JP5328981B2 - 化成処理めっき鋼板およびその製造方法 - Google Patents
化成処理めっき鋼板およびその製造方法 Download PDFInfo
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- JP5328981B2 JP5328981B2 JP2012520302A JP2012520302A JP5328981B2 JP 5328981 B2 JP5328981 B2 JP 5328981B2 JP 2012520302 A JP2012520302 A JP 2012520302A JP 2012520302 A JP2012520302 A JP 2012520302A JP 5328981 B2 JP5328981 B2 JP 5328981B2
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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
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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
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- C—CHEMISTRY; METALLURGY
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- 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
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- Y10T428/12—All metal or with adjacent metals
- Y10T428/12493—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.]
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- Y10T428/12542—More than one such component
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- Y10T428/12493—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.]
- Y10T428/12736—Al-base component
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Description
[1]Alを85〜99質量%含むAl系合金めっき鋼板と、前記Al系合金めっき鋼板の表面に形成された、膜厚0.5〜10μmの化成処理皮膜と、を有する化成処理Al系めっき鋼板であって;前記化成処理皮膜は、カルボキシル基、スルホン酸基およびこれらの塩からなる群から選ばれる親水性官能基0.05〜5質量%とF原子7〜20質量%とを含有するフッ素含有樹脂と、前記フッ素含有樹脂に対して金属換算で0.1〜5質量%の4A族金属化合物とを含有する、化成処理Al系めっき鋼板。
[2]前記フッ素含有樹脂が有するカルボキシル基とスルホン酸基との比率は、カルボキシル基/スルホン酸基のモル比で5〜60の範囲内である、[1]に記載の化成処理Al系めっき鋼板。
[3]前記化成処理皮膜は、さらにリン酸塩を含有し;前記フッ素含有樹脂に対する前記リン酸塩の量は、P換算で0.05〜3質量%の範囲内である、[1]または[2]に記載の化成処理Al系めっき鋼板。
[4]前記化成処理皮膜は、さらにシランカップリング剤を含有し;前記フッ素含有樹脂に対する前記シランカップリング剤の量は、0.5〜5質量%の範囲内である、[1]〜[3]のいずれか一項に記載の化成処理Al系めっき鋼板。
[5]前記4A族金属は、Ti、Zr、Hfおよびこれらの組み合わせからなる群から選ばれる、[1]〜[4]のいずれかに記載の化成処理Al系めっき鋼板。
[6]前記Al系合金めっき鋼板と、前記化成処理皮膜との間に形成された、バルブメタルの酸化物または水酸化物、およびバルブメタルのフッ化物を含有する下地化成処理皮膜をさらに有する、[1]〜[5]のいずれか一項に記載の化成処理Al系めっき鋼板。
[7]Alを85〜99質量%含むAl系合金めっき鋼板を準備するステップと、前記Al系合金めっき鋼板の表面に化成処理液を塗布し、乾燥させて、膜厚が0.5〜10μmの化成処理皮膜を形成するステップとを含み;前記化成処理液は、カルボキシル基、スルホン酸基およびこれらの塩からなる群から選ばれる親水性官能基0.05〜5質量%とF原子7〜20質量%とを含有し、数平均分子量が1000〜200万の範囲内であるフッ素含有樹脂と、4A族金属の酸素酸塩、フッ化物、水酸化物、有機酸塩、炭酸塩または過酸化塩のいずれかとを含有し、かつ前記フッ素含有樹脂に対する、前記4A族金属の酸素酸塩、フッ化物、水酸化物、有機酸塩、炭酸塩または過酸化塩の量は、金属換算で0.1〜5質量%の範囲内である、化成処理Al系めっき鋼板の製造方法。
[8]前記フッ素含有樹脂が有するカルボキシル基とスルホン酸基との比率は、カルボキシル基/スルホン酸基のモル比で5〜60の範囲内である、[7]に記載の化成処理Al系めっき鋼板の製造方法。
[9]前記化成処理液は、さらにリン酸塩を含有し;前記フッ素含有樹脂に対する前記リン酸塩の量は、P換算で0.05〜3質量%の範囲内である、[7]または[8]に記載の化成処理Al系めっき鋼板の製造方法。
[10]前記化成処理液は、さらにシランカップリング剤を含有し;前記フッ素含有樹脂に対する前記シランカップリング剤の量は、0.5〜5質量%の範囲内である、[7]〜[9]のいずれか一項に記載の化成処理Al系めっき鋼板の製造方法。
[11]前記4A族金属は、Ti、Zr、Hfおよびこれらの組み合わせからなる群から選ばれる、[7]〜[10]のいずれか一項に記載の化成処理Al系めっき鋼板の製造方法。
[12]前記化成処理皮膜を形成するステップの前に、前記Al系合金めっき鋼板の表面に下地化成処理液を塗布し、乾燥させて、下地化成処理皮膜を形成するステップをさらに含み;前記下地化成処理液は、バルブメタル塩とフッ化物イオンとを含有する、[7]〜[11]のいずれか一項に記載の化成処理Al系めっき鋼板の製造方法。
本発明の化成処理Al系めっき鋼板は、Al系合金めっき鋼板(化成処理原板)と、Al系合金めっき鋼板の表面に形成された化成処理皮膜とを有する。本発明の化成処理Al系めっき鋼板は、化成処理皮膜が親水性官能基(カルボキシル基やスルホン酸基など)を導入した高分子量のフッ素含有樹脂および4A族金属化合物を含むことを一つの特徴とする。
化成処理原板としては、耐食性および意匠性に優れる、Al系合金めっき鋼板が使用される。ここで「Al系合金めっき鋼板」とは、Alを85〜99質量%含み、残部が実質的にSiのAl系合金めっき層を有する鋼板を意味する。Al系合金めっき鋼板の例には、溶融Al−9%Siめっき鋼板などが含まれる。
化成処理原板として使用されるAl系合金めっき鋼板の表面には、バルブメタルの酸化物または水酸化物と、バルブメタルのフッ化物とを含有する下地化成処理皮膜が形成されている場合もある。このように、Al系合金めっき鋼板の表面に下地化成処理皮膜が形成されている場合、化成処理皮膜は、下地化成処理皮膜を介してAl系合金めっき鋼板の表面に形成される。
化成処理皮膜は、上述のAl系合金めっき鋼板(化成処理原板)の表面に形成されている。化成処理原板の表面には、下地となる皮膜を形成するなどの下地化成処理をしてもよいが、下地化成処理をしなくてもよい。なお、化成処理原板の表面に下地化成処理をしない場合には、化成処理原板の表面には化成処理皮膜が直接形成される。この化成処理皮膜は、Al系合金めっき鋼板の耐候性や耐水性などを向上させる。
化成処理皮膜は、フッ素含有樹脂、より具体的にはフッ素含有オレフィン樹脂を主成分として含む。化成処理皮膜に主成分として含まれるフッ素含有樹脂の量は、70〜99質量%の範囲内が好ましい。前述の通り、化成処理皮膜を構成する有機樹脂としてフッ素含有樹脂を用いることで、化成処理皮膜の耐候性(耐紫外線性)を向上させることができる。
化成処理皮膜は、4A族金属化合物を含む。4A族金属化合物は、水系フッ素含有樹脂中のカルボキシル基やスルホン酸基などの官能基と反応しやすく、水系フッ素含有樹脂の硬化または架橋反応を促進する。そのため、低温乾燥でも化成処理皮膜の耐水性を向上させることができる。
化成処理皮膜は、さらにリン酸塩を含むことが好ましい。リン酸塩は、Al系合金めっき鋼板のめっき層表面と反応して、化成処理皮膜のAl系合金めっき鋼板への密着性を向上させる。
化成処理皮膜は、さらにシランカップリング剤を含むことが好ましい。シランカップリング剤を配合することで、化成処理皮膜の密着性をより向上させることができる。シランカップリング剤としては、アミノ基、エポキシ基、メルカプト基、アクリロキシ基、メタクリロキシ基、アルコキシ基、ビニル基、スチリル基、イソシアネート基、クロロプロピル基などの官能基を1種類または2種類以上含むシラン化合物が使用される。
本発明の化成処理Al系めっき鋼板の製造方法は、特に限定されないが、例えば以下の方法により製造されうる。
第1のステップでは、化成処理原板として前述のAl系合金めっき鋼板を準備する。
第2のステップでは、前述の親水性官能基を有するフッ素含有樹脂(好ましくは、フッ素含有オレフィン樹脂)と4A族金属化合物とを含む化成処理液を準備する。
第3のステップでは、第1のステップで準備したAl系合金めっき鋼板の表面に、化成処理皮膜を形成する。化成処理皮膜を形成するには、第2のステップで準備した化成処理液を第1のステップで準備したAl系合金めっき鋼板の表面に塗布し、乾燥させればよい。
下地化成処理皮膜を形成するステップでは、化成処理皮膜を形成する前に、第1のステップで準備したAl系合金めっき鋼板の表面に下地化成処理液を塗布して塗布膜を形成する。下地化成処理液は、例えば、ロールコート法、スピンコート法、スプレー法などなどで塗布することができる。下地化成処理液の塗布量は、バルブメタル付着量が1mg/m2以上となるように調整することが好ましい。得られる化成処理鋼板に十分な耐食性を付与するためである。また、下地化成処理液の塗布量は、形成される下地化成処理皮膜の厚さが3nm以上1000nm以下となるように調整することが好ましい。3nm以上で十分な耐食性が発現し、1000nmを超えると鋼板を成形加工しようとするときに、応力によってクラックが発生するおそれがある。
1.化成処理Al系めっき鋼板の作製(1)
板厚0.8mmのSPCCを基材として、溶融Al−9質量%Si合金めっき鋼板(めっき付着量45g/m2)を作製した。本実施例では、この溶融Al−9質量%Si合金めっき鋼板を化成処理原板として使用した。
(1)促進耐候性試験
各化成処理Al系めっき鋼板から試験片を切り出し、JIS K5600−7−7:2008に準拠して促進耐候性試験(キセノンランプ法)を実施した。本試験では、キセノンアーク灯の光を120分間照射する間に18分間水を噴射する工程を1サイクル(2時間)とし、この工程を0〜1000サイクル(0、500、1000サイクル)繰り返した。
各化成処理Al系めっき鋼板について、促進耐候試験前後の化成処理皮膜の厚さを断面検鏡により測定し、塗膜残存率を求めた。各化成処理Al系めっき鋼板について、塗膜残存率が95%以上の場合は「◎」、80%以上95%未満の場合は「○」、60%以上80%未満の場合は「△」、30%以上60%未満の場合は「▲」、30%未満の場合は「×」と評価した。
各化成処理Al系めっき鋼板について、促進耐候試験前後の試験片(サイズ:30mm×150mm)を用いてドロービード試験(金型のビード高さ:4mm、加圧力:1.0kN)した後、金型が摺動した部分の皮膜残存率を計測した。皮膜残存率が95%以上の場合は「◎」、80%以上95%未満の場合は「○」、60%以上80%未満の場合は「△」、30%以上60%未満の場合は「▲」、30%未満の場合は「×」と評価した。
各化成処理Al系めっき鋼板について、促進耐候試験後の試験片を用いて塩水噴霧試験(JIS Z2371に準拠;120時間)を行い、平坦部の白錆発生面積率を評価した。各化成処理Al系めっき鋼板について、白錆発生面積率が5%以下の場合は「◎」、5%を超え10%以下の場合は「○」、10%を超え30%以下の場合は「△」、30%を超え50%以下の場合は「▲」、50%を超える場合は「×」と評価した。
各化成処理Al系めっき鋼板(実施例1〜6、参考例1、比較例1〜4)についての、使用した処理液の種類、ならびに耐候性試験、皮膜密着性試験および平坦部耐食性試験の評価結果を表4に示す。
(1)下地化成処理皮膜の形成
前述のAl系合金めっき鋼板の表面に、表5に示す組成の下地化成処理液を塗布した後、到達板温70〜170℃で加熱乾燥して下地化成処理皮膜を形成した。蛍光X線分析装置を使用し、形成された下地化成処理皮膜の組成を分析した。結果を表6に示す。
形成された下地化成処理皮膜の表面に前述の処理液No.7の化成処理液を塗布し、到達板温140℃で加熱乾燥して、膜厚2.0μmの化成処理皮膜を形成した。
前述の「化成処理Al系めっき鋼板の評価(1)」と同様の手法により、作製した化成処理Al系めっき鋼板について促進耐候性試験を実施した。そして、作製した化成処理Al系めっき鋼板の耐候性、耐黒変性、ならびに平坦部およびクロスカット部の耐食性を評価した。評価結果を表7に示す。クロスカット部の耐食性については、以下に示す手順で評価した。
各化成処理Al系めっき鋼板について、促進耐候試験後、X字型の切り込み部(クロスカット部)を表面に形成して、めっき層を露出させた。試験片を得た。得られた試験片に塩水噴霧試験(JIS Z2371に準拠;120時間)を行い、クロスカット部の白錆発生面積率を評価した。各化成処理Zn系めっき鋼板について、白錆発生面積率が5%以下の場合は「◎」、5%を超え10%以下の場合は「○」、10%を超え30%以下の場合は「△」、30%を超え50%以下の場合は「▲」、50%を超える場合は「×」と評価した。
参考実験として、フッ素樹脂皮膜中の4A族金属化合物の量および乳化剤の量と、透湿度との関係を調べた結果を示す。
Claims (10)
- Alを85〜99質量%含むAl系合金めっき鋼板と、
前記Al系合金めっき鋼板の表面に形成された、膜厚0.5〜10μmの化成処理皮膜と、を有する化成処理Al系めっき鋼板であって、
前記化成処理皮膜は、カルボキシル基、スルホン酸基およびこれらの塩からなる群から選ばれる親水性官能基0.05〜5質量%とF原子7〜20質量%とを含有するフッ素含有樹脂と、前記フッ素含有樹脂に対して金属換算で0.1〜5質量%の4A族金属化合物とを含有し、
前記フッ素含有樹脂が有するカルボキシル基とスルホン酸基との比率は、カルボキシル基/スルホン酸基のモル比で5〜60の範囲内である、
化成処理Al系めっき鋼板。 - 前記化成処理皮膜は、さらにリン酸塩を含有し、
前記フッ素含有樹脂に対する前記リン酸塩の量は、P換算で0.05〜3質量%の範囲内である、
請求項1に記載の化成処理Al系めっき鋼板。 - 前記化成処理皮膜は、さらにシランカップリング剤を含有し、
前記フッ素含有樹脂に対する前記シランカップリング剤の量は、0.5〜5質量%の範囲内である、
請求項1に記載の化成処理Al系めっき鋼板。 - 前記4A族金属は、Ti、Zr、Hfおよびこれらの組み合わせからなる群から選ばれる、請求項1に記載の化成処理Al系めっき鋼板。
- 前記Al系合金めっき鋼板と、前記化成処理皮膜との間に形成された、
Ti、Zr、Hf、V、Nb、Ta、MoおよびWからなる群から選ばれるバルブメタルの酸化物または水酸化物、ならびにTi、Zr、Hf、V、Nb、Ta、MoおよびWからなる群から選ばれるバルブメタルのフッ化物を含有する下地化成処理皮膜をさらに有する、請求項1に記載の化成処理Al系めっき鋼板。 - Alを85〜99質量%含むAl系合金めっき鋼板を準備するステップと、
前記Al系合金めっき鋼板の表面に化成処理液を塗布し、乾燥させて、膜厚が0.5〜10μmの化成処理皮膜を形成するステップとを含み、
前記化成処理液は、カルボキシル基、スルホン酸基およびこれらの塩からなる群から選ばれる親水性官能基0.05〜5質量%とF原子7〜20質量%とを含有し、数平均分子量が1000〜200万の範囲内であるフッ素含有樹脂と、4A族金属の酸素酸塩、フッ化物、水酸化物、有機酸塩、炭酸塩または過酸化塩のいずれかとを含有し、かつ
前記フッ素含有樹脂に対する、前記4A族金属の酸素酸塩、フッ化物、水酸化物、有機酸塩、炭酸塩または過酸化塩の量は、金属換算で0.1〜5質量%の範囲内であり、
前記フッ素含有樹脂が有するカルボキシル基とスルホン酸基との比率は、カルボキシル基/スルホン酸基のモル比で5〜60の範囲内である、
化成処理Al系めっき鋼板の製造方法。 - 前記化成処理液は、さらにリン酸塩を含有し、
前記フッ素含有樹脂に対する前記リン酸塩の量は、P換算で0.05〜3質量%の範囲内である、
請求項6に記載の化成処理Al系めっき鋼板の製造方法。 - 前記化成処理液は、さらにシランカップリング剤を含有し、
前記フッ素含有樹脂に対する前記シランカップリング剤の量は、0.5〜5質量%の範囲内である、
請求項6に記載の化成処理Al系めっき鋼板の製造方法。 - 前記4A族金属は、Ti、Zr、Hfおよびこれらの組み合わせからなる群から選ばれる、請求項6に記載の化成処理Al系めっき鋼板の製造方法。
- 前記化成処理皮膜を形成するステップの前に、前記Al系合金めっき鋼板の表面に下地化成処理液を塗布し、乾燥させて、下地化成処理皮膜を形成するステップをさらに含み、
前記下地化成処理液は、Ti、Zr、Hf、V、Nb、Ta、MoおよびWからなる群から選ばれるバルブメタルの塩とフッ化物イオンとを含有する、
請求項6に記載の化成処理Al系めっき鋼板の製造方法。
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