JP5693819B2 - 腐食防止剤のナノレザーバーを含む腐食防止顔料 - Google Patents
腐食防止剤のナノレザーバーを含む腐食防止顔料 Download PDFInfo
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- JP5693819B2 JP5693819B2 JP2008557661A JP2008557661A JP5693819B2 JP 5693819 B2 JP5693819 B2 JP 5693819B2 JP 2008557661 A JP2008557661 A JP 2008557661A JP 2008557661 A JP2008557661 A JP 2008557661A JP 5693819 B2 JP5693819 B2 JP 5693819B2
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Description
金属の腐食は、多大な経済的損失をもたらす金属構造の主要な破壊プロセスの一つである。通常ポリマー被覆系が金属表面上に適用され、腐食攻撃から金属構造を保護するために、腐食性の化学種のための稠密なバリヤを提供する。バリヤが損傷され、腐食剤が金属表面に浸透すると、被覆系は腐食プロセスを止めることはできない。金属の有効な保護のための耐腐食性被覆のためにこれまでに開発された最も有効な解決策は、クロム酸塩含有化成被覆を使用することである。しかしながら、六価クロム化学種は、DNA損傷や癌を含むいくつかの疾病の原因であり得、これが、欧州において2007年からCr6+含有耐腐食被覆を禁止する主要な理由である。
本発明は、特に、基板表面上への、溶液からの反対に荷電した化学種(高分子電解質、ナノ粒子、酵素、デンドリマー)の交互積層(LbL)堆積の近年発展した技術(G. Decher, J.D. Hong, J. Schmitt, Thin Solid Films 1992, 210/211, 831, and G. Decher, Science 1997, 277, 1232)は、ナノメーター厚さの正確さで集積した、調節された貯蔵/放出性能を有する腐食防止剤レザーバーを調製するための非常に有効な方法に相当する、という驚くべき発見に基づいている。
本発明の具体例において、モデル金属基板としてのアルミニウム合金AA2024上に堆積された、ハイブリッドエポキシ官能化ZrO2/SiO2ゾルゲル被覆中に閉じ込められた交互積層集積ナノレザーバーの耐腐食及び自己修復作用が、調査された。ポリ(エチレンイミン)/ポリ(スチレンスルホナート)(PEI/PSS)層で被覆された70nmのSiO2粒子が、ナノレザーバーとして使用された。腐食防止剤ベンゾトリアゾールが、LbL集積工程で高分子電解質多重層内に取り込まれ、その放出は、アルミニウム合金の腐食中のpH変化により開始されることができる。
腐食試験の間被覆された基板に関する物理化学的プロセスの数値評価を提供することができる、電気化学的インピーダンス測定が、ハイブリッドゾルゲル膜の腐食保護性能を評価するためになされた。電気化学的インピーダンス分光分析法のために、飽和カロメル参照電極、対電極としての白金箔及び作用電極としての露出試料(3.4cm2)から成るファラデーケージ中の3電極配置が、使用された。インピーダンス測定は、PCI4Controllerを有するGamry FAS2 Femtostatにより、デケードあたり10ステップで100KHz〜10mHz周波数範囲の10mV正弦波摂動適用での開回路電位でなされた。インピーダンスプロットは、腐食プロセスの間のアルミニウム合金電極の状態をシミュレートするために、互換性のある等価回路に適合された。
スに基づいて現れる。ドープされないハイブリッド膜とナノレザーバーを添加された膜に対しては、インピーダンススペクトルに腐食の兆候は全く見出されず、腐食化学種に対する有効なバリヤ性を示した。直接導入されたベンゾトリアゾールを有するゾルゲル膜により保護された合金表面に関する活性な腐食プロセスは、水溶液に添加された遊離ベンゾトリアゾールが、AA2024アルミニウム合金上の腐食プロセスの非常に有効な防止剤として知られるという事実にもかかわらず、任意の防止作用の不在を示している。
追加的な実験が、被覆に添加されたナノレシーバーの自己修復作用の証拠を提供するためになされた。人工欠陥(各試料ごとに50μmサイズの5つの欠陥)が、合金表面への腐食媒体の直接的進入を与えるために、0.005M NaCl中での浸漬後に微小針によりゾルゲル膜中に形成された。欠陥試料の浸漬開始後すぐのインピーダンススペクトルは、インピーダンスの減少と、損傷されたゾーンでの活性プロセスに由来する低周波数でのデータの散乱を示す。ドープされないゾルゲル膜の場合には、欠陥の形成は、長期間のデータの散乱を引き起こし、それゆえ、欠陥は、0.005Mの電解質中でただ1日後にこの膜で形成された。複合膜は、浸漬の14日後に人工的に離脱された。中間酸化物層の抵抗は、インピーダンススペクトルの低周波数部分から計算された。図5bは、0.05M NaCl中での欠陥形成後の酸化物膜の抵抗の漸進的変化を示す。ドープされない被覆の初期抵抗は、欠陥形成前のより短い浸漬期間に基づいてより高い。酸化物抵抗の急速な減少は、欠陥が導入されるとすぐに生起する。続く抵抗の漸進的低下は、腐食保護性能の劣化を示す。酸化物の抵抗も、ナノレザーバーで充填されたハイブリッド膜の欠陥形成後すぐに減少する。しかしながら、インピーダンスの初期の低下後に、酸化物膜抵抗の非常に重要な回復が更なる60時間の浸漬中に生起する。抵抗の増加は、ナノレザーバードープゾルゲル被覆中の欠陥の自己修復を明らかに示す。このような自己修復作用は、ドープされないゾルゲル膜で被覆されたAA2024の場合に明らかでなかった。したがって、自己修復効果は、損傷領域でナノ容器から放出されたベンゾトリアゾールに最大限由来する可能性がある。
応用電子(Applicable Electoronics)装置を使用する振動電極走査技術(SVET)が、ナノ複合材料の前処理の自己修復能力を証明するために使用された。この方法は、表面に沿った陰極及び陽極電流の分布をマッピングする局所的な腐食活性を示すことができる。直径約200ミクロンの欠陥が、図6a、bに示されるゾルゲル前処理されたAA2024表面に形成された。高い陰極電流密度は、非ドープ被覆が0.05M NaCl中に浸漬されると、欠陥を起点に即座に出現し、明確な腐食活性を示す。欠陥は、全ての試験中で活性なままである(図6c、e、g)。ナノ容器でドープされたハイブッド膜で被覆された試料は、完全に異なる挙動をする。最初の10時間には、欠陥ゾーンには、顕著な電流は全く存在しない(図6d)。約24時間後にのみ、陰極電流が出現する。しかしながら、活性開始後2時間、腐食の効果的な抑制がおこり、局所電流密度の減少が生起する。欠陥位置の陰極活性は、連続的な48時間の浸漬後に再度殆ど見えなくなる(図6h)。被覆系中に形成される相対的に大きな人工欠陥での腐食活性の効果的な抑制は、ナノ容器でドープされたハイブッド前処理の自己修復能力を明らかに証明している。
Mg+2H2O→Mg2++2OH−+H2↑。
Mg→Mg2++2e−。
ポリ(アリルアミン)/ポリ(アクリル酸)(PAH/PAA)層で被覆された150nmのZrO2粒子が、ナノレザーバーとして使用された。腐食防止剤キノリノールが、LbL集積工程で高分子電解質多重層内に閉じ込められた。その放出は、鋼合金腐食中のpH変化により開始することができる。
50nm直径の天然起源中空アルミノ珪酸塩(ハロイサイト)が、ナノレレザ−バーの別のタイプとして使用された。腐食防止剤メルカプトベンゾトリアゾールが、真空ポンプ下、10mg/mlのエタノール溶液から環状空隙内部に閉じ込められた。空隙を防止剤で完全に満たすために、閉じ込め手順が4度繰り返された。次いで、ハロイサイト粒子の外部表面はpHに規制される閉じ込められたメルカプトベンゾトリアゾールの徐々の放出を達成するために、高分子電解質多重層で被覆された(正のPAH吸着が、第1段階での0.5M NaCl中の2mg/mlのPAHからなされた。得られたハロイサイトの洗浄が各吸着工程後に、蒸留水によりなされた。次いで、負のPAA層の吸着が、0.5M NaCl中の2mg/mlのPAAから実行された。PAA/PSS吸着が、2度繰り返された。)。
Claims (21)
- 金属製品及び金属構造物の有効な腐食保護のための腐食防止剤のナノ容器を含む腐食防止顔料であって、1〜1000nmの範囲の平均寸法を有するナノ容器は、pH又は温度の変化から選ばれる特定のトリガーに応答し、前記トリガーの作用後に前記防止剤を放出することができるが、前記トリガーの作用前には前記防止剤の放出を引き起こさないポリマー若しくは高分子電解質シェルを含み、ここで、前記防止剤は、1以上のアミノ基を含む有機化合物、アゾール誘導体化合物、1以上のカルボキシル基或いはカルボン酸塩を含む有機化合物及び1以上のピリジニウム或いはピラジン基を含む有機化合物から成る群より選択される有機化合物を含むか、前記防止剤は、バナジウム酸(VO3 −)を含み、
および前記ナノ容器は、ポリマー若しくは高分子電解質シェルで被覆された中空高分子電解質カプセル、中空ポリマーカプセル、ナノチューブ、ハロイサイト又は中空あるいは多孔ナノ粒子を含む群から選ばれ、ここで、前記防止剤は、前記カプセル、ナノチューブ、ハロイサイト又ナノ粒子の空隙もしくは多孔中に組み込まれる、
腐食防止顔料。 - 防止剤が、ベンゾトリアゾール、メルカプトベンゾトリアゾール、キナルジン酸若しくはキノリノールである、請求項1記載の顔料。
- 防止剤が、請求項1又は2で特定される2以上の化合物を含む、請求項1又は2記載の顔料。
- ナノ粒子が、SiO2、ZrO2、TiO2若しくはCeO2のナノ粒子である、請求項1乃至3何れか1項記載の顔料。
- ポリマー若しくは高分子電解質シェルは、防止剤が点在するものである、請求項1乃至4何れか1項記載の顔料。
- ナノ容器は、防止剤が点在する交互積層高分子電解質シェルで被覆されたナノ粒子を含む、請求項5記載の顔料。
- ポリマー若しくは高分子電解質シェルが、ポリ(アルキレンイミン)、ポリ(スチレンスルホナート)、ポリ(アリルアミン)、ポリビニルアルコール、ポリ(ヒドロキシ酪酸)、ポリスチレン、ポリ(ジアリルジメチルアンモニウムクロライド)、ポリ(メタ)アクリル酸、ポリアルキレングリコール、ポリ(ビニルピリジン)並びにゼラチン、アガロース、セルロース、アルギン酸、デキストラン、カゼイン、ポリアルギニン、ポリグリシン、ポリグルタミン酸、ポリアスパラギン酸のようなバイオポリマー及びポリアミノ酸並びにそれらの誘導体、コポリマー若しくは混合物から成る群より選択される1以上のポリマー若しくは高分子電解質を含む、請求項1乃至6何れか1項記載の顔料。
- ポリマー若しくは高分子電解質シェルが、正に荷電した高分子電解質と負に荷電した高分子電解質の交互の層を含む、請求項7記載の顔料。
- 正に荷電した高分子電解質が、ポリ(エチレンイミン)であり、負に荷電した高分子電解質が、ポリ(スチレンスルホナート)である、請求項8記載の顔料。
- 1以上の前記高分子電解質層上に堆積され、少なくとも1つの前記高分子電解質層により被覆された1以上の防止剤の層を更に含む、請求項7乃至9何れか1項記載の顔料。
- 請求項1乃至10何れか1項記載の顔料を含む、耐腐食被覆。
- ゾルゲル膜を更に含む、請求項11記載の耐腐食被覆。
- ゾルゲル膜が、ハイブリッドSiO2-ZrO2膜である、請求項12記載の耐腐食被覆。
- 特定のトリガーに敏感に反応し、前記トリガーの作用後に前記防止剤を放出することのできる1〜1000nmの範囲の平均寸法を有するポリマー若しくは高分子電解質シェルを含むナノスケールのレザーバー中に腐食防止剤に組み込むことを含む、請求項1乃至10何れか1項記載の腐食防止剤顔料を調製する方法。
- ポリマー若しくは高分子電解質シェルは、表面重合、表面堆積、交互積層集積若しくは自己集積技術により形成される、請求項14記載の方法。
- 中空ナノスケール固体基体が、前記ポリマー若しくは高分子電解質シェルにより被覆される、請求項15記載の方法。
- ナノ粒子が、交互積層高分子電解質シェルにより被覆される、請求項16記載の方法。
- 交互積層高分子電解質シェルは、防止剤が点在するものである、請求項17記載の方法。
- pH又は温度から選択される特定のトリガーに前記顔料を暴露し、ポリマー若しくは高分子電解質シェルに前記腐食防止剤を放出させることを含む、請求項1乃至10何れか1項記載の顔料から腐食防止剤の制御可能な放出を提供する方法。
- 請求項1乃至10何れか1項記載の顔料の、前処理物、プライマー、ポリマー被覆処方、粉末被覆、塗料及びコンクリートへの組み込みを含む金属製品若しくは金属構造物の腐食を妨害若しくは防止する方法。
- 顔料が粉末若しくは懸濁液の形である、請求項20記載の方法。
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DE102004013637A1 (de) * | 2004-03-19 | 2005-10-13 | Capsulution Nanoscience Ag | Verfahren zur Herstellung von CS-Partikeln und Mikrokapseln unter Verwendung poröser Template sowie CS-Partikel und Mikrokapseln |
JP5052014B2 (ja) * | 2006-02-15 | 2012-10-17 | 株式会社トクヤマ | 防錆材 |
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