JP7443253B2 - 複合金属構造体の選択的リン酸塩処理方法 - Google Patents
複合金属構造体の選択的リン酸塩処理方法 Download PDFInfo
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- JP7443253B2 JP7443253B2 JP2020566876A JP2020566876A JP7443253B2 JP 7443253 B2 JP7443253 B2 JP 7443253B2 JP 2020566876 A JP2020566876 A JP 2020566876A JP 2020566876 A JP2020566876 A JP 2020566876A JP 7443253 B2 JP7443253 B2 JP 7443253B2
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- Prior art keywords
- zinc phosphate
- phosphate treatment
- ions
- zinc
- composition
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- 238000011282 treatment Methods 0.000 title claims description 94
- 229910052751 metal Inorganic materials 0.000 title claims description 79
- 239000002184 metal Substances 0.000 title claims description 79
- 238000000034 method Methods 0.000 title claims description 68
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- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 title claims description 55
- 229910019142 PO4 Inorganic materials 0.000 title claims description 52
- 239000010452 phosphate Substances 0.000 title claims description 48
- 239000000203 mixture Substances 0.000 claims description 125
- LRXTYHSAJDENHV-UHFFFAOYSA-H zinc phosphate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O LRXTYHSAJDENHV-UHFFFAOYSA-H 0.000 claims description 100
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- 150000001875 compounds Chemical class 0.000 claims description 29
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- 229910010272 inorganic material Inorganic materials 0.000 claims description 25
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- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 11
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- 150000003839 salts Chemical class 0.000 description 4
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- 229910002651 NO3 Inorganic materials 0.000 description 3
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 3
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- QGHDLJAZIIFENW-UHFFFAOYSA-N 4-[1,1,1,3,3,3-hexafluoro-2-(4-hydroxy-3-prop-2-enylphenyl)propan-2-yl]-2-prop-2-enylphenol Chemical group C1=C(CC=C)C(O)=CC=C1C(C(F)(F)F)(C(F)(F)F)C1=CC=C(O)C(CC=C)=C1 QGHDLJAZIIFENW-UHFFFAOYSA-N 0.000 description 1
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- IRXRGVFLQOSHOH-UHFFFAOYSA-L dipotassium;oxalate Chemical compound [K+].[K+].[O-]C(=O)C([O-])=O IRXRGVFLQOSHOH-UHFFFAOYSA-L 0.000 description 1
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- VSZWPYCFIRKVQL-UHFFFAOYSA-N selanylidenegallium;selenium Chemical compound [Se].[Se]=[Ga].[Se]=[Ga] VSZWPYCFIRKVQL-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
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Description
3Na+(aq)+Al3+(aq)+6F-(aq)→Na3AlF6(s)↓または
リン酸塩処理組成物中のナトリウムイオンは、添加剤に、例えば特に、添加剤および/または促進剤に由来する。ここで、特に言及すべき添加剤は、フッ化ナトリウム、硝酸ナトリウム、リン酸ナトリウムおよび水酸化ナトリウムであり、特に言及すべき促進剤は、亜硝酸ナトリウムである。同じことが、カリウムイオンにも当てはまる。これらの添加剤は、状況および既存の浴パラメータに応じて浴に添加する。対照的にアルミニウムイオンは、リン酸塩処理浴組成物の酸性媒体中で酸洗いすることにより、複合金属構造体のアルミニウム部分から除去される。
(I) 第1の工程で、鉄および亜鉛で作られた部分上に0.5~5g/m2の範囲のコーティング質量を有する、表面を覆う結晶性リン酸亜鉛層の形成をもたらすが、アルミニウム部分上に少なくとも0.5g/m2のコーティング質量を有するリン酸亜鉛層を生成しない、水性リン酸亜鉛処理組成物を用いた複合金属構造体の処理、および次いで中間水すすぎ操作を行って、
(II) 第2の工程で、2.0~5.5の範囲のpHを有する水性酸性不動態化組成物の複合金属構造体への施与を含み、酸性不動態化組成物が、亜鉛および鉄で作られた部分上で結晶性リン酸亜鉛の50%以下を除去するが、表面を覆う結晶性リン酸塩層を構成していないアルミニウム部分上に不動態層を形成し、
工程(I)におけるリン酸亜鉛処理組成物が、ナトリウムイオンおよび/またはカリウムイオンの、およびアルミニウムイオンの含有量を含み、
工程(I)におけるリン酸亜鉛処理組成物が、20~65℃の範囲の温度を有し、少なくとも5mg/lであるが200mg/lを超えない遊離フッ化物含有量を含み、
少なくとも0.04g/lであるが3.2g/l以下の、BF4として計算される水溶性無機化合物の形態のホウ素がリン酸亜鉛処理組成物中に存在し、および
リン酸亜鉛処理組成物中の、KClが添加された遊離酸のポイント数が、少なくとも0.6ポイントである。
本発明の文脈における「複合金属構造体」とは、ハイブリッド組成物の金属構成要素、特にシャーシである。複合金属構造体は、亜鉛の表面、アルミニウムの表面、および任意の鉄の表面と同様に、他の金属の表面および/または非金属、特にプラスチックの表面を有してもよい。
10mLのリン酸塩処理組成物を、適した容器、例えば300mLの三角フラスコにピペットで入れる。リン酸塩処理組成物が錯体フッ化物を含む場合、追加の塩化カリウム6~8gを試料に加える。次いで、pHメーターおよび電極を使用して、0.1 M NaOHで滴定を行い、pHを4.0にする。この滴定で消費される0.1 M NaOHの量(リン酸塩処理組成物10mlあたりのmlで表す)は、KCl(FA、KCl)が添加された遊離酸価を、ポイントで表す。
複合金属構造体の表面における酸性酸洗い浸食の場合、プロトンは水素に還元されるという点で消費される。これによって、表面でpHが上昇する。今回本発明の文脈において、驚くべきことに、ヘキサフルオロシリケートなどのフルオロシリケートは、pHが上昇すると、フッ化物イオン(遊離フッ化物)を、テトラフルオロボレートなどの対応するフルオロボレートよりも著しく大幅に放出することが見出された。それ故、フルオロシリケートの場合、表面でフッ化物イオンの含有量がさらにより著しく増加し、ナトリウム/カリウムおよびアルミニウムイオンの適切な含有量がもたらされると、最終的には対応するクリオライトの析出の増加を引き起こす(質量作用の法則を参照)。
(A値×T)/(Ftot.×[B]×1000)
(式中、「T」は温度/℃、「Ftot.」は総フッ化物含有量/(mol/l)、および「[B]」は元素ホウ素の濃度/(mol/l)を表す)が、0.13~22.5、好ましくは0.2~15、およびより好ましくは0.4~10の範囲にあるときに、特に効率的に低減できることが見出された。
遊離酸(希釈酸)(FA(dil.))
(W.Rausch「Die Phosphatierung von Metallen」、Eugen G.Leuze Verlag、第3版、2005年、セクション8.1、第333~334頁参照)
遊離酸(希釈)の決定のため、10mlのリン酸塩処理組成物を、300mlの三角フラスコなどの適した容器にピペットを使って入れる。次いで、150mlの完全脱塩水を添加する。pH計及び電極を使用して、4.7のpHになるまで0.1M NaOHによる滴定を実施する。この滴定において消費された0.1M NaOHの、希釈したリン酸塩処理組成物10ml当たりのmlで表す量により、遊離酸(希釈)(FA(dil.))の値がポイントで得られる。
(W.Rausch「Die Phosphatierung von Metallen」、Eugen G.Leuze Verlag、第3版、2005年、セクション8.2、第334~336頁参照)
遊離酸(希釈)の測定に続き、希釈したリン酸塩処理組成物をシュウ酸カリウム溶液に添加した後、pH計及び電極を使用して、8.9のpHになるまで0.1M NaOHによって滴定する。この手順において、希釈したリン酸塩処理組成物10ml当たりのmlで表す0.1M NaOHの消費量により、フィッシャー総酸(TAF)がポイントで得られる。
(W.Rausch「Die Phosphatierung von Metallen」、Eugen G.Leuze Verlag、第3版、2005年、セクション8.3、第336~338頁参照)
総酸(TA)は、存在する二価カチオン、及び遊離したリン酸及び結合したリン酸(後者はホスフェートである)の合計である。総酸は、pH計及び電極を使用して、0.1M NaOHの消費量によって測定される。この目的のために、10mlのリン酸塩処理組成物を、300mlの三角フラスコなどの適した容器にピペットを使って入れ、25mlの完全脱塩水によって希釈する。これに続いて、pH9になるように0.1M NaOHによる滴定を実施する。この手順の間の、希釈したリン酸塩処理組成物10ml当たりのmlで表す消費量が、総酸(TA)のポイント数に対応する。
(W.Rausch「Die Phosphatierung von Metallen」、Eugen G.Leuze Verlag、第3版、2005年、セクション8.4、第338頁参照)
酸価(A値)と呼ばれるものは、KClが添加された遊離酸のフィッシャー総酸に対する比、すなわち(FA、KCl):FTAの比を表し、遊離酸(FA)の数値をフィッシャー総酸値(FTA)で除することによって得られる。
- 0.07~0.25g/lの亜硝酸塩(亜硝酸ナトリウムとして計算される)、
- 約0.1~2g/lのニトログアニジン、
- 8~51mg/lの過酸化水素。
- 0~2g/lの硫酸塩、
- 0.01~500mg/l(ニッケルを含まないリン酸亜鉛処理組成物の場合)または0.01~20g/l(ニッケルを含有するリン酸亜鉛処理組成物の場合)の硝酸塩。
- 0.3~2g/l、好ましくは0.5~1.5g/lのマンガン(II)、
- 0.3~2g/l、好ましくは0.8~1.2g/lのニッケル(II)、
- 0.001~0.2g/l、好ましくは0.005~0.1g/lの鉄(III)。
(a) P2O5として計算して5~50g/lのリン酸イオン、
(b) 0.3~3g/lの亜鉛イオン、
(c) 少なくとも5mg/lであるが200mg/l以下の遊離フッ化物、および
(d) 少なくとも0.04g/lであるが3.2g/l以下のBF4として計算される水溶性無機化合物の形態のホウ素
を有し、
そのリン酸亜鉛処理組成物が、ナトリウムイオンおよび/またはカリウムイオンおよびアルミニウムイオンの含有量をさらに含む。
(A値×T)/(Ftot.×[B]×1000)
(式中、「T」は温度/℃、「Ftot.」は総フッ化物含有量/(mol/l)、および「[B]」は元素ホウ素の濃度/(mol/l)を表す)が、0.13~22.5、好ましくは0.2~15、およびより好ましくは0.4~10の範囲にあるときに、特に効率的に低減できることが見出された。
Claims (12)
- アルミニウムで作られた少なくとも一部分と、亜鉛で作られた少なくとも一部分と、任意の、鉄で作られたさらなる部分とを含む複合金属構造体の化学的前処理および選択的リン酸塩処理の方法であって、
(I) 第1の工程で、前記鉄で作られた部分および前記亜鉛で作られた部分上に0.5~5g/m2の範囲のコーティング質量を有する、表面を覆う結晶性リン酸亜鉛層の形成をもたらすが、前記アルミニウム部分上に少なくとも0.5g/m2のコーティング質量を有するリン酸亜鉛層を生成しない、水性リン酸亜鉛処理組成物を用いた前記複合金属構造体の処理、および次いで中間水すすぎ操作を行って、
(II) 第2の工程で、2.0~5.5の範囲のpHを有する水性酸性不動態化組成物の前記複合金属構造体への施与
を含み、前記酸性不動態化組成物が、前記亜鉛で作られた部分および前記鉄で作られた部分上で前記結晶性リン酸亜鉛の50%以下を除去するが、表面を覆う結晶性リン酸塩層を構成していない前記アルミニウム部分上に不動態層を形成し、
工程(I)におけるリン酸亜鉛処理組成物が、ナトリウムイオンおよび/またはカリウムイオンの、およびアルミニウムイオンの含有量を含み、
工程(I)におけるリン酸亜鉛処理組成物が、20~65℃の範囲の温度を有し、少なくとも5mg/lであるが200mg/lを超えない遊離フッ化物含有量を含み、
少なくとも0.04g/lであるが3.2g/l以下の、BF4として計算される水溶性無機化合物の形態のホウ素が前記リン酸亜鉛処理組成物中に存在し、および
前記リン酸亜鉛処理組成物中の、KClが添加された遊離酸のポイント数が少なくとも0.6ポイントであり、且つ
工程(I)におけるリン酸亜鉛処理組成物中のナトリウムイオンおよび/またはカリウムイオン(ナトリウムとして計算する)の含有量が、1~4g/lの範囲にあり、前記遊離フッ化物含有量が50~150mg/lの範囲にあり、且つ
工程(I)におけるリン酸亜鉛処理組成物中のケイ素(SiF 6 として計算される)を含む無機化合物の含有量が、25mg/l未満である、方法。 - 工程(I)におけるリン酸亜鉛処理組成物が、10~200mg/lの範囲の遊離フッ化物含有量を有する、請求項1に記載の方法。
- 工程(I)におけるリン酸亜鉛処理組成物が、BF4として計算される水溶性無機化合物の形態のホウ素を、0.08~2g/lの範囲の濃度で有する、請求項1または2に記載の方法。
- 工程(I)におけるリン酸亜鉛処理組成物が、0.6~3.0ポイントの範囲のKClが添加された遊離酸のポイント数を有する、請求項1から3のいずれか一項に記載の方法。
- 工程(I)におけるリン酸亜鉛処理組成物について、無次元商
(A値×T)/(Ftot.×[B]×1000)
が、0.13~22.5の範囲にある、請求項1から4のいずれか一項に記載の方法。 - 工程(I)におけるリン酸亜鉛処理組成物が、以下のカチオンのうちの1種以上
- 0.3~2g/lのマンガン(II)、
- 0.3~2g/lのニッケル(II)、
- 0.001~0.2g/lの鉄(III)
をさらに含む、請求項1から5のいずれか一項に記載の方法。 - 工程(II)における不動態化組成物のpHが、2.5~5.5の範囲にある、請求項1から6のいずれか一項に記載の方法。
- 工程(II)における不動態化組成物が、Ti、Zrおよび/またはHfを錯化した形態で、20~500mg/l(Ti、Zrおよび/またはHfとして計算される)の範囲の濃度で、および任意のさらなる金属イオンを、水溶性化合物の形態で含む、請求項1から7のいずれか一項に記載の方法。
- 工程(II)における不動態化組成物が、少なくとも1種のオルガノシランおよび/または少なくとも1種のその加水分解生成物、および/または少なくとも1種のその縮合生成物を、5~200mg/l(Siとして計算される)の範囲の濃度でさらに含む、請求項1から8のいずれか一項に記載の方法。
- 請求項1~6のいずれか一項に記載の方法に使用するためのリン酸亜鉛処理組成物であって、
KClが添加された遊離酸の少なくとも0.6ポイントのポイント数、および
(a) P2O5として計算して5~50g/lのリン酸イオン、
(b) 0.3~3g/lの亜鉛イオン、
(c) 少なくとも50mg/lであるが150mg/l以下の遊離フッ化物、および
(d) 少なくとも0.04g/lであるが3.2g/l以下のBF4として計算される水溶性無機化合物の形態のホウ素
を有し、
前記リン酸亜鉛処理組成物が、ナトリウムイオンおよび/またはカリウムイオン(ナトリウムとして計算する)の含有量を1~4g/lの範囲に含み、およびアルミニウムイオンの含有量をさらに含む、リン酸亜鉛処理組成物。 - 適した溶媒および/または分散媒で希釈し、および任意にNaOHを使用してpHを調整することによって請求項10に記載のリン酸亜鉛処理組成物を得ることができる、濃縮物。
- アルミニウムで作られた少なくとも一部分と、亜鉛で作られた少なくとも一部分と、任意の、鉄で作られたさらなる部分とを含み、請求項1から9のいずれか一項に記載の方法によって得ることができる、複合金属構造体の、自動車部品メーカー産業に、自動車製造の車体構造に、農業用機械構造に、造船に、建設部門または白物製品の製造における使用方法。
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