により上記のようなプラズマエッチング処理を1回または複数回行い(ステップ21)、その後、イオン化しやすいガス例えばArガスのプラズマを生成し、Ar+イオンによるスパッタ処理を行う(ステップ22)。これによりガス供給配管表面のClを取り除く。この場合、Clを除去した後は不動態膜が不安定なCrの状態となるため、その後、酸素ガス(O2ガス)またはドライエア(D−Air)をガス供給配管10を介してチャンバ2内に供給してチャンバ2内をパージする(ステップ23)。これにより不動態膜を再酸化させる。その後、チャンバ2の大気開放を行う(ステップ24)。
次に、本発明の第4の実施形態に係る処理方法について説明する。
本実施形態においては、図9に示すように、チャンバ2内で上述したプラズマエッチング処理(ステップ31)を複数回繰り返し行うに際し、一回のプラズマエッチング処理が終了後、次のウエハのプラズマエッチングの間のアイドリングの際に、ガス供給配管10を介してチャンバ2内に酸素ガス(O2ガス)またはドライエア(D−Air)を供給し、チャンバ内をパージする(ステップ32)。これを大気開放までの一連の処理の間、常時続ける。
ここではステンレス鋼(SUS)の試験片を複数準備し、これらを塩素ガス(Cl2ガス)に曝した後、一部を窒素ガス(N2ガス)雰囲気で、残部を水分が0.5ppm以下の実質的に水分が存在しない状態に管理したドライエア(D−Air)雰囲気で72時間保管した。
なお、本発明は上記実施形態に限定されることなく本発明の思想の範囲内で種々変形可能である。例えば、上記実施形態では、ステンレス鋼製のガス供給配管の不動態膜の腐食を抑制する例を示したが、チャンバ内部材であるステンレス鋼製ネジや導電性確保のためのステンレス鋼製スパイラルチューブにも効果があり、さらにステンレス鋼の不動態膜のみならず、配管やチャンバ内の表面等に酸化アルミニウム(Al2O3)、酸化イットリウム(Y2O3)等の他の酸化物の膜が形成されている場合にも適用可能であり、その場合にも同様に腐食防止効果を得ることができる。
2;チャンバ
2a;本体部
2b;蓋部
4;載置台
7;高周波電源
8;シャワーヘッド
9;ガス導入口
10;ガス供給配管
11;排気管
12;排気装置
W;半導体ウエハ(被処理体)
Claims (9)
- チャンバ内を真空に保持しつつ、ガス供給配管を介して前記チャンバ内にハロゲン系ガスを供給して被処理体に所定の処理を行う処理装置であって、前記ガス供給配管の表面または前記チャンバの表面に酸化膜が形成された処理装置における処理方法であって、
前記チャンバ内で被処理体に対する前記所定の処理を1回または複数回行った後、前記チャンバを大気開放するにあたり、前記大気開放に先立って、前記ガス供給配管を介して前記チャンバに酸素ガスを供給して前記チャンバをパージし、前記ガス供給配管または前記チャンバに付着している前記ハロゲン系ガスの成分を除去するとともに、前記ガス供給配管の前記酸化膜または前記チャンバの前記酸化膜の腐食部分を再酸化することを特徴とする、ハロゲン系ガスを用いる処理装置における処理方法。 - 前記パージと同時に、または前記パージに先立って、イオンスパッタ処理を行うことを特徴とする請求項1に記載の、ハロゲン系ガスを用いる処理装置における処理方法。
- 前記イオンスパッタ処理は、アルゴンガスのプラズマを生成して得られたアルゴンイオンを用いて行われることを特徴とする請求項2に記載の、ハロゲン系ガスを用いる処理装置における処理方法。
- チャンバ内を真空に保持しつつ、ガス供給配管を介して前記チャンバ内にハロゲン系ガスを供給して被処理体に所定の処理を行う処理装置であって、前記ガス供給配管の表面または前記チャンバの表面に酸化膜が形成された処理装置における処理方法であって、
前記チャンバ内で被処理体に対する前記所定の処理を1回または複数回行った後、前記チャンバを大気開放するにあたり、前記大気開放に先立って、前記ガス供給配管を介して前記チャンバ内に酸素ガスを供給しつつ前記チャンバ内に酸素プラズマを生成し、または前記ガス供給配管を介して前記チャンバに酸素プラズマを供給して、前記チャンバ内を前記酸素プラズマにより処理し、前記ガス供給配管または前記チャンバに付着している前記ハロゲン系ガスの成分を除去するとともに、前記ガス供給配管の前記酸化膜または前記チャンバの前記酸化膜の腐食部分を再酸化することを特徴とする、ハロゲン系ガスを用いる処理装置における処理方法。 - チャンバ内を真空に保持しつつ、ガス供給配管を介して前記チャンバ内にハロゲン系ガスを供給して被処理体に所定の処理を行う処理装置であって、前記ガス供給配管の表面または前記チャンバの表面に酸化膜が形成された処理装置における処理方法であって、
前記チャンバ内で被処理体に対して前記所定の処理を、前記チャンバを真空に保持したまま複数回行い、これら複数回の前記所定の処理の間のアイドリングの際に、前記ガス供給配管を介して前記チャンバに酸素ガスを供給し、前記チャンバをパージし、前記ガス供給配管または前記チャンバに付着している前記ハロゲン系ガスの成分を除去するとともに、前記ガス供給配管の前記酸化膜または前記チャンバの前記酸化膜の腐食部分を再酸化することを特徴とする、ハロゲン系ガスを用いる処理装置における処理方法。 - 前記アイドリングの際の前記パージは、酸素ガスに窒素ガスを混合して行うことを特徴とする請求項5に記載の、ハロゲン系ガスを用いる処理装置における処理方法
- 前記アイドリングの際の前記パージを酸素ガスにより所定期間行った後、前記アイドリングの残りの期間に、前記チャンバ内を窒素ガスによりパージすることを特徴とする請求項5に記載の、ハロゲン系ガスを用いる処理装置における処理方法。
- 前記チャンバに接続されたガス供給配管は、ステンレス鋼製であり、前記酸化膜はクロムの不動態膜であることを特徴とする請求項1から請求項7のいずれか1項に記載の、ハロゲン系ガスを用いる処理装置における処理方法。
- 前記ハロゲン系ガスは、塩素ガスであることを特徴とする請求項1から請求項8のいずれか1項に記載の、ハロゲン系ガスを用いる処理装置における処理方法。
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