JP6282700B2 - 鉄金属基板を処理するための方法 - Google Patents
鉄金属基板を処理するための方法 Download PDFInfo
- Publication number
- JP6282700B2 JP6282700B2 JP2016174472A JP2016174472A JP6282700B2 JP 6282700 B2 JP6282700 B2 JP 6282700B2 JP 2016174472 A JP2016174472 A JP 2016174472A JP 2016174472 A JP2016174472 A JP 2016174472A JP 6282700 B2 JP6282700 B2 JP 6282700B2
- Authority
- JP
- Japan
- Prior art keywords
- bath
- metal
- phosphate
- pretreatment
- iron
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 238000000034 method Methods 0.000 title claims description 125
- 229910052751 metal Inorganic materials 0.000 title claims description 124
- 239000002184 metal Substances 0.000 title claims description 124
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- 238000012545 processing Methods 0.000 title description 11
- 239000000203 mixture Substances 0.000 claims description 199
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 183
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 118
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- 239000011347 resin Substances 0.000 claims description 61
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 55
- 238000000576 coating method Methods 0.000 claims description 50
- 239000011248 coating agent Substances 0.000 claims description 34
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 claims description 27
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- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 claims description 11
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- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 claims description 4
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- 229910052727 yttrium Inorganic materials 0.000 description 17
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- 125000002091 cationic group Chemical group 0.000 description 8
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- 238000006243 chemical reaction Methods 0.000 description 7
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- DXIGZHYPWYIZLM-UHFFFAOYSA-J tetrafluorozirconium;dihydrofluoride Chemical compound F.F.F[Zr](F)(F)F DXIGZHYPWYIZLM-UHFFFAOYSA-J 0.000 description 7
- 239000005955 Ferric phosphate Substances 0.000 description 6
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Images
Classifications
-
- 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
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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
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- 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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- 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
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Description
本願は、2011年12月7日に出願された、米国特許第12/237,770号明細書の一部継続出願であり、2008年9月25日に出願された米国特許第8,097,093号明細書として現在取得されている米国特許第13/313,473号明細書の一部継続出願である。本願は、参考として本明細書により援用される、2007年9月28日に出願された米国仮特許出願第60/975,957号明細書の利益を主張する。
本発明は、冷間圧延鋼、熱間圧延鋼、および電気亜鉛めっき鋼などの、鉄金属基板を処理するための方法に関する。本発明は、被覆された鉄金属基板にも関する。本発明は、前処理浴が加工ライン上にある場合、前処理組成物によって被覆される物品の存在下にあるときと前処理浴がオフシフトにあるときとの両方において、前処理浴から鉄を除去するための方法にも関する。
改善された耐蝕性および塗料接着を目的とした、金属基板上での保護コーティングの使用は、一般的である。そのような基板を被覆するための従来の技法は、リン酸塩皮膜処理およびクロム含有リンスにより金属基板の前処理を行うことを含む技法を含む。典型的なリン酸塩皮膜処理は、リン酸塩が少なくとも約1,000百万分率(「ppm」)の範囲内で操作され、それが廃棄物処理の問題をもたらす。したがって、そのようなリン酸塩および/またはクロム含有組成物の使用は、環境上および健康上の懸念をもたらす。
ある観点では、本発明は、鉄金属基板を被覆するための方法を対象とする。
本発明の実施形態において、例えば以下の項目が提供される。
(項目1)
IIIB族および/またはIV族金属を含む前処理組成物を含有する前処理浴から、鉄を除去するための方法であって、
(a)前記前処理浴のpHを少なくとも0.2低減させる工程と;
(b)(a)において前記前処理浴にリン酸イオンを添加する工程と;
(c)(b)において前記前処理浴のpHを少なくとも0.2上昇させる工程と
を含む方法。
(項目2)
前記前処理浴のpHを少なくとも1.0低減させる、項目1に記載の方法。
(項目3)
前記低減させる工程が、前記前処理浴に酸を添加する工程を含む、項目1に記載の方法。
(項目4)
前記酸が、IVB族フルオロ金属酸、リン酸、硫酸、スルファミン酸、硝酸、およびこれらの混合物を含む、項目3に記載の方法。
(項目5)
前記酸がヘキサフルオロジルコン酸を含む、項目3に記載の方法。
(項目6)
前記リン酸イオンの供給源が、アルカリ金属オルトリン酸塩、オルトリン酸アンモニウム、およびこれらの混合物を含む、項目1に記載の方法。
(項目7)
前記リン酸イオンの供給源が、リン酸一ナトリウムを含む、項目1に記載の方法。
(項目8)
(c)において前記前処理浴が、鉄を実質的に含まない、項目1に記載の方法。
(項目9)
(b)において前記前処理浴に酸化剤を添加する工程をさらに含む、項目1に記載の方法。
(項目10)
前記酸化剤が過酸化物化合物を含む、項目9に記載の方法。
(項目11)
(c)において前記前処理浴を濾過する工程をさらに含む、項目1に記載の方法。
(項目12)
前記前処理組成物によって被覆される物品が存在しない状態で行われる、項目1に記載の方法。
(項目13)
前記IIIB族および/またはIVB族金属がジルコニウムを含む、項目1に記載の方法。
(項目14)
前記前処理組成物がリン酸イオンをさらに含む、項目1に記載の方法。
(項目15)
IIIB族および/またはIVB族金属を含む前処理組成物を含有する前処理浴から、鉄を除去するための方法であって、
(a)前記前処理浴に酸を添加して、前記前処理組成物のpHを4.0よりも低く低減させる工程と;
(b)(a)において前記前処理浴にリン酸イオンを添加する工程と;
(c)(b)において前記前処理浴のpHを4から5.5に上昇させる工程と
を含む方法。
(項目16)
前記酸がヘキサフルオロジルコン酸を含む、項目15に記載の方法。
(項目17)
前記リン酸塩の供給源がリン酸一ナトリウムを含む、項目15に記載の方法。
(項目18)
(b)において前記前処理浴に酸化剤を添加する工程をさらに含む、項目15に記載の方法。
(項目19)
前記酸化剤が過酸化物化合物を含む、項目18に記載の方法。
(項目20)
(c)において前記前処理浴を濾過する工程をさらに含む、項目15に記載の方法。
(項目21)
工程(c)の後の前記前処理浴中の前記前処理組成物が、1:1から1.7:1重量部のリン酸塩と第二鉄イオンとの重量比を含む、項目15に記載の方法。
(項目22)
前記前処理組成物によって被覆される物品が存在しない状態で行われる、項目15に記載の方法。
(項目23)
前記前処理組成物がリン酸イオンをさらに含む、項目15に記載の方法。
以下に詳細に記述する目的で、本発明は、反対の内容が明らかに示されている場合を除き、様々な代替の変形例および工程順序を想定することができると理解される。さらに、任意の操作実施例に記載されているもの以外、または他に指示されている場合、例えば本明細書および特許請求の範囲で使用される成分の量を表す全ての数値は、全ての場合において、「約」という用語によって修飾されることが理解される。したがって、反対の内容が示されない限り、以下の明細書および添付される特許請求の範囲に記述される数値パラメーターは、本発明によって得られる所望の性質に応じて変化してもよい近似値である。最低でも、特許請求の範囲に対する均等物の教義の適用を限定しようとするものではなく、各数値パラメーターは、報告された有効桁の数に照らしてかつ通常の丸め技法を適用することによって、少なくとも解釈されるべきである。
259 920 Aに記載されているようなモリブデン化合物を含む。対照的に、その他の実施形態では、前処理組成物は、任意のモリブデン化合物を実質的に含まず、またはある場合には完全に含まない。
896、Eastman Chemical,Inc.のAccurate Dispersions divisionから市販されているCHARISMA COLORANTSおよびMAXITONER INDUSTRIAL COLORANTSなど、水ベースのまたは水混和性の担体に分散させた顔料が含まれるが、これらに限定するものではない。
一実験において、5つの清浄な鋼パネルを、pHが約1.8〜2.4でありフルオロジルコン酸およびリン酸を含有する(Zr 90ppm、およびPO4 −3 10ppm)水溶液中に置いた。第一鉄濃度を約30ppmに増やした後、パネルを透明溶液から取り出し、1ガロン(3.78リットル)ずつに分けた。
鋼パネルを、従来のアルカリベースの清浄剤を使用して清浄化し、水道水で2回濯ぎ、10〜150ppmの範囲のジルコニウムおよび10〜100ppm範囲のリン酸塩を含有する浴内で処理し、次いで引き続き水道水で濯いだ。処理した鋼パネルに、共にPPG
Industries Inc.から市販されているP590陽イオン性エポキシ電着コーティングまたはPCT79111トリグリシジルイソシアヌレート−ポリエステル粉末コーティングを塗装した。腐蝕性能は、ジルコニウムで処理され塗装されたパネルを、ASTM B117に従って表2.0に示される時間にわたり中性塩水噴霧に曝すことによって決定した。この試験における1000時間の中性塩水噴霧曝露での、陽イオン性エポキシ電着コーティングの許容される性能は、1/2幅スクライブ損失が4.0〜5.0mmであった。500時間の中性塩水噴霧曝露での、TGIC−ポリエステル粉末で許容される性能は、1/2幅スクライブ損失が2.0〜3.0mmであった。以下の結果は、許容される腐蝕性能を、リン酸イオンがジルコニウム処理浴に添加された場合に得ることができることを実証する。実施例1.0に示したように、リン酸イオンが低濃度の場合、処理浴は褐色に変化して、酸化鉄またはオキシ水酸化鉄の存在を示す。
前処理溶液を調製し、そこに多量のヘキサフルオロジルコン酸を添加した。冷間圧延鋼パネルを被覆する前に、浴のpHを4.7に調節した。ACT Labs(Hillsdale、MI)から得たパネルを、まず、アルカリ性清浄剤(PPG Industries Chemkleen 611L、2%および140〜150°F)で噴霧清浄し、2回濯いだ後に、前処理ゾーンに進入させた。ジルコニウム浴をパネルに9psiで60秒間噴霧した。次いでそれらを水道水で濯ぎ、最後に脱イオン水ハロで濯いだ後に、赤外線乾燥工程に進めた。
実際に、錆で酷く汚染されている浴は、半透明のオレンジ溶液の外観の後に、不透明な褐色がかった赤になり、これは不溶性の第二鉄錯体に最初に変換されたことを示す。一実験において、100ppmのジルコニウムを含有する10ガロンの低pH浴(約2.7)を、全鉄が50ppmに到達するまで鋼パネルに数時間噴霧した。第一鉄は約40ppmであった。浴は10ppmの可溶性第二鉄イオンを含有していたが、それは無色透明であった。大きいサンプルをいくつかに分割し、そこに高レベルのリン酸塩を添加して、pHが5に上昇した後に浴の初期退色を防止し得るレベルを決定した。リン酸塩を含まない対照サンプルの場合、第二鉄レベルは24ppmまで増加し、その直後に浴が変色し始めた。この実験結果を表3.0に示す。
鉄を含有する濃縮物は、ヘキサフルオロジルコン酸を脱イオン水に溶かした溶液であってリン酸塩を含有しない溶液中に、清浄な鋼パネルを2日間吊るすことによって得た。最終の第一鉄レベルは約900ppmであり、第二鉄は33ppmであった。次いで濃縮物を水道水で希釈して、約20ppmの第一鉄および3ppmの第二鉄を得た。様々な量のリン酸を添加し、その後、全ての第一鉄を第二鉄に変換するのに十分な過酸化水素を添加した。次いでpHを、各浴ごとに4.7に調節した。静止状態に1日放置した後、リン酸塩およびジルコニウムに関して浴を分析した。結果を図4にプロットする。明らかなように、約30ppmのリン酸塩は、溶液中に当初の65ppmのジルコニウムのほとんどを維持しながら20ppmの第二鉄を除去するのに十分と考えられる。
実施例6は、第二鉄(Fe+3)をオフシフトの前処理浴から除去できることを実証するために実施した。
図5に示され実施例6に記述されたデータは、リン酸塩を低pHの前処理浴に添加することにより、第二鉄が前処理浴から除去されることを実証した。しかし実際に、基板を処理するのに使用されてきた前処理浴は、前処理浴から除去するために第二鉄に変換されなければならない第一鉄をしばしば含有する。実施例7と、表4に示され本明細書に記述されるデータは、前処理浴に酸化剤を添加することによって、当初は第一鉄状態にあった鉄の除去が改善されることを実証する。
この実施例では、3.60gのヘキサフルオロジルコン酸を水3リットルに添加して、240ppmのジルコニウムを有する溶液を得ることにより、作用前処理浴を作製した。溶液のpHを4.5に上昇させるのに十分な量のChemfil緩衝液を添加した。硫酸第一鉄7水和物0.31gを添加することにより、20ppmの第一鉄が得られた。錆粒子の形成を防止するために、ヘキサフルオロジルコン酸約14滴を直ぐに添加して、pHを3.3に低下させた。浴は透明であった。Hachメーターを使用して、全鉄濃度が23.2ppmであることを測定し、第一鉄は19.5ppmであった。
Claims (12)
- 鉄金属基板を被覆するための方法であって、
(a)前記金属基板を、4から5.5のpHを有する水性前処理組成物と接触させる工程であって、
前記水性前処理組成物が、
(a)IVB族金属化合物、
(b)リン酸イオン、および
(c)水
を含み、前記IVB族金属化合物は、10から500ppmの金属量で前記前処理組成物中に存在し、前記前処理組成物中のIVB族金属とリン酸イオンとの重量比が少なくとも0.8:1であり、前記リン酸イオンが、前記前処理組成物の浴内で、(i)前記浴内での不溶性の錆の形成を本質的に防止するのに十分な量で、かつ(ii)前記金属基板上で少なくとも10mg/m2の被覆率を有するIVB族金属被膜の堆積を防止するのに不十分な量で、かつ(iii)リン酸イオンと第二鉄イオンとの重量比、1から1.8:1をもたらす量で維持される、工程と;
(b)前記基板を、被膜形成樹脂を含むコーティング組成物と接触させて耐蝕特性を示す被覆された金属基板を形成する工程と
を含み、
ここで、前記IVB族金属がジルコニウム、チタン、ハフニウムまたはこれらの混合物である、
方法。 - 前記リン酸イオンが、アルカリ金属オルトリン酸塩、オルトリン酸アンモニウム、およびこれらの混合物を含む、請求項1に記載の方法。
- 前記リン酸イオンが、リン酸一ナトリウムを含む、請求項1に記載の方法。
- 前記水性前処理組成物が、鉄を実質的に含まない、請求項1に記載の方法。
- 前記水性前処理組成物が、酸化剤をさらに含む、請求項1に記載の方法。
- 前記酸化剤が過酸化物化合物を含む、請求項5に記載の方法。
- 鉄金属基板を被覆するための方法であって、
(a)前記金属基板を、4から5.5のpHを有する水性前処理組成物と接触させる工程であって、
前記水性前処理組成物が、
(a)IVB族金属化合物、
(b)リン酸イオン、および
(c)水
を含み、前記IVB族金属化合物は、10から500ppmの金属量で前記前処理組成物中に存在し、前記前処理組成物中のIVB族金属とリン酸イオンとの重量比が少なくとも0.8:1であり、前記リン酸イオンが、前記前処理組成物の浴内で、(i)前記浴内での不溶性の錆の形成を本質的に防止するのに十分な量で、(ii)前記金属基板上で少なくとも10mg/m2の被覆率を有するIVB族金属被膜の堆積を防止するのに不十分な量で、かつ(iii)リン酸イオンと、第一鉄状態にある追加の可溶性の鉄との重量比が1.8から10:1の範囲になる量で維持される、工程と;
(b)前記基板を、被膜形成樹脂を含むコーティング組成物と接触させて耐蝕特性を示す被覆された金属基板を形成する工程と
を含み、
ここで、前記IVB族金属がジルコニウム、チタン、ハフニウムまたはこれらの混合物である、
方法。 - 前記リン酸イオンが、アルカリ金属オルトリン酸塩、オルトリン酸アンモニウム、およびこれらの混合物を含む、請求項7に記載の方法。
- 前記リン酸イオンが、リン酸一ナトリウムを含む、請求項7に記載の方法。
- 前記水性前処理組成物が、鉄を実質的に含まない、請求項7に記載の方法。
- 前記水性前処理組成物が、酸化剤をさらに含む、請求項7に記載の方法。
- 前記酸化剤が過酸化物化合物を含む、請求項11に記載の方法。
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KR102416141B1 (ko) * | 2014-01-23 | 2022-07-04 | 케메탈 게엠베하 | 금속 표면을 코팅하는 방법, 이러한 방식으로 코팅된 기판, 및 이의 용도 |
CN106011823B (zh) * | 2016-07-29 | 2018-06-19 | 南京科润工业介质股份有限公司 | 一种用于提高金属耐蚀性的表面处理剂 |
CN108842130B (zh) * | 2018-07-12 | 2020-05-12 | 中国航发哈尔滨轴承有限公司 | 一种利用球面滚子化学热处理专用工装对球面滚子表面改性的方法 |
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KR20150115916A (ko) | 2015-10-14 |
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CA2898751A1 (en) | 2014-09-12 |
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MY171863A (en) | 2019-11-05 |
EP2964806A1 (en) | 2016-01-13 |
JP2016223019A (ja) | 2016-12-28 |
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CA2898751C (en) | 2017-09-19 |
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HK1211062A1 (en) | 2016-05-13 |
SG11201505264XA (en) | 2015-08-28 |
BR112015019200B1 (pt) | 2021-07-20 |
AU2014226289B2 (en) | 2016-09-15 |
AU2014226289A1 (en) | 2015-07-23 |
CN105026615A (zh) | 2015-11-04 |
CN108842149A (zh) | 2018-11-20 |
UA113689C2 (xx) | 2017-02-27 |
KR101714292B1 (ko) | 2017-03-08 |
TW201443283A (zh) | 2014-11-16 |
EP2964806B1 (en) | 2020-08-05 |
WO2014137796A1 (en) | 2014-09-12 |
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