JP2021512220A - 金属基板を処理するためのシステムおよび方法 - Google Patents
金属基板を処理するためのシステムおよび方法 Download PDFInfo
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- JP2021512220A JP2021512220A JP2020541552A JP2020541552A JP2021512220A JP 2021512220 A JP2021512220 A JP 2021512220A JP 2020541552 A JP2020541552 A JP 2020541552A JP 2020541552 A JP2020541552 A JP 2020541552A JP 2021512220 A JP2021512220 A JP 2021512220A
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Images
Classifications
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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
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
- C23C22/34—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing fluorides or complex fluorides
- C23C22/36—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing fluorides or complex fluorides containing also phosphates
- C23C22/361—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing fluorides or complex fluorides containing also phosphates containing titanium, zirconium or hafnium compounds
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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
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/73—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals characterised by the process
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- C—CHEMISTRY; METALLURGY
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Abstract
Description
本出願は、参照により本明細書に組み込まれる、「Systems and Methods for Treating a Metal Substrate」と題された2018年1月30日に出願された米国仮特許出願第62/623,735号に対する優先権を主張する。
本発明は、基板を処理するための組成物、システム、および方法に関する。本発明はまた、システムおよび方法による処理によって取得可能な基板に関する。
航空宇宙産業、商業産業、民間産業で使用される金属の酸化および劣化は深刻でコストのかかる問題である。これらの用途で使用される金属の酸化および劣化を防ぐために、金属表面に無機保護コーティングを塗布することができる。しかしながら、これらの組成物および方法を使用して調製されたコーティングの少なくともいくつかは、表面上に腐食および/またはピットを発生させる可能性がある。したがって、既知の変換コーティングの欠陥、欠点、および望ましくないパラメータのうちのいくつかを克服する変換組成物および/または処理システムが必要である。
本明細書には、三価クロムカチオンおよび水性担体を含む第1の組成物が開示される。
以下の詳細な説明のために、本発明は、反対に明示的に記載された場合を除き、様々な代替的な変形および工程順序を仮定し得ることを理解すべきである。さらに、任意の操作例以外に、または別段の指示がない限り、値、量、パーセンテージ、範囲、サブ範囲、および端数を表すものなどすべての数字は、用語が明示的に表示されていなくても、「約」という単語が前置きされているかのように読み取られ得る。したがって、特に異議を唱えない限り、以下の明細書および添付の特許請求の範囲に説明される数値パラメータは概算であり、本発明により得られるべき所望の特性に応じて変更してもよい。最低限でも、また特許請求の範囲の均等物の原則の適用を限定しようとするものではなく、各数値パラメータは少なくとも、報告された有効数字の数を考慮して、また通常の端数処理技術を適用することによって解釈されるべきである。クローズドエンドまたはオープンエンドの数値範囲が本明細書に記載されている場合、数値範囲内または数値範囲によって包含されるすべての数字、値、量、パーセンテージ、サブ範囲、および端数は、これらの数字、値、量、パーセンテージ、サブ範囲、および端数が、それらの全体が明示的に書き出されたかのように、本出願の元の開示に具体的に含まれ、かつそれに属するものと見なされるものとする。
態様1.第1の組成物であって、
組成物の総重量に基づいて、0.005g/L〜2g/Lの量の三価クロムカチオンと、
水性担体と、を含む、第1の組成物。
少なくとも一部、基板表面を、いずれかの態様1〜9に記載の組成物と接触させることを含む方法。
実施例で使用した材料:
過マンガン酸カリウム、ACS、99.0%(Alfa Aesar、CAS#7722−64−7、ロット#E02R022)
2Lのガラスビーカーおよび攪拌棒を脱イオン水ですすぎ、溶媒(MEK)で2回拭き取り、次に、きれいなペーパータオルで乾燥させた。ビーカーをAdventurer Pro AV8101計量スケール上に配置し、計量スケールをゼロにした。計量紙(4×4、12578−165)のVMP片を使用して、4.5028gの過マンガン酸カリウム、濃い紫色の固体を、Adventurer Pro AV264スケールを使用して計量し、ビーカーに移した。次に、ビーカーに1195.5gの脱イオン水を加えた。次に、ビーカーをCole−Parmer StableTemp Ceramic Stirrer(型番第03406−10)上に配置し、すべての固体が完全に溶解するまで中程度に溶液をゆっくりと攪拌した。
2Lのガラスビーカーおよび攪拌棒を脱イオン水ですすぎ、溶媒(MEK)で2回拭き取り、次に、きれいなペーパータオルで乾燥させた。ビーカーをAdventurer Pro AV8101計量スケール上に配置し、計量スケールをゼロにした。VWR5.0オンスの試料容器および使い捨てプラスチックピペットを使用して、0.1263gの硝酸セリウム(III)溶液を、Adventurer Pro AV264スケールを使用して計量し、ビーカーに移した。次に、ビーカーに600.0gの脱イオン水を加え、上述の攪拌プレート上でよく混合した。
2Lのガラスビーカーおよび攪拌棒を脱イオン水ですすぎ、溶媒(MEK)で2回拭き取り、次に、きれいなペーパータオルで乾燥させた。ビーカーをAdventurer Pro AV8101計量スケール上に配置し、計量スケールをゼロにした。VWR5.0オンスの試料容器および使い捨てプラスチックピペットを使用して、0.2124gの硝酸イットリウム(III)溶液を、Adventurer Pro AV264スケールを使用して計量し、ビーカーに移した。次に、ビーカーに500.0gの脱イオン水を加え、上述の攪拌プレート上でよく混合した。
2Lのガラスビーカーおよび攪拌棒を脱イオン水ですすぎ、溶媒(MEK)で2回拭き取り、次に、きれいなペーパータオルで乾燥させた。ビーカーをAdventurer Pro AV8101計量スケール上に配置し、計量スケールをゼロにした。計量紙(4×4、12578−165)のVMP片を使用して、10.0000gのクロム(III)硫酸カリウム十二水和物を、Adventurer Pro AV264スケールを使用して計量し、ビーカーに移した。次に、ビーカーに1590.0gの脱イオン水を加えた。次に、ビーカーを上述の攪拌プレート上に配置し、すべての固体が完全に溶解するまで中程度に溶液をゆっくりと攪拌した。
2Lのガラスビーカーおよび攪拌棒を脱イオン水ですすぎ、溶媒(MEK)で2回拭き取り、次に、きれいなペーパータオルで乾燥させた。ビーカーをAdventurer Pro AV8101計量スケール上に配置し、計量スケールをゼロにした。計量紙(4×4、12578−165)のVMP片を使用して、10.0070gの塩基性クロム(III)硫酸、濃い緑色の粉末を、Adventurer Pro AV264スケールを使用して計量し、ビーカーに移した。次に、ビーカーに1590.0gの脱イオン水を加えた。次に、ビーカーを上述の攪拌プレート上に配置し、すべての固体が完全に溶解するまで中程度に溶液をゆっくりと攪拌した。
2Lのガラスビーカーおよび攪拌棒を脱イオン水ですすぎ、溶媒(MEK)で2回拭き取り、次に、きれいなペーパータオルで乾燥させた。ビーカーをAdventurer Pro AV8101計量スケール上に配置し、計量スケールをゼロにした。計量紙(4×4、12578−165)のVMP片を使用して、9.0041gのヘキサフルオロジルコン酸カリウム、白色結晶化固体を、Adventurer Pro AV264スケールを使用して計量し、ビーカーに移した。次に、ビーカーに1191.0gの脱イオン水を加えた。次に、ビーカーを上述の攪拌プレート上に配置し、すべての固体が完全に溶解するまで中程度に溶液をゆっくりと攪拌した。
2Lのガラスビーカーおよび攪拌棒を脱イオン水ですすぎ、溶媒(MEK)で2回拭き取り、次に、きれいなペーパータオルで乾燥させた。ビーカーをAdventurer Pro AV8101計量スケール上に配置し、計量スケールをゼロにした。計量紙(4×4、12578−165)のVMP片を使用して、0.0427gのヘキサフルオロジルコン酸カリウム、白色結晶化固体を、Adventurer Pro AV264スケールによって計量し、ビーカーに移した。次に、ビーカーに800.0gの脱イオン水を加えた。次に、ビーカーを上述の攪拌プレート上に配置し、すべての固体が完全に溶解するまで中程度にゆっくりと攪拌した。ヘキサフルオロジルコン酸カリウムが完全に溶解した後、200.0gの過マンガン酸カリウム原液を同じビーカーに加え、よく混合した。
2Lのガラスビーカーおよび攪拌棒を脱イオン水ですすぎ、溶媒(MEK)で2回拭き取り、次に、きれいなペーパータオルで乾燥させた。ビーカーをAdventurer Pro AV8101計量スケール上に配置し、計量スケールをゼロにした。計量紙(4×4、12578−165)のVMP片を使用して、0.0422gの硫酸亜鉛七水和物、白色結晶化固体を、Adventurer Pro AV264スケールによって計量し、ビーカーに移した。次に、ビーカーに800.0gの脱イオン水を加えた。次に、ビーカーを上述の攪拌プレート上に配置し、すべての固体が完全に溶解するまで中程度にゆっくりと攪拌した。硫酸亜鉛七水和物が完全に溶解した後、200.0gの過マンガン酸カリウム原液を同じビーカーに加え、よく混合した。
2Lのガラスビーカーおよび攪拌棒を脱イオン水ですすぎ、溶媒(MEK)で2回拭き取り、次に、きれいなペーパータオルで乾燥させた。ビーカーをAdventurer Pro AV8101計量スケール上に配置し、計量スケールをゼロにした。計量紙(4×4、12578−165)のVMP片を使用して、0.0422gのリン酸ナトリウム十二水和物を、Adventurer Pro AV264スケールによって計量し、ビーカーに移した。次に、ビーカーに800.0gの脱イオン水を加えた。次に、ビーカーを上述の攪拌プレート上に配置し、すべての固体が完全に溶解するまで中程度にゆっくりと攪拌した。リン酸ナトリウム十二水和物が完全に溶解した後、200.0gの過マンガン酸カリウム原液を同じビーカーに加え、よく混合した。
以下に記載される各実験について、パネルをASTM B 117に従って操作された中性塩水噴霧キャビネット内に、示される期間配置した。腐食性能はMIL−C−5541に従って評価され、エッジ付近の任意のピット、キズ、金属欠陥、または加工クランプ保持エリアは省略され/カウントされていない。データは表4〜8に報告される。
パネル調製−実施例1A
各々寸法3インチ×10インチ×0.032インチ(Priority Metals、カリフォルニア州オレンジカウンティ)の21枚のアルミニウム2024−T3ベア基板を、各々メチルエチルケトン(100%)および使い捨て布で片面2回ずつ手で拭いた。各パネルは、化学洗浄の前に空気乾燥させた。次に、各パネルを、SocoMore脱脂剤(SocoClean A3432)に、127°Fで6分間、中程度の攪拌で浸漬した。次に、パネルを30秒間噴霧すすぎし、2分間浸漬すすぎし、次に、攪拌せずに室温で6分間、SocoMore脱酸剤(SocoSurf A1858/1806)に浸漬した。次に、パネルを2つの追加の浸漬すすぎタンクに慎重に浸漬し、パネルを30秒間噴霧すすぎし、2分間浸漬すすぎした。次に、3つのパネルを、組成物#1(Alodine 1200、製造業者の指示に従って調製されたHenkel AG&Co.から市販されている六価クロム含有変換組成物)、または組成物#2〜#7(上述)のうちの1つを含有する浴に2分間浸漬した(すなわち、パネルは浴ごとに3回実行された)。次に、各パネルを2つの別々の浸漬すすぎタンクに各々2分間浸漬した。最後に、各パネルを、18日間の中性塩水噴霧試験の前に、プラスチックトレイ上で、周囲条件で一晩乾燥させた。データは表4に報告される。
各々寸法3インチ×10インチ×0.032インチ(Priority Metals、カリフォルニア州オレンジカウンティ)の12枚のアルミニウム2024−T3ベア基板を、各々メチルエチルケトン(100%)および使い捨て布で片面2回ずつ手で拭いた。各パネルは、化学洗浄の前に空気乾燥させた。次に、各パネルを、SocoMore脱脂剤(SocoClean A3432)に、127°Fで6分間、中程度の攪拌で浸漬した。次に、各パネルを30秒間噴霧すすぎし、2分間浸漬すすぎし、次に、攪拌せずに室温で6分間、SocoMore脱酸剤(SocoSurf A1858/1806)に浸漬した。次に、各パネルを2つの追加の浸漬すすぎタンクに慎重に浸漬し、パネルを30秒間噴霧すすぎし、2分間浸漬すすぎした。次に、3つのパネルを、組成物#8〜#11のうちの1つを含有する浴に5分間浸漬した(すなわち、パネルは浴ごとに3回実行された)。次に、各パネルを2つの別々の浸漬すすぎタンクに各々2分間浸漬した。最後に、各パネルを、18日間の中性塩水噴霧試験の前に、プラスチックトレイ上で、周囲条件で一晩乾燥させた。データは表5に報告される。
各々寸法3インチ×10インチ×0.032インチ(Priority Metals、カリフォルニア州オレンジカウンティ)の12枚のアルミニウム2024−T3ベア基板を、メチルエチルケトン(100%)および使い捨て布で片面2回ずつ手で拭き、化学洗浄の前に空気乾燥させた。最初に、各パネルを、SocoMore脱脂剤(SocoClean A3432)に、127°Fで6分間、中程度の攪拌で浸漬した。次に、各パネルを30秒間噴霧すすぎし、2分間浸漬すすぎした。第2に、各パネルを、SocoMore脱酸剤(SocoSurf A1858/1806)に、室温で6分間、攪拌なしに浸漬した。次に、各パネルを2つの追加の浸漬すすぎタンクに慎重に浸漬して脱酸剤の大部分を除去し、パネルを30秒間噴霧すすぎし、2分間浸漬すすぎして残留脱酸剤を除去した。第3に、各パネルを組成物#2に2分間浸漬した。次に、各パネルを2つの別々の浸漬すすぎタンクに各々2分間浸漬した。次に、3つのパネルを、組成物#8〜#11のうちの1つを含有する浴に5分間浸漬した(すなわち、パネルは浴ごとに3回実行された)。次に、各パネルを2つの別々の浸漬用すすぎタンクに各タンク2分間浸漬すすぎした。最後に、各パネルを、18日間の中性塩水噴霧試験の前に、実験室のプラスチックトレイ上で一晩乾燥させた。データは表7に報告される。
実施例2A:寸法3インチ×10インチ×0.032インチ(Priority Metals、カリフォルニア州オレンジカウンティ)の1枚のアルミニウム2024−T3ベア基板を、メチルエチルケトン(100%)および使い捨て布で片面2回ずつ手で拭き、化学洗浄の前に空気乾燥させた。最初に、パネルを、洗浄組成物#12に、室温で6分間、中程度の攪拌で浸漬した。次に、パネルを30秒間噴霧すすぎし、2分間浸漬すすぎした。次に、すすいだパネルを、組成物#10を含む組成物中に6分間浸漬した。次に、パネルを2つの別々の浸漬すすぎタンクに各々2分間浸漬した。次に、パネルは、指触乾燥状態になるまで、室温で空気乾燥された。パネルのグレースケール画像を図1(A)に示す。パネルは、金色の着色がほとんどない青みがかった色であった。パネルを、図2(A)〜図2(C)に示すカラースケールに従って評価した。図2(A)〜図2(C)に示すように、1のランクは金色の着色を示さないパネルを示し、5のランクは黄色の色相が濃いパネルを示す。図2(A)〜図2(C)において、ダップルマーキングは、パネル上の金色の着色箇所とそのような着色の密度を模式的に示している。実施例2Aで処理したパネルは、2にランク付けされ、図2(A)に示される。
Claims (20)
- 金属基板を処理するためのシステムであって、
過マンガン酸アニオンを含む変換組成物と、
三価クロムカチオンを含む密封組成物であって、前記密封組成物の総重量に基づいて、0.005g/L〜2g/Lの量の三価クロムカチオンを含む、密封組成物と、を含む、システム。 - 前記過マンガン酸アニオンは、前記変換組成物の総重量に基づいて、0.1g/L〜1g/Lの量で前記変換組成物中に存在する、請求項1に記載のシステム。
- 前記変換組成物は、前記変換組成物の総重量に基づいて、0.001g/L〜0.005g/Lの量で前記変換組成物中に存在する希土類金属カチオン、および/または前記変換組成物の総重量に基づいて、0.001g/L〜0.005g/Lの量で前記変換組成物中に存在するIII族金属カチオンを含む少なくとも1つのコインヒビターをさらに含む、請求項1に記載のシステム。
- 前記密封組成物は、前記三価クロムカチオンで塩を形成するのに好適なアニオンをさらに含む、請求項1に記載のシステム。
- 前記密封組成物は、少なくとも1つの遷移金属カチオンを含む少なくとも1つのコインヒビターをさらに含む、請求項1に記載のシステム。
- 前記遷移金属カチオンは、前記密封組成物の総重量に基づいて、0.05g/L〜5g/Lの量で前記密封組成物中に存在するIVB族金属カチオンを含む、請求項5に記載のシステム。
- 洗浄組成物をさらに含む、請求項1に記載のシステム。
- 前記洗浄組成物は、水酸化物源、リン酸塩源、ならびに/または金属カチオンおよび/もしくはアゾールを含む腐食抑制剤を含む、請求項7に記載のシステム。
- 前記洗浄組成物は、7〜13のpHを有する、請求項7に記載のシステム。
- 脱酸剤をさらに含む、請求項1に記載のシステム。
- 請求項1に記載のシステムで基板を処理する方法。
- 請求項1に記載のシステムで取得可能な基板。
- 前記基板は、
(a)ASTM B117に従って操作された中性塩水噴霧キャビネット内で少なくとも18日間曝露され、MIL−C−5541に従って評価された後、前記変換組成物および前記密封組成物で処理されていない基板と比較して、前記基板表面上のピット数の少なくとも25%の減少を示し、かつ/または
(b)ASTM B117に従って操作された中性塩水噴霧キャビネット内で少なくとも18日間曝露され、MIL−C−5541に従って評価された後、20個未満のピットを有する、請求項12に記載の基板。 - 金属基板を処理するためのシステムであって、
水酸化物源、リン酸塩源、ならびに/または金属カチオンおよび/もしくはアゾールを含む腐食抑制剤を含む洗浄組成物と、
三価クロムカチオンを含む変換組成物であって、前記変換組成物の総重量に基づいて、0.005g/L〜2g/Lの量の三価クロムカチオンを含む、変換組成物と、を含むシステム。 - 前記洗浄組成物は、ポリビニルピロリドン、アラントイン、界面活性剤、増粘剤、シラン、および/またはアルコールのうちの少なくとも1つを含む添加剤をさらに含む、請求項14に記載のシステム。
- 前記変換組成物は、少なくとも1つの遷移金属カチオンを含む少なくとも1つのコインヒビターをさらに含む、請求項14に記載のシステム。
- 前記遷移金属カチオンは、前記変換組成物の総重量に基づいて、0.05g/L〜5g/Lの量で前記変換組成物中に存在するIVB族金属カチオンを含む、請求項16に記載のシステム。
- 請求項14に記載のシステムで基板を処理する方法。
- 請求項14に記載のシステムで取得可能な基板。
- 前記基板は、
(a)ASTM B117に従って操作された中性塩水噴霧キャビネット内で少なくとも18日間曝露され、MIL−C−5541に従って評価された後、前記変換組成物で処理されていない基板と比較して、前記基板表面上のピット数の少なくとも25%の減少を示し、かつ/または
(b)ASTM B117に従って操作された中性塩水噴霧キャビネット内で少なくとも18日間曝露され、MIL−C−5541に従って評価された後、20個未満のピットを有する、請求項19に記載の基板。
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