JP4982659B2 - シリカ質膜の製造法およびそれにより製造されたシリカ質膜付き基板 - Google Patents
シリカ質膜の製造法およびそれにより製造されたシリカ質膜付き基板 Download PDFInfo
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- JP4982659B2 JP4982659B2 JP2007554912A JP2007554912A JP4982659B2 JP 4982659 B2 JP4982659 B2 JP 4982659B2 JP 2007554912 A JP2007554912 A JP 2007554912A JP 2007554912 A JP2007554912 A JP 2007554912A JP 4982659 B2 JP4982659 B2 JP 4982659B2
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- film
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- siliceous
- polysilazane
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- 238000004519 manufacturing process Methods 0.000 title claims description 18
- 238000000034 method Methods 0.000 claims description 90
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 78
- 229920001709 polysilazane Polymers 0.000 claims description 68
- 239000001257 hydrogen Substances 0.000 claims description 49
- 229910052739 hydrogen Inorganic materials 0.000 claims description 49
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 45
- 239000000377 silicon dioxide Substances 0.000 claims description 39
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- 229910052710 silicon Inorganic materials 0.000 claims description 24
- 239000010703 silicon Substances 0.000 claims description 24
- 238000010438 heat treatment Methods 0.000 claims description 23
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 22
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- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 3
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- 238000003756 stirring Methods 0.000 description 3
- FYGHSUNMUKGBRK-UHFFFAOYSA-N 1,2,3-trimethylbenzene Chemical compound CC1=CC=CC(C)=C1C FYGHSUNMUKGBRK-UHFFFAOYSA-N 0.000 description 2
- KVNYFPKFSJIPBJ-UHFFFAOYSA-N 1,2-diethylbenzene Chemical compound CCC1=CC=CC=C1CC KVNYFPKFSJIPBJ-UHFFFAOYSA-N 0.000 description 2
- DURPTKYDGMDSBL-UHFFFAOYSA-N 1-butoxybutane Chemical compound CCCCOCCCC DURPTKYDGMDSBL-UHFFFAOYSA-N 0.000 description 2
- AFABGHUZZDYHJO-UHFFFAOYSA-N 2-Methylpentane Chemical compound CCCC(C)C AFABGHUZZDYHJO-UHFFFAOYSA-N 0.000 description 2
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- RDOXTESZEPMUJZ-UHFFFAOYSA-N anisole Chemical compound COC1=CC=CC=C1 RDOXTESZEPMUJZ-UHFFFAOYSA-N 0.000 description 2
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- 238000009835 boiling Methods 0.000 description 2
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- 125000004122 cyclic group Chemical group 0.000 description 2
- HGCIXCUEYOPUTN-UHFFFAOYSA-N cyclohexene Chemical compound C1CCC=CC1 HGCIXCUEYOPUTN-UHFFFAOYSA-N 0.000 description 2
- NNBZCPXTIHJBJL-UHFFFAOYSA-N decalin Chemical compound C1CCCC2CCCCC21 NNBZCPXTIHJBJL-UHFFFAOYSA-N 0.000 description 2
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- 230000008021 deposition Effects 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- MROCJMGDEKINLD-UHFFFAOYSA-N dichlorosilane Chemical compound Cl[SiH2]Cl MROCJMGDEKINLD-UHFFFAOYSA-N 0.000 description 2
- IIEWJVIFRVWJOD-UHFFFAOYSA-N ethylcyclohexane Chemical compound CCC1CCCCC1 IIEWJVIFRVWJOD-UHFFFAOYSA-N 0.000 description 2
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- UAEPNZWRGJTJPN-UHFFFAOYSA-N methylcyclohexane Chemical compound CC1CCCCC1 UAEPNZWRGJTJPN-UHFFFAOYSA-N 0.000 description 2
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- BKIMMITUMNQMOS-UHFFFAOYSA-N nonane Chemical compound CCCCCCCCC BKIMMITUMNQMOS-UHFFFAOYSA-N 0.000 description 2
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- CFJYNSNXFXLKNS-UHFFFAOYSA-N p-menthane Chemical compound CC(C)C1CCC(C)CC1 CFJYNSNXFXLKNS-UHFFFAOYSA-N 0.000 description 2
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- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/70—Manufacture or treatment of devices consisting of a plurality of solid state components formed in or on a common substrate or of parts thereof; Manufacture of integrated circuit devices or of parts thereof
- H01L21/71—Manufacture of specific parts of devices defined in group H01L21/70
- H01L21/76—Making of isolation regions between components
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- H—ELECTRICITY
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- H01L21/70—Manufacture or treatment of devices consisting of a plurality of solid state components formed in or on a common substrate or of parts thereof; Manufacture of integrated circuit devices or of parts thereof
- H01L21/71—Manufacture of specific parts of devices defined in group H01L21/70
- H01L21/76—Making of isolation regions between components
- H01L21/762—Dielectric regions, e.g. EPIC dielectric isolation, LOCOS; Trench refilling techniques, SOI technology, use of channel stoppers
- H01L21/76224—Dielectric regions, e.g. EPIC dielectric isolation, LOCOS; Trench refilling techniques, SOI technology, use of channel stoppers using trench refilling with dielectric materials
- H01L21/76227—Dielectric regions, e.g. EPIC dielectric isolation, LOCOS; Trench refilling techniques, SOI technology, use of channel stoppers using trench refilling with dielectric materials the dielectric materials being obtained by full chemical transformation of non-dielectric materials, such as polycristalline silicon, metals
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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
- C23C16/22—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
- C23C16/40—Oxides
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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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- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
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- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
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- H01L21/02164—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 the material containing silicon the material being a silicon oxide, e.g. SiO2
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- H01L21/02219—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 the layer being characterised by the precursor material for deposition the precursor containing a compound comprising Si the compound comprising silicon and nitrogen
- H01L21/02222—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 the layer being characterised by the precursor material for deposition the precursor containing a compound comprising Si the compound comprising silicon and nitrogen the compound being a silazane
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- H01L21/02296—Forming insulating materials on a substrate characterised by the treatment performed before or after the formation of the layer
- H01L21/02299—Forming insulating materials on a substrate characterised by the treatment performed before or after the formation of the layer pre-treatment
- H01L21/02304—Forming insulating materials on a substrate characterised by the treatment performed before or after the formation of the layer pre-treatment formation of intermediate layers, e.g. buffer layers, layers to improve adhesion, lattice match or diffusion barriers
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- H—ELECTRICITY
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- H01L21/02318—Forming insulating materials on a substrate characterised by the treatment performed before or after the formation of the layer post-treatment
- H01L21/02337—Forming insulating materials on a substrate characterised by the treatment performed before or after the formation of the layer post-treatment treatment by exposure to a gas or vapour
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- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
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Description
凹凸を有するシリコン基板の表面上に、二次イオン質量分析により測定される水素含有量が9×1020atms/cm3以上である絶縁膜を形成させる絶縁膜形成工程、
前記基板にポリシラザン化合物を含んでなる組成物を塗布する塗布工程、および
塗布済み基板を加熱処理してポリシラザン化合物を二酸化シリコン膜に転化させる硬化工程
を含んでなることを特徴とするものである。
また、本発明によるシリカ質膜付き基板は、前記の方法により形成されたシリカ質膜を具備してなることを特徴とするものである。
2 窒化ケイ素膜
3 絶縁膜
4 ポリシラザン塗膜
5 絶縁膜を含む溝付き基板
6 シリカ質膜
本発明によるシリカ質膜の製造法によれば、凹凸のあるシリコン基板上に、ボイドがなく、膜質も均質な被膜を形成することができる。したがって、電子デバイスのトランジスター部やキャパシター部の平坦化絶縁膜(プリメタル絶縁膜)として形成することも、また溝付きシリコン基板上にシリカ質膜を形成させて溝を埋封することによって、トレンチ・アイソレーション構造を形成することもできる。以下、トレンチ・アイソレーション構造を形成させる方法に基づいて本発明を説明する。
凹凸を有するシリコン基板の表面上に、二次イオン質量分析(以下、SIMS分析といいます)により測定される水素含有量が9×1020atms/cm3以上である絶縁膜を形成させる絶縁膜形成工程、
前記基板にポリシラザン化合物を含んでなる組成物を塗布する塗布工程、および
塗布済み基板を加熱処理してポリシラザン化合物を二酸化シリコン膜に転化させる硬化工程。
本発明による方法において、絶縁膜形成工程に先立ち、凹凸を有するシリコン基板を準備する。特にトレンチ・アイソレーション構造を形成させる場合には所望の溝パターンを有するシリコン基板を準備する。この溝形成には、任意の方法を用いることができ、例えば特許文献1または2にも記載されている。具体的な方法は、以下に示すとおりである。
測定装置: Physical Electronics社製 6600
一次イオン種: Cs+
一次加速電圧: 5.0kV
検出領域: 120μm×192μm
次に、前記した絶縁膜形成工程により絶縁膜に溝が形成されたシリコン基板上にシリカ質膜の材料となるポリシラザン化合物を含む組成物の塗膜を形成させる。
ポリシラザン組成物を塗布した後、必要に応じてプリベーク工程(詳細後述)に付した後、ポリシラザン塗膜をシリカ質膜に転化させて硬化させるために、基板全体を加熱する。通常は、基板全体を硬化炉などに投入して加熱するのが一般的である。
ポリシラザン溶液が塗布された基板を、硬化工程に先立っては、プリベーク処理をすることができる。この工程では、ポリシラザン塗膜中に含まれる溶媒の完全除去と、ポリシラザン塗膜の予備硬化を目的とするものである。特にポリシラザンを用いる本発明のトレンチ・アイソレーション構造の形成方法においては、プリベーク処理をすることにより、シリカ質膜の緻密性が向上するので、プリベーク工程を組み合わせることが好ましい。
硬化させた後、硬化した二酸化シリコン膜の不要な部分は除去することが好ましい。そのために、まず研磨工程により、基板表面にあるポリシラザン塗膜を研磨により除去する。この工程が研磨工程である。この研磨工程は、硬化処理の後に行うほか、プリベーク工程を組み合わせる場合には、プリベーク直後に行うこともできる。
前記の研磨工程において、基板表面の、ポリシラザンに由来するシリカ質膜はほとんど除去されるが、残存しているシリカ質膜を除去するために、さらにエッチング処理を行うことが好ましい。エッチング処理はエッチング液を用いるのが一般的であり、エッチング液としては、シリカ質膜を除去できるものであれば特に限定されないが、通常はフッ化アンモニウムを含有するフッ酸水溶液を用いる。この水溶液のフッ化アンモニウム濃度は5%以上であることが好ましく、30%以上であることがより好ましい。
本発明によるシリカ質膜付き基材は、前記したトレンチ・アイソレーション構造の形成方法を例に説明したシリカ質膜の製造法により製造されたものである。このようなシリカ質膜付き基板は、シリカ質膜の膜質がいたるところで均一であるため、機械的な強度も均一であり、またエッチングや研磨などの加工を行った際にも均一性および平坦性が保たれ、優れた最終製品を得ることができる。
以下、本発明をSTI(シャロートレンチアイソレーション)構造の素子分離溝の埋込み技術を想定した実施例について、図1を参照しながら説明する。
これにより、図1に示すような構成のサンプルが形成された。
実施例1と同様の構成のサンプルにおいて、図1に示されるプラズマTEOS膜の代わりにプラズマ化学気相成長法(PE−CVD)による窒化ケイ素膜を20nm堆積させた。
上記PE−CVD技術を用いて窒化膜ケイ素膜3を形成する際の成膜条件は、次の通りである。即ち、SiH4/NH3ガス流量およびソースバワー/バイアスバワーの条件を、SiH4/NH3=55/110sccm、SRF/BRF=4400/2600W、基板温度を400℃とした。
ボリシラザン溶液の製膜および熱処理は実施例1と同一条件にて行った。
実施例1と同様の構成のサンプルにおいて、図1に示されるプラズマTEOS膜の代わりに低圧CVD法により形成した窒化ケイ素膜(LP−CVD窒化ケイ素膜)を20nm堆積させた。
ポリシラザン溶液の製膜および加熱処理は実施例1と同一条件にて行った。
実施例1と同様にプラズマTEOS技術を用いて二酸化ケイ素膜3を20nm堆積させた後、ここまでの構成のサンプルを一度、窒素雰囲気中700℃でアニーリングした。上記アニーリングを行った後のプラズマTEOS膜は水素含有量の少ない膜であり、このことはベタ膜のSIMS分析ならびにTDS分析によって確認された。即ち、SIMS分析によれば膜中におよそ8×1020atms/cm3の水素を含み、TDS分析によれば真空中700℃までの条件下でも、吸着水分が放出されることを除き特にガスの放出は認められず、放出され得る水素を含んでいなかった。
アニーリング処理によってプラズマTEOSの成膜時に多量に含まれていた水素が放出されたと考えられる。ポリシラザン溶液の製膜および熱処理は実施例1と同一条件にて行った。
実施例1 1.447
実施例2 1.448
比較例1 1.445
参考例1 1.444
この結果により、全てのサンプルのポリシラザン塗膜4は二酸化ケイ素膜になっていることが確認された。
実施例1と同様の構成のサンプルにおいて、実施例1に示されるプラズマTEOS膜の代わりにSiH4およびO2をソースとしたプラズマ化学気相成長法による二酸化ケイ素膜を20nm堆積させた。
上記二酸化ケイ素膜3を形成する際の成膜条件は、次の通りである。即ち、SiH4/O2ガス流量およびソースバワー/バイアスバワーの条件を、SiH4/O2=50/100sccm、SRF/BRF=4500/3000W、基板温度を250℃とした。
実施例1と同様の構成のサンプルにおいて、図1に示されるプラズマTEOS膜の代わりにSiH4およびO2をソースとした低圧化学気相成長法による二酸化ケイ素膜を20nm堆積させた。
上記二酸化ケイ素膜3を形成する際の成膜条件は、次の通りである。即ち、SiH4/O2ガス流量の条件を、SiH4/O2=50/100sccm、基板温度を700℃、圧力を1Torrとした。
ボリシラザン溶液の製膜および熱処理は実施例1と同一条件にて行った。
実施例1と同様の構成のサンプルにおいて、実施例1に示されるプラズマTEOS膜の代わりにTEOSおよびO2をソースとした低圧化学気相成長法による二酸化ケイ素膜を20nm堆積させた。
上記二酸化ケイ素膜3を形成する際の成膜条件は、次の通りである。即ち、TEOS/O2ガス流量の条件を、TEOS/O2=50/100sccm、基板温度を700℃、圧力を1Torrとした。
ボリシラザン溶液の製膜および熱処理は実施例1と同一条件にて行った。
実施例1と同様の構成のサンプルにおいて、実施例1に示されるプラズマTEOS膜の代わりにSiH4およびN2Oをソースとしたラピッドサーマル蒸着法による二酸化ケイ素膜を20nm堆積させた。
上記二酸化ケイ素膜3を形成する際の成膜条件は、次の通りである。即ち、SiH4/N2Oガス流量の条件を、SiH4/N2O=10/250sccm、基板温度を800℃とした。
ボリシラザン溶液の製膜および熱処理は実施例1と同一条件にて行った。
まず、溝の長手方向に対して垂直な方向で基板を切断し、断面の溝部分を日立製作所製モデルS−4600のSEMにて倍率100,000倍で断面に垂直な方向から観察し、図2(エッチング前)に示す絶縁膜を含む溝付き基板5からシリカ質膜6表面までの長さ(a)を測定する。
微細溝内部のエッチングレート(A)および溝外部のエッチングレート(B)をそれぞれ得られた(a)、(b)、および(c)を用いて以下の方法によって計算して求めた。
(A)=(c)
(B)=(a)−(b)
以上の方法によって測定した結果は表1に示す通りであった。
Claims (8)
- 凹凸を有するシリコン基板の表面上に、二次イオン質量分析により測定される水素含有量が9×1020atms/cm3以上である絶縁膜を形成させる絶縁膜形成工程、
前記絶縁膜が形成された後、前記基板にポリシラザン化合物を含んでなる組成物を塗布する塗布工程、および
塗布済み基板を加熱処理してポリシラザン化合物を二酸化シリコン膜に転化させる硬化工程
を含んでなることを特徴とする、シリカ質膜の製造法。 - 絶縁膜がテトラエトキシシランを用いたプラズマ化学気相成長法により形成される二酸化ケイ素膜である、請求項1に記載のシリカ質膜の製造法。
- 絶縁膜がプラズマ化学気相成長法により形成される窒化ケイ素膜である、請求項1に記載のシリカ質膜の製造法。
- 加熱処理を水蒸気濃度1%以上の不活性ガスまたは酸素雰囲気下で行う、請求項1〜3のいずれか1項に記載のシリカ質膜の製造法。
- 加熱処理における加熱温度が400℃以上1,200℃以下である、請求項1〜4のいずれか1項に記載のシリカ質膜の製造法。
- 絶縁膜の厚さが、1〜100nmである、請求項1〜5のいずれか1項に記載のシリカ質膜の製造法。
- 凹凸を有するシリコン基板がトレンチ・アイソレーション構造形成用の溝付き基板であり、請求項1〜6に記載の方法により前記溝を埋封する、トレンチ・アイソレーション構造の形成法。
- 請求項7に記載の方法により形成されたトレンチ・アイソレーション構造を有することを特徴とする基板。
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JP4607613B2 (ja) * | 2005-02-09 | 2011-01-05 | 株式会社東芝 | 半導体装置の製造方法 |
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JPH1079382A (ja) * | 1996-09-05 | 1998-03-24 | Hitachi Ltd | Si−F結合を有するSiO2膜の成膜方法および半導体装置 |
JPH1187332A (ja) * | 1997-09-02 | 1999-03-30 | Nec Corp | 半導体装置及びその製造方法 |
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KR102021571B1 (ko) * | 2018-05-14 | 2019-09-16 | 재단법인대구경북과학기술원 | 산소 제거를 위한 전처리를 수행한 유연 기판을 포함하는 유연 박막 태양전지 및 이의 제조방법 |
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JPWO2007083654A1 (ja) | 2009-06-11 |
EP1978548A4 (en) | 2011-11-23 |
KR101352816B1 (ko) | 2014-01-20 |
TWI389250B (zh) | 2013-03-11 |
US20090278223A1 (en) | 2009-11-12 |
CN101366103A (zh) | 2009-02-11 |
WO2007083654A8 (ja) | 2008-03-27 |
EP1978548A1 (en) | 2008-10-08 |
TW200739804A (en) | 2007-10-16 |
CN101366103B (zh) | 2010-06-02 |
EP1978548B1 (en) | 2013-09-11 |
KR20080094055A (ko) | 2008-10-22 |
WO2007083654A1 (ja) | 2007-07-26 |
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