JP2005175466A - 反応器表面から物質を除去するための方法、装置及び混合物 - Google Patents
反応器表面から物質を除去するための方法、装置及び混合物 Download PDFInfo
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- JP2005175466A JP2005175466A JP2004342118A JP2004342118A JP2005175466A JP 2005175466 A JP2005175466 A JP 2005175466A JP 2004342118 A JP2004342118 A JP 2004342118A JP 2004342118 A JP2004342118 A JP 2004342118A JP 2005175466 A JP2005175466 A JP 2005175466A
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- FAQYAMRNWDIXMY-UHFFFAOYSA-N trichloroborane Chemical compound ClB(Cl)Cl FAQYAMRNWDIXMY-UHFFFAOYSA-N 0.000 description 1
- 125000003866 trichloromethyl group Chemical group ClC(Cl)(Cl)* 0.000 description 1
- JOHWNGGYGAVMGU-UHFFFAOYSA-N trifluorochlorine Chemical compound FCl(F)F JOHWNGGYGAVMGU-UHFFFAOYSA-N 0.000 description 1
- 125000002023 trifluoromethyl group Chemical group FC(F)(F)* 0.000 description 1
- SMBZJSVIKJMSFP-UHFFFAOYSA-N trifluoromethyl hypofluorite Chemical compound FOC(F)(F)F SMBZJSVIKJMSFP-UHFFFAOYSA-N 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 238000013022 venting Methods 0.000 description 1
- 238000001039 wet etching Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
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Abstract
【解決手段】一つの態様において、基材30から二酸化ケイ素よりも誘電率の大きい物質40を除去するための方法であって、当該物質40を、ハロゲン含有化合物、ホウ素含有化合物、水素含有化合物、窒素含有化合物、キレート化用化合物、炭素含有化合物、クロロシラン、ヒドロクロロシラン、又はオルガノクロロシランからなる群からの少なくとも1種のものを含む反応剤20と反応させて揮発性生成物70を生成し、そしてこの揮発性生成物70を基材30から除去し、それにより基材30から物質40を除去する。
【選択図】図1a
Description
CO(g)+Cl2(g) → COCl2
1.5C2Cl4(g)+Al2O3 → 2AlCl3(g)+3CO(g)
表8は、この反応が100℃より高い温度で熱力学的に有利であることを示している。
6O2(g)+Al2O3+3C2H2Cl2(g)
=2AlCl3(g)+6CO2(g)+3H2O(g)
表9は、このような反応が0℃と1000℃の間の温度で熱力学的に有利であることを示している。
3C2H2Cl2(g)+Al2O3+3O2(g)
=2AlCl3(g)+6CO(g)+3H2O(g)
表10に示したように、このような部分的な酸化反応はやはり熱力学的に有利である。
2Cl2(g)+Al2O3+C2H2Cl2(g)
=2AlCl3(g)+H2O(g)+2CO(g)
同様に、4:1のCl2:C2H2Cl2モル比では次の反応が可能になる。
4Cl2(g)+Al2O3+C2H2Cl2(g)
=3.333AlCl3(g)
+H2O(g)+2CO2(g)
両方の反応とも、表11と12に示したように、熱力学的に有利である。すすの生成を制御するために塩素を使用することは、過剰量の塩素が金属酸化物の塩素化を促進するので、より望ましい。
HfO2+C5H2O2F6+2Cl2+O2
=HfCl4(g)+H2O(g)+3COF2(g)+2CO(g)
C5H2O2Cl6+Al2O3+0.5O2
=2AlCl3(g)+5CO(g)+H2O(g)
であり、そして、
2C5H2O2Cl6+3HfO2+O2
=3HfCl4(g)+10CO(g)+2H2O(g)
である。
C5H2O2Cl6+Al2O3+Cl2
=2AlCl3(g)+5CO(g)+2HCl(g)
パワーはプラズマエッチング・クリーニングにおける重要な処理パラメータの一つであるから、BCl3プラズマによるAl2O3エッチングのパワー依存性を評価した。結果を下記の表24に列記する。
500mTorrの圧力において、50Wと200Wの間の全てのパワーレベルでHfO2のエッチングを行った。結果を下記の表27に列記する。
500mTorrの圧力及び50Wと200Wの間の種々の圧力レベルを使用して、ZrO2試料でいくつかの実験を行った。結果を下記の表28に列記する。
Al2O3試料の熱エッチング・クリーニング用のエッチング剤としてBCl3を使用して、いくつかの実験を行った。プロセス変数は、下方電極温度、チャンバ圧力、そしてBCl3流量であった。結果を表29に列記する。
HfO2試料の熱エッチング・クリーニング用のエッチング剤としてBCl3を使用して、同様の一組の実験を行った。プロセス変数は、下方電極温度、チャンバ圧力、そしてBCl3流量であった。結果を表30に列記する。
図2に示したのと同じ装置において、例1〜3と同じ方法に従って、8.7スタンダード立方センチメートル(sccm)のNF3と49.3sccmのHeの混合物を使用して、一組のプラズマ実験を行った。3つの異なる高k材料のAl2O3、HfO2及びZrO2を、いろいろなパワー密度とチャンバ圧力で試験した。詳しい実験条件と結果を表31に提示する。表31の結果は、より高いパワー密度と低下したチャンバ圧力がより大きなエッチング速度をもたらすことを示している。一部の事例では、バイアス電圧がより高かったが、これは、エッチング反応が活性化エネルギー障壁を克服するのをより活発なイオン衝撃が助けて活発なイオンによる物理スパッタリングを促進する結果に至る。より低いチャンバ圧力でも、反応副生物の被着と拡散がより速くなることがある。先の例におけるBCl3プラズマ実験の結果と比較すると、NF3プラズマは、Al2O3、HfO2、又はZrO2試料のいずれかについてエッチング速度を有意に低下させた。
BCl3とNF3の混合物を使用して、3つの異なる高k材料のHfO2、ZrO2、及びHfSixOyのエッチング速度を試験した。HfO2の場合は、BCl3の流量は10sccmであり、NF3の流量を調整していろいろなNF3対BCl3体積比を得た。ZrO2とHfSixOyの場合は、全体流量は20sccmであり、BCl3とNF3の流量を調整してそれに応じいろいろなNF3対BCl3体積比を得た。全ての実験について、パワー密度は0.55W/cm2であり、チャンバ圧力は500mTorrであった。実験は、図2に示したのと同じ設備を使用し、そして例1〜3及び比較例1と同じ方法に従って行った。
30 基材(反応チャンバ)
32 反応チャンバの側壁
40 除去すべき物質
50 外部エネルギー源
60 活性種
70 揮発性生成物
Claims (31)
- 反応器表面から物質を除去するための方法であって、
当該反応器表面を有する反応器を準備し、ここにおいて、(a)当該反応器表面は当該物質の膜で少なくとも部分的に被覆されており、(b)当該物質は、遷移金属酸化物、遷移金属ケイ酸塩、13族金属酸化物、13族金属ケイ酸塩、窒素を含有する13族金属酸化物、窒素を含有する13族金属ケイ酸塩、窒素を含有する遷移金属酸化物、窒素を含有する遷移金属ケイ酸塩からなる群より選ばれる少なくとも1種のもの、あるいは、遷移金属酸化物、遷移金属ケイ酸塩、13族金属酸化物、13族金属ケイ酸塩、窒素を含有する遷移金属酸化物、窒素を含有する遷移金属ケイ酸塩、窒素を含有する13族金属酸化物、又は窒素を含有する13族金属ケイ酸塩からなる群より選ばれる少なくとも1つの層を含む積層体であり、そして(c)当該物質は二酸化ケイ素の誘電率よりも大きい誘電率を有すること、
当該物質を反応剤と反応させて揮発性生成物を作り、ここにおいて、当該反応剤は、ハロゲン含有化合物、ホウ素含有化合物、炭素含有化合物、水素含有化合物、窒素含有化合物、キレート化用化合物、クロロシラン化合物、ヒドロクロロシラン化合物、又はオルガノクロロシラン化合物からなる群より選ばれる少なくとも1種のものを含むこと、
そして当該反応器から当該揮発性生成物を除去して、それにより当該表面から当該物質を除去すること、
を含む,反応器表面からの物質除去方法。 - 前記反応器が原子層堆積反応器である、請求項1記載の方法。
- 前記物質が、Al2O3、HfO2、ZrO2、HfSixOy、及びZrSixOy(これらの式中のxは0より大きい数であり、yは2x+2である)からなる群、並びに窒素を含有する前述の化合物のいずれかより選ばれる少なくとも1つのものである、請求項1記載の方法。
- 前記反応剤が、BCl3、COCl2、HCl、Cl2、ClF3、NF3、F2、及びNFzCl3-z(この式のzは0〜2の整数である)からなる群より選ばれる少なくとも1つのものである、請求項1記載の方法。
- 前記反応剤がCOとCl2のその場での反応により生成されるCOCl2である、請求項4記載の方法。
- 前記反応剤がBCl3である、請求項4記載の方法。
- 前記反応剤が式CxHyClz(この式のxは1〜6の範囲の数であり、yは0〜13の範囲の数であり、zは1〜14の範囲の数である)を有する炭素含有化合物である、請求項1記載の方法。
- 前記反応剤をガスボンベ、安全な送給装置、又は真空送給装置から前記物質へ送給する、請求項1記載の方法。
- 前記反応剤を使用箇所の発生器によりその場で生成する、請求項1記載の方法。
- 前記物質を不活性ガス希釈剤で希釈した前記反応剤と接触させる、請求項1記載の方法。
- 前記反応剤がハロゲン含有化合物の混合物を含む、請求項1記載の方法。
- 前記ハロゲン含有化合物の混合物が少なくとも1種の塩素含有ガスと50体積%未満の少なくとも1種のフッ素含有ガスを含む、請求項11記載の方法。
- 反応チャンバの表面の少なくとも一部分から物質を除去するための方法であって、
当該表面の少なくとも一部が当該物質で少なくとも部分的に被覆され、そして当該物質が4.1以上の誘電率を有し、且つ、遷移金属酸化物、遷移金属ケイ酸塩、13族金属酸化物、13族金属ケイ酸塩、窒素を含有する13族金属酸化物、窒素を含有する13族金属ケイ酸塩、窒素を含有する遷移金属酸化物、窒素を含有する遷移金属ケイ酸塩からなる群のうちの少なくとも1種のもの、あるいは、遷移金属酸化物、遷移金属ケイ酸塩、13族金属酸化物、13族金属ケイ酸塩、窒素を含有する13族金属酸化物、窒素を含有する13族金属ケイ酸塩、窒素を含有する遷移金属酸化物、窒素を含有する遷移金属ケイ酸塩からなる群のうちの少なくとも1層を含む積層体である反応チャンバを準備すること、
反応剤を当該反応チャンバへ導入し、ここにおいて、当該反応剤は、ハロゲン含有化合物、ホウ素含有化合物、炭素含有化合物、水素含有化合物、窒素含有化合物、キレート化用化合物、クロロシラン化合物、ヒドロクロロシラン化合物、又はオルガノクロロシラン化合物からなる群より選ばれる少なくとも1種のものを含むこと、
当該物質を当該反応剤と反応させ揮発性生成物を生成するのに十分な1以上のエネルギー源に当該反応剤を暴露すること、
そして当該揮発性生成物を当該反応チャンバから除去すること、
を含む、反応チャンバ表面からの物質除去方法。 - 前記反応剤をガスボンベ、安全な送給装置、又は真空送給装置から前記物質へ送給する、請求項13記載の方法。
- 前記反応剤を使用箇所の発生器によりその場で生成する、請求項13記載の方法。
- 前記物質を不活性ガス希釈剤で希釈した前記反応剤と接触させる、請求項13記載の方法。
- 前記反応剤を非反応性の支持材上に被着させる、請求項13記載の方法。
- 前記反応剤を1以上のエネルギー源に暴露し、この暴露工程を前記導入する工程の前に行う、請求項13記載の方法。
- 前記反応剤を1以上のエネルギー源に暴露し、この暴露工程を前記導入する工程の少なくとも一部分の間に行う、請求項13記載の方法。
- 前記暴露工程の温度が少なくとも150℃である、請求項13記載の方法。
- 前記暴露工程の圧力が少なくとも10mTorrである、請求項13記載の方法。
- 前記反応剤がハロゲン含有化合物の混合物を含む、請求項13記載の方法。
- 前記混合物が少なくとも1種の塩素含有ガスと50体積%未満の少なくとも1種のを含む、請求項13記載の方法。
- 反応器の少なくとも1つの表面から物質を除去するための装置であって、
ハロゲン含有化合物、ホウ素含有化合物、炭素含有化合物、水素含有化合物、窒素含有化合物、キレート化用化合物、クロロシラン化合物、ヒドロクロロシラン化合物、又はオルガノクロロシラン化合物からなる群より選ばれる少なくとも1種の反応剤、及び、
当該少なくとも1種の反応剤が被着した非反応性支持材、
を含む、反応器表面からの物質除去装置。 - 反応器の少なくとも1つの表面から物質を除去するための混合物であって、
ハロゲン含有化合物、ホウ素含有化合物、炭素含有化合物、水素含有化合物、窒素含有化合物、キレート化用化合物、クロロシラン化合物、ヒドロクロロシラン化合物、又はオルガノクロロシラン化合物からなる群より選ばれる少なくとも1種の反応剤、及び、
不活性希釈剤、
を含む混合物。 - 基材の少なくとも1つの表面から物質を除去するための方法であって、
遷移金属酸化物、遷移金属ケイ酸塩、Al2O3以外の13族金属酸化物、13族金属ケイ酸塩、窒素を含有する13族金属酸化物、窒素を含有する13族金属ケイ酸塩、窒素を含有する遷移金属酸化物、窒素を含有する遷移金属ケイ酸塩からなる群より選ばれる少なくとも1種のもの、あるいは、遷移金属酸化物、遷移金属ケイ酸塩、13族金属酸化物、13族金属ケイ酸塩、窒素を含有する13族金属酸化物、窒素を含有する13族金属ケイ酸塩、窒素を含有する遷移金属酸化物、又は窒素を含有する遷移金属ケイ酸塩からなる群のうちの少なくとも1つの層を含む積層体である物質の膜で少なくとも部分的に被覆された基材であり、当該物質が二酸化ケイ素の誘電率より大きい誘電率を有する基材を用意すること、
当該物質を、ハロゲン含有化合物、ホウ素含有化合物、炭素含有化合物、水素含有化合物、窒素含有化合物、キレート化用化合物、クロロシラン化合物、ヒドロクロロシラン化合物、又はオルガノクロロシラン化合物からなる群からの少なくとも1種のものを含む反応剤と反応させて、揮発性生成物を生成すること、
そして当該基材から当該揮発性生成物を除去し、それにより当該基材から当該物質を除去すること、
を含む、基材表面からの物質除去方法。 - 前記物質が、HfO2、ZrO2、HfSixOy、ZrSixOy(これらの式中のxは0より大きく、yは2x+2である)、Al2SiwOz(この式のwは0より大きく、zは2w+3である)からなる群、又は窒素を含有する前述の化合物のいずれかより選ばれる少なくとも1種のものである、請求項26記載の方法。
- 前記物質が、遷移金属酸化物、遷移金属ケイ酸塩、13族金属酸化物、13族金属ケイ酸塩、窒素を含有する遷移金属酸化物、窒素を含有する遷移金属ケイ酸塩、窒素を含有する13族金属酸化物、又は窒素を含有する13族金属ケイ酸塩からなる群より選ばれる少なくとも1種の材料の層を含む積層体である、請求項26記載の方法。
- 前記反応剤が、BCl3、COCl2、HCl、Cl2、ClF3、NF3、F2、及びNFzCl3-z(この式のzは0〜2の整数である)からなる群より選ばれる少なくとも1つのものである、請求項26記載の方法。
- 前記物質が、HfO2、ZrO2、HfSixOy、ZrSixOy(これらの式中のxは0より大きく、yは2x+2である)、Al2SiwOz(この式のwは0より大きく、zは2w+3である)からなる群、又は窒素を含有する前述の化合物のいずれかより選ばれる少なくとも1つのものである、請求項26記載の方法。
- 反応器表面から物質を除去するための方法であって、
当該反応器表面を有する反応器を準備し、ここにおいて、(a)当該反応器表面は当該物質の膜で少なくとも部分的に被覆されており、(b)当該物質は、遷移金属酸化物、遷移金属ケイ酸塩、13族金属酸化物、13族金属ケイ酸塩、窒素を含有する13族金属酸化物、窒素を含有する13族金属ケイ酸塩、窒素を含有する遷移金属酸化物、窒素を含有する遷移金属ケイ酸塩からなる群より選ばれる少なくとも1種のもの、あるいは、遷移金属酸化物、遷移金属ケイ酸塩、13族金属酸化物、13族金属ケイ酸塩、窒素を含有する遷移金属酸化物、窒素を含有する遷移金属ケイ酸塩、窒素を含有する13族金属酸化物、又は窒素を含有する13族金属ケイ酸塩からなる群より選ばれる少なくとも1つの層を含む積層体であり、そして(c)当該物質は二酸化ケイ素の誘電率よりも大きい誘電率を有すること、
当該物質を、少なくとも1種のフッ素含有化合物と、塩素含有化合物、臭素含有化合物、又はヨウ素含有化合物から選ばれる少なくとも1種とを含む反応剤であって、当該フッ素含有化合物が当該反応剤の量の50体積%未満である反応剤と反応させること、
そして当該反応器から揮発性生成物を除去して、それにより当該表面から当該物質を除去すること、
を含む、反応器表面からの物質除去方法。
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Also Published As
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US20040129671A1 (en) | 2004-07-08 |
CN100372055C (zh) | 2008-02-27 |
TW200518178A (en) | 2005-06-01 |
KR20050050579A (ko) | 2005-05-31 |
SG112101A1 (en) | 2005-06-29 |
SG135203A1 (en) | 2007-09-28 |
CN1638028A (zh) | 2005-07-13 |
EP1538235A1 (en) | 2005-06-08 |
KR100667723B1 (ko) | 2007-01-15 |
US7357138B2 (en) | 2008-04-15 |
TWI267898B (en) | 2006-12-01 |
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