JP7117292B2 - 鋼、亜鉛めっき鋼、アルミニウム、アルミニウム合金、マグネシウムおよび/または亜鉛-マグネシウム合金を含む金属表面を腐食保護前処理するための改善された方法 - Google Patents
鋼、亜鉛めっき鋼、アルミニウム、アルミニウム合金、マグネシウムおよび/または亜鉛-マグネシウム合金を含む金属表面を腐食保護前処理するための改善された方法 Download PDFInfo
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- JP7117292B2 JP7117292B2 JP2019514730A JP2019514730A JP7117292B2 JP 7117292 B2 JP7117292 B2 JP 7117292B2 JP 2019514730 A JP2019514730 A JP 2019514730A JP 2019514730 A JP2019514730 A JP 2019514730A JP 7117292 B2 JP7117292 B2 JP 7117292B2
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- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- 125000003396 thiol group Chemical group [H]S* 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- FBBATURSCRIBHN-UHFFFAOYSA-N triethoxy-[3-(3-triethoxysilylpropyldisulfanyl)propyl]silane Chemical group CCO[Si](OCC)(OCC)CCCSSCCC[Si](OCC)(OCC)OCC FBBATURSCRIBHN-UHFFFAOYSA-N 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N urea group Chemical group NC(=O)N XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 1
- ZTWTYVWXUKTLCP-UHFFFAOYSA-N vinylphosphonic acid Chemical compound OP(O)(=O)C=C ZTWTYVWXUKTLCP-UHFFFAOYSA-N 0.000 description 1
- NLVXSWCKKBEXTG-UHFFFAOYSA-N vinylsulfonic acid Chemical compound OS(=O)(=O)C=C NLVXSWCKKBEXTG-UHFFFAOYSA-N 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
- XJUNLJFOHNHSAR-UHFFFAOYSA-J zirconium(4+);dicarbonate Chemical compound [Zr+4].[O-]C([O-])=O.[O-]C([O-])=O XJUNLJFOHNHSAR-UHFFFAOYSA-J 0.000 description 1
Classifications
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- C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
- C09D133/04—Homopolymers or copolymers of esters
- C09D133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C09D133/10—Homopolymers or copolymers of methacrylic acid esters
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- B05D1/00—Processes for applying liquids or other fluent materials
- B05D1/36—Successively applying liquids or other fluent materials, e.g. without intermediate treatment
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- C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
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- C09D161/00—Coating compositions based on condensation polymers of aldehydes or ketones; Coating compositions based on derivatives of such polymers
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- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/04—Polysiloxanes
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
- C09D5/082—Anti-corrosive paints characterised by the anti-corrosive pigment
- C09D5/084—Inorganic compounds
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
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- 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
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- 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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- 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
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- 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
- C23C22/40—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 molybdates, tungstates or vanadates
- C23C22/44—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 molybdates, tungstates or vanadates containing also fluorides or complex fluorides
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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
- 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
- C23C22/78—Pretreatment of the material to be coated
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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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- 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
- C23C22/82—After-treatment
- C23C22/83—Chemical after-treatment
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- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D1/00—Processes for applying liquids or other fluent materials
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- B05D2202/00—Metallic substrate
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- B05D2202/25—Metallic substrate based on light metals based on Al
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- 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
- C23C2222/00—Aspects relating to chemical surface treatment of metallic material by reaction of the surface with a reactive medium
- C23C2222/20—Use of solutions containing silanes
Description
i)a1)チタン化合物、ジルコニウム化合物およびハフニウム化合物からなる群から選択される少なくとも1種の化合物を含む酸性水性組成物A、ならびに
ii)b1)少なくとも1種の(メタ)アクリレート樹脂およびb2)少なくとも1種のフェノール樹脂を含む水性組成物B
と接触させ、
金属表面を、
i)第一に組成物Aと、次いで、組成物Bと、
ii)第一に組成物Bと、次いで、組成物Aと、かつ/または
iii)組成物Aおよび組成物Bと同時に
接触させる。
本発明において、「水性組成物」は、溶媒/分散媒としての水だけでなく、溶媒/分散媒の総量に対して50質量%未満の他の有機溶媒/分散媒も含む組成物を含む。
i)第一に組成物Aと、次いで、組成物Bと、
ii)第一に組成物Bと、次いで、組成物Aと、かつ/または
iii)組成物Aおよび組成物Bと同時に接触させる」
という表現は、以下の実施形態も包含されることを意味すると解釈されるべきである:
好ましい1種の実施形態によれば、金属表面を、第一に組成物Aと、次いで、組成物Bと接触させ、これは、組成物Bが後すすぎ剤として使用されることを意味する。
PEOx-PPOy-PEOz(I)
(式中、PEOはポリエチレンオキシドであり、PPOはポリプロピレンオキシドであり、xおよびzは、それぞれの場合において、4~12の範囲内の整数であり、yは、35~65の範囲内の整数である)
の少なくとも1種のトリブロックコポリマーを含む。
R1O-(CH2)x-Z-(CH2)y-OR2(II)
(式中、R1およびR2は、それぞれの場合において、互いに独立してHまたはHO-(CH2)w-基(式中、w≧2)であり、xおよびyは、それぞれの場合において、互いに独立して1~4であり、Zは、硫黄原子またはC-C三重結合である)
の少なくとも1種の化合物b4)をさらに含む。
組成物Aは、好ましくは、成分a1)としてチタン、ジルコニウムおよびハフニウムの錯フッ化物からなる群から選択される少なくとも1種の錯フッ化物を含む。
- 亜鉛カチオン:0.1~5g/l
- 銅カチオン:5~50g/l
- セリウムカチオン:5~50mg/l
- モリブデン化合物:10~100mg/l(モリブデンとして計算)。
i)(ジルコニウムとして計算された)成分a1)のみに対して5~500mg/m2、好ましくは10~200、特に好ましくは30~120mg/m2、および任意に
ii)(ケイ素として計算された)成分a2)のみに対して0.5~50mg/m2、好ましくは1~30、特に好ましくは2~10mg/m2
の層質量を有する、金属表面を提供する。
基材:
溶融亜鉛めっき鋼(HDG)でできたシート(10.5×19cm)および冷間圧延鋼(CRS)でできたその他を基材として使用した。
すべての実施例において、Gardoclean(登録商標)S 5176(Chemetall製;リン酸塩、ホウ酸塩および界面活性剤を含む)を穏やかなアルカリ浸漬洗浄剤として使用した。この目的のために、15g/lを50l浴中で調製し、60℃まで加熱し、10.0~11.0の範囲内のpHで3分間吹き付けることにより基材を洗浄した。続いて、基材を水道水および脱イオン水ですすいだ。
異なる量の樹脂混合物(表1:「Resin mix.」参照)を本発明にしたがって任意に添加した脱イオン水を使用して、前すすぎを実施した。この樹脂混合物は、質量平均分子量160g/molを有する以下のレゾール(例示的な式)
化成処理浴については、Oxsilan(登録商標)添加剤9936(Chemetall(ドイツ)製;フッ化物およびジルコニウム化合物を含む)および任意にOxsilan(登録商標)9810/3(Chemetall(ドイツ)製;アミノシランを含む。表3:「シラン」参照)を、ジルコニウム濃度100~130mg/lおよび(Siとして計算された)シラン濃度20~30mg/lになるような量で50lバッチに加えた。浴温度は30℃に設定した。希薄炭酸水素ナトリウム溶液および希薄フッ化水素酸(5%強度)を添加することにより、pHおよび遊離フッ化物含有量をそれぞれpH=4.8および30~40mg/lに設定した。
後すすぎ剤については、本発明にしたがって任意に、本発明による前すすぎ剤に関連して既に説明した様々な量の樹脂混合物(表2:「Resin mix.」参照)、ならびに任意に、本発明による化成処理浴に関連して既に説明した100mg/lの特定のトリブロックコポリマー(表2:「Stabil.」参照)を添加した脱イオン水を使用した。
蛍光X線分析:
前処理した基材上の層質量(LW)(mg/m2)を蛍光X線分析(XRF)により決定した。本明細書では、塗布されたジルコニウムの量を測定した。
前処理した基材をCECにより塗装した。Cathoguard(登録商標)800(BASF(ドイツ)製)をこの目的のために使用した。続いて、重ね塗りを施した。これはDaimler Blackであった。DIN EN ISO 2808(2007 version)にしたがって、層厚測定器により塗装層の厚さを決定した。厚さは90~110μmの範囲内であった。
さらに、4種の異なる腐食試験を実施した:
1.)60回を超えるVolkswagen仕様PV 1210(2010-02 version)による腐食サイクル試験、
2.)10回を超えるVDA試験シート621-415およびDIN EN ISO 20567-1(1982 version;method C)による腐食サイクル試験、
3.)DIN EN ISO 4628-8(2013-03 version)による腐食サイクル試験Meko S test c、および
4.)FFM_C-AN_01941(2.0 version)によるカソード分極
DIN EN ISO 4628-8(2012 version)にしたがって、腐食性剥離(mm)をそれぞれの場合において決定した(表4:「Cd」参照)。報告値は、それぞれの場合における3枚のシートの平均値である。
表4は、前すすぎ剤、化成処理浴および後すすぎ剤に本発明による樹脂混合物を添加することにより、腐食性剥離の減少が確認できることを示す(実施例の値と、比較例CE1、CE8およびCE27の値とを比較されたい)。
Claims (20)
- 鋼、亜鉛めっき鋼、アルミニウム、アルミニウム合金、マグネシウムおよび/または亜鉛-マグネシウム合金を含む金属表面を防食前処理するための方法であって、前記金属表面を、
i)a1)チタン化合物、ジルコニウム化合物およびハフニウム化合物からなる群から選択される少なくとも1種の化合物を含む酸性水性組成物A、ならびに
ii)b1)少なくとも1種の(メタ)アクリレート樹脂およびb2)少なくとも1種のフェノール樹脂を含む水性組成物B
と接触させ、
前記金属表面を、
i)第一に前記組成物Aと、次いで、前記組成物Bと、
ii)第一に前記組成物Bと、次いで、前記組成物Aと、または
iii)前記組成物Aおよび前記組成物Bと同時に
接触させる、方法であって、
前記少なくとも1種の(メタ)アクリレート樹脂b1)が、メタクリル酸エステルおよびアクリル酸のコポリマーである、方法。 - 金属表面を、第一に前記組成物Aと、次いで、前記組成物Bと接触させる、請求項1に記載の方法。
- 前記少なくとも1種の(メタ)アクリレート樹脂b1)が、メタクリル酸メチルおよびアクリル酸のコポリマーである、請求項1または2に記載の方法。
- 前記少なくとも1種の(メタ)アクリレート樹脂b1)が、80~98質量%のメタクリル酸メチルおよび2~20質量%のアクリル酸(合計:100質量%)を含む、請求項3に記載の方法。
- 前記少なくとも1種の(メタ)アクリレート樹脂b1)が、ヒドロキシル基、シリル基、アルキル基、アリール基、ヘテロアルキル基、ヘテロアリール基、チオ基、アミノ基、アミド基、ニトリル基、エポキシ基、メルカプト基、ウレイド基、ニトロ基、ハロ基および/またはシアノ基をさらに含む、請求項1から4のいずれか一項に記載の方法。
- 前記少なくとも1種の(メタ)アクリレート樹脂b1)が、1000~500000g/molの範囲内の質量平均分子量を有する、請求項1から5のいずれか一項に記載の方法。
- 前記少なくとも1種のフェノール樹脂b2)がレゾールである、請求項1から6のいずれか一項に記載の方法。
- 前記少なくとも1種のフェノール樹脂b2)が、100~5000g/molの範囲内の質量平均分子量を有する、請求項1から7のいずれか一項に記載の方法。
- 前記組成物Bが、1:1~10:1の質量比の前記成分b1)およびb2)を含む、請求項1から8のいずれか一項に記載の方法。
- 前記組成物B中のb1)およびb2)合計の濃度が、(固体添加として計算された)20~400mg/lの範囲内である、請求項1から9のいずれか一項に記載の方法。
- 前記組成物Bが、式I:
PEOx-PPOy-PEOz(I)
(式中、xおよびzは、それぞれの場合において、4~12の範囲内の整数であり、yは、35~65の範囲内の整数である)
の少なくとも1種のトリブロックコポリマーを安定剤b3)として含む、請求項1から10のいずれか一項に記載の方法。 - 前記組成物B中の前記安定剤b3)の(固体添加として計算された)質量濃度が、(メタ)アクリレート樹脂b1)およびフェノール樹脂b2)の総濃度の1.5~2.5倍である、請求項11に記載の方法。
- 前記組成物Bが、式II
R1O-(CH2)x-Z-(CH2)y-OR2(II)
(式中、R1およびR2は、それぞれの場合において、互いに独立してHまたはHO-(CH2)w-基(式中、w≧2)であり、xおよびyは、それぞれの場合において、互いに独立して1~4であり、Zは、硫黄原子またはC-C三重結合である)
の少なくとも1種の化合物b4)をさらに含む、請求項1から12のいずれか一項に記載の方法。 - 前記組成物Bが、さらなる成分b5)として少なくとも1種のモリブデン化合物を含む、請求項1から13のいずれか一項に記載の方法。
- 前記組成物A中の前記成分a1)が、チタン、ジルコニウムおよびハフニウムの錯フッ化物からなる群から選択される少なくとも1種の錯フッ化物である、請求項1から14のいずれか一項に記載の方法。
- 前記組成物Aが、a2)オルガノアルコキシシラン、オルガノシラノール、ポリオルガノシラノール、オルガノシロキサンおよびポリオルガノシロキサンからなる群から選択される少なくとも1種の化合物をさらに含む、請求項1から15のいずれか一項に記載の方法。
- 成分a2)が、オルガノアルコキシシラン/オルガノシラノール単位あたり少なくとも1個のアミノ基、尿素基、イミド基、イミノ基および/またはウレイド基をそれぞれの場合において有する少なくとも1種のオルガノアルコキシシラン、オルガノシラノール、ポリオルガノシラノール、オルガノシロキサンおよび/またはポリオルガノシロキサンである、請求項16に記載の方法。
- 前記組成物Aが、成分a3)として、0.1~5g/lの亜鉛カチオン、5~50mg/lの銅カチオンおよび/または5~50mg/lのセリウムカチオンおよび/または(モリブデンとして計算された)10~100mg/lの少なくとも1種のモリブデン化合物をさらに含む、請求項1から17のいずれか一項に記載の方法。
- 金属表面が、鋼および/または亜鉛めっき鋼を含む、請求項1から18のいずれか一項に記載の方法。
- 請求項1から19のいずれか一項に記載の方法により塗装された金属基材を、自動車産業における、鉄道車両用における、航空宇宙産業における、家庭用電気機器、制御装置または試験装置の装置構成における、機械工学における、建築産業における、または家具産業における、個々の構成部品、あらかじめ取り付けられた要素または連結された要素の生産用に使用するか、
ガードレール、ランプ、またはクラッディングの生産用に使用するか、
ボディーワークまたはボディーワーク部品の生産用に使用する、
方法。
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