JP7161192B2 - 積層コーティング層、積層コーティング層を形成する方法及び積層構造の判定方法 - Google Patents
積層コーティング層、積層コーティング層を形成する方法及び積層構造の判定方法 Download PDFInfo
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- JP7161192B2 JP7161192B2 JP2018235833A JP2018235833A JP7161192B2 JP 7161192 B2 JP7161192 B2 JP 7161192B2 JP 2018235833 A JP2018235833 A JP 2018235833A JP 2018235833 A JP2018235833 A JP 2018235833A JP 7161192 B2 JP7161192 B2 JP 7161192B2
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- alumina
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- 238000000034 method Methods 0.000 title claims description 62
- 239000011247 coating layer Substances 0.000 title claims description 33
- 239000010410 layer Substances 0.000 claims description 157
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- 229910044991 metal oxide Inorganic materials 0.000 claims description 29
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- 239000011347 resin Substances 0.000 claims description 23
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 23
- 238000000231 atomic layer deposition Methods 0.000 claims description 22
- 125000002524 organometallic group Chemical group 0.000 claims description 21
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- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 claims description 10
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
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- 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
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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
- C23C16/44—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 method of coating
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- C23C16/45523—Pulsed gas flow or change of composition over time
- C23C16/45525—Atomic layer deposition [ALD]
- C23C16/45527—Atomic layer deposition [ALD] characterized by the ALD cycle, e.g. different flows or temperatures during half-reactions, unusual pulsing sequence, use of precursor mixtures or auxiliary reactants or activations
- C23C16/45529—Atomic layer deposition [ALD] characterized by the ALD cycle, e.g. different flows or temperatures during half-reactions, unusual pulsing sequence, use of precursor mixtures or auxiliary reactants or activations specially adapted for making a layer stack of alternating different compositions or gradient compositions
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Description
また、前記処理対象物の表面が非平坦表面であり、前記密着層が、前記樹脂膜からなる、ことが好ましい。
また、前記防湿層が、50nm以下の膜厚のアルミナ膜の単一層であるか、又は50nm以下の膜厚のアルミナ膜と歪緩和膜とを交互に多層積層した構造を含む、ことが好ましい。
また、前記歪緩和膜が、III属ではない金属の酸化物を含有する膜、又は不純物として炭素を含有する膜、又は樹脂膜である、ことが好ましい。
(1)前記有機金属ガス導入手段により、前記被処理対象物に前記有機金属ガスを導入する工程と、
(2)前記排気手段により、前記被処理対象物周囲の有機金属ガスを排気する工程と、
(3)前記励起加湿ガス導入手段により、前記被処理対象物に前記励起された加湿ガスを導入する工程と、
(4)前記排気手段により、前記被処理対象物周囲の加湿ガスを排気する工程と、
を実行し、(1)~(4)の工程を繰り返すことで、前記金属酸化膜を形成する、
積層コーティング層を形成する方法にある。
(1)前記有機金属ガス導入手段により、前記処理容器内に前記有機金属ガスを導入する工程と、
(2)前記排気手段により、前記処理容器内の有機金属ガスを排気する工程と、
(3)前記加湿ガス導入手段により、前記処理容器内に前記励起された加湿ガスを導入する工程と、
(4)前記排気手段により、前記処理容器内の加湿ガスを排気する工程と、
を実行し、(1)~(4)の工程を繰り返すことで、前記被処理対象物の表面に酸化膜を形成するものである。
する上で、波長λiは300nm~800nmの範囲とし、隣り合う波長の間隔は1nmとしている(波長の総数はM=501となる)。この合致度を示すφをつかって、経験的に閾値を決め、コピーを判定する。ここではその閾値を3.5°未満、できれば2.0°とする。この閾値は、発明者の調査により、3層膜の内の任意の2層を入れ替えた場合、合致度関数が3.5°より大きくなることを経験的に見いだしており、3.5°以下にすることで膜が入れ替わった時の不良が検出できることによる。また、2°という数値は安全係数を考えて、2°と設定した。
本発明に係るコーティング膜の構造と実施方法を示す。
本実施例として、基材1としてのステンレス板(SUS430材)にコーティング膜を形成した事例を図2に示す。このとき、コーティング膜の積層において室温原子層堆積法を活用した。
実施例1の比較例として、基材1のステンレス材(SUS430)に、直接、アルミナを20nmで室温原子層堆積法で形成した事例のTEM写真を図3に示す。膜の製造方法は実施例1と同じである。膜厚は実施例1より少ない20nmであるが、アルミナ膜の応力で、膜の浮き上がりが観測され、剥がれが起きていることが分かる。
アルミニウム金属を基材として用い、アルミナ層とアルミナ炭素含有と層の交互積層を、室温原子層堆積法により、総膜厚70nmで形成した。この場合の密着層は、数nmの自然酸化により形成された酸化アルミニウムである。アルミナ層とアルミナ炭素含有層との交互積層において、アルミナ層とアルミナ炭素含有層とはそれぞれ4nm、2nmであり、層の数もそれぞれ12とした。
アルミナ層とアルミナ炭素含有層との交互積層の代わりに、アルミナ単層膜とした以外は、実施例2と同様に実施した。アルミナ層は単層で、約70nmの膜とした。
実施例2及び比較例2のサンプルを、質量パーセント濃度35%の濃塩酸中に、温度22℃で浸漬させたときの腐食の度合いを評価した。この結果は、図4に示す。
基材として亜鉛メッキ板を用い、これに密着層としてPMMA(アクリル樹脂膜)を形成し、この上に、実施例1と同様に、アルミナを主成分とする防湿層を形成した。
密着層としてPMMA(アクリル樹脂膜)を形成しない以外は、実施例3と同様に実施した。
実施例3及び比較例3のサンプルについて、質量パーセント濃度35%の濃塩酸60秒浸漬による腐食の度合いを調べた。この結果は、図5に示す。
実施例3では、腐食はほとんど見られなかったが、比較例3では、腐食が観察された。
本実施例では、基材としてステンレス材(SUS304)を用い、密着層として酸化膜を形成した後、単純アルミナ層15nmを室温原子層堆積法で形成し、その後、PMMA樹脂層を歪緩和層として3μmの厚さで形成し、その上に単純アルミナ層15nmを室温原子層堆積法で形成し、防湿層とした。
密着層としてPMMA樹脂層を設けない以外は、実施例4と同様に実施した。
実施例4及び比較例4のサンプルについて、質量パーセント濃度35%の濃塩酸20分浸漬による腐食の度合いを調べた。この結果は、図6に示す。
本実施例は、基材としてステンレス材(SUS304)を用い、単純アルミナ層を30nm形成して、その上に防水層である酸化ニオブ(Nb2O5)を5nmで形成した積層コーティング層とした。密着層は、SUS304の自然酸化層である。
防水層として酸化ニオブ(Nb2O5)層を設けない以外は、実施例5と同様に実施した。
実施例5及び比較例5のサンプルについて、質量パーセント濃度35%の濃塩酸30分浸漬による腐食の度合いを調べた。この結果は、図7に示す。
金属基材である鉄の上に、密着層としてTiO2を4nm、その上に防湿層のアルミナが10から100nmであり、さらに防水層としてSiO2層を6.5nmである膜構造を検査した。
2 密着層
3 防湿層
4 防水層
Claims (7)
- 表面が親水性表面である 被処理対象物上に低温原子層堆積膜で構成された金属酸化膜を含むコーティング層であり、前記コーティング層において被処理対象物の表面から密着層、防湿層、及び防水層の少なくとも2層を少なくとも1組具備し、
前記密着層は、シリカ膜からなり、
前記防湿層は、アルミナを主成分とする膜であり、
前記防水層は、シリカ膜、酸化ニオブ膜及び酸化ジルコニウム膜から選択される金属酸化膜、及び樹脂膜の少なくとも1種の膜からなる、
積層コーティング層。 - 表面が非平坦表面である被処理対象物上に低温原子層堆積膜で構成された金属酸化膜を含むコーティング層であり、前記コーティング層において被処理対象物の表面から密着層、防湿層、及び防水層の少なくとも2層を少なくとも1組具備し、
前記密着層は、樹脂膜からなり、
前記防湿層は、アルミナを主成分とする膜であり、
前記防水層は、シリカ膜、酸化ニオブ膜及び酸化ジルコニウム膜から選択される金属酸化膜、及び樹脂膜の少なくとも1種の膜からなる、
積層コーティング層。 - 請求項1又は2において、前記防湿層が、50nm以下の膜厚のアルミナ膜の単一層であるか、又は50nm以下の膜厚のアルミナ膜と歪緩和膜とを交互に多層積層した構造を含む、
積層コーティング層。 - 被処理対象物上に低温原子層堆積膜で構成された金属酸化膜を含むコーティング層であり、前記コーティング層において被処理対象物の表面から密着層、防湿層、及び防水層の少なくとも2層を少なくとも1組具備し、
前記密着層は、金属酸化膜、及び樹脂膜から選択される少なくとも1種の膜からなり、
前記防湿層は、アルミナを主成分とする膜であり、且つ50nm以下の膜厚のアルミナ膜の単一層であるか、又は50nm以下の膜厚のアルミナ膜と歪緩和膜とを交互に多層積層した構造を含むものであり、
前記防水層は、シリカ膜、酸化ニオブ膜及び酸化ジルコニウム膜から選択される金属酸化膜、及び樹脂膜の少なくとも1種の膜からなる、
積層コーティング層。 - 請求項3又は4において、前記歪緩和膜が、III属ではない金属の酸化物を含有する膜、又は不純物として炭素を含有する膜、又は樹脂膜である、
積層コーティング層。 - 請求項1~5の何れか一項に記載の積層コーティング層を形成する方法であって、
被処理対象物を格納できる処理容器を備える真空容器を用意し、前記処理容器内のガスを排気できる排気手段と、前記処理容器内に有機金属ガスを導入して充満させる有機金属ガス導入手段と、前記処理容器内に励起された加湿ガスを導入して充満させる加湿ガス導入手段とを前記真空容器に連結し、
(1)前記有機金属ガス導入手段により、前記被処理対象物に前記有機金属ガスを導入する工程と、
(2)前記排気手段により、前記被処理対象物周囲の有機金属ガスを排気する工程と、
(3)前記加湿ガス導入手段により、前記被処理対象物に前記励起された加湿ガスを導入する工程と、
(4)前記排気手段により、前記被処理対象物周囲の加湿ガスを排気する工程と、
を実行し、(1)~(4)の工程を繰り返すことで、前記金属酸化膜を形成する、
積層コーティング層を形成する方法。 - 請求項1~5の何れか一項に記載の積層コーティング層が設けられた基材に、S偏光の光とP偏光の光を同振幅で、表面に対して照射し、得られた反射光において、S偏光の反射光とP偏光の反射光の強度比をtanΨとし、S偏光の反射光とP偏光の反射光の位相差をΔとし、これらのΨとΔを300~800nmの範囲で実測して、Ψ1とΔ1とし、想定した積層構造に基づいて、前記防湿層の膜厚を変数dAとして、マトリクス法によりΨ2とΔ2の理論値を300~800nmの範囲で計算し、実測値と計算値の合致度を評価する関数として、次の関数φを定義し、
積層構造の判定方法。
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US10882275B2 (en) * | 2012-11-29 | 2021-01-05 | Lg Chem, Ltd. | Gas barrier film with protective coating layer containing inorganic particles |
TWI549823B (zh) * | 2013-03-29 | 2016-09-21 | 財團法人工業技術研究院 | 複合膜及其製造方法 |
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JP2011018707A (ja) | 2009-07-07 | 2011-01-27 | Hitachi Kokusai Electric Inc | 半導体装置の製造方法及び基板処理装置 |
WO2011111586A1 (ja) | 2010-03-12 | 2011-09-15 | 旭硝子株式会社 | 積層体およびその製造方法 |
JP2015166170A (ja) | 2014-03-04 | 2015-09-24 | 東洋製罐グループホールディングス株式会社 | ガスバリア性積層体 |
JP2018506859A (ja) | 2015-02-13 | 2018-03-08 | インテグリス・インコーポレーテッド | 基材物品および装置の特性および性能を増強するためのコーティング |
WO2017057775A1 (ja) | 2015-10-02 | 2017-04-06 | 国立大学法人山形大学 | 内面コーティング方法及び装置 |
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