JP7447245B2 - 優れた耐黒変性及び耐アルカリ性を付与する三元系溶融亜鉛合金めっき鋼板用表面処理組成物、これを用いて表面処理された三元系溶融亜鉛合金めっき鋼板及びその製造方法 - Google Patents
優れた耐黒変性及び耐アルカリ性を付与する三元系溶融亜鉛合金めっき鋼板用表面処理組成物、これを用いて表面処理された三元系溶融亜鉛合金めっき鋼板及びその製造方法 Download PDFInfo
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- JP7447245B2 JP7447245B2 JP2022518825A JP2022518825A JP7447245B2 JP 7447245 B2 JP7447245 B2 JP 7447245B2 JP 2022518825 A JP2022518825 A JP 2022518825A JP 2022518825 A JP2022518825 A JP 2022518825A JP 7447245 B2 JP7447245 B2 JP 7447245B2
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- zinc alloy
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- BSVBQGMMJUBVOD-UHFFFAOYSA-N trisodium borate Chemical compound [Na+].[Na+].[Na+].[O-]B([O-])[O-] BSVBQGMMJUBVOD-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
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- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D2503/00—Polyurethanes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D2518/00—Other type of polymers
- B05D2518/10—Silicon-containing polymers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G2150/00—Compositions for coatings
- C08G2150/90—Compositions for anticorrosive coatings
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/22—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen
- C08G77/26—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen nitrogen-containing groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/28—Nitrogen-containing compounds
- C08K2003/282—Binary compounds of nitrogen with aluminium
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
- C08K2003/3009—Sulfides
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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
- 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
200mgKOH/gであることが好ましい。上記ポリエステルポリオールまたはポリカ
ーボネートポリオールの水酸基値が80mgKOH/g未満である場合、水分散安定性が
低下し、無機化合物との反応のための官能基部位(site)が不足することで、要求さ
れる物性を確保し難いことができる。一方、水酸基値が200mgKOH/gを超える場
合、水分散安定性は優れるものの、皮膜転造後の耐水性、耐食性及びアルカリ脱脂性が低
下する問題が発生する可能性がある。上記ポリエステルポリオールまたはポリカーボネー
トポリオールの水酸基値は、例えば、80~180mgKOH/g、80~150mgKOH/g、100~200mgKOH/g、100~150mgKOH/gであり、より好ましくは100~150mgKOH/gである。
成物内に存在する残留酸を制御することにより、耐黒変性の低下及び耐食性の低下を防止
するために添加され、カルボジイミド系化合物及びオキサゾリン系化合物から選択された1種以上が用いられることができる。
(試験及び評価方法)
本実施例で表面処理された鋼板の物性評価の方法及び評価基準は、以下のとおりである。
ASTM B117に規定した方法に基づいて、試験片を処理した後、経時による鋼板
の白錆発生率を測定した。この時、評価基準は以下のとおりである。
◎:白錆発生時間が144時間以上
〇:白錆発生時間が96時間以上144時間未満
△:白錆発生時間が55時間以上96時間未満
×:白錆発生時間が55時間未満
試験片をエリクセン試験機(Erichsen tester)を用いて6mmの高さ
に押し上げた後、48時間経過したときに白錆発生程度を測定した。この時、評価基準は
以下のとおりである。
◎:48時間経過後に白錆発生が5%未満
△:48時間経過後に白錆発生が5%以上7%未満
×:48時間経過後に白錆発生が7%以上
試験片を50℃、相対湿度95%が維持される恒温恒湿器に120時間放置することにより、試験前/後の試験片の色変化(色差:ΔE)を観察した。この時、評価基準は以下のとおりである。
◎:ΔE≦2
〇:2<ΔE≦3
△:3<ΔE≦4
×:ΔE>4
試験片をアルカリ脱脂溶液に60℃、2分間浸漬後に水洗、Air blowing後の前/後の色差(ΔE)を測定した。アルカリ脱脂溶液は、大韓パーカライジング社のFinecleaner L 4460 A:20g/2.4L+L 4460 B 12g/2.4L(pH=12)を用いた。この時、評価基準は以下のとおりである。
◎:ΔE≦2
〇:2<ΔE≦3
△:3<ΔE≦4
×:ΔE>4
溶接性は、空圧式AC Spot溶接機を用いて加圧力250kg、溶接時間15Cycle、通電電流は7.5kAでSpatterがなく、一定の強度を維持するから評価した。この時、評価基準は以下のとおりである。
〇:溶接可能
△:溶接は可能であるが品質不良
×:溶接不可能
製造された表面処理溶液組成物200ミリリットルを50℃の温度のオーブンに保管した後、7日経過後の沈殿またはゲル発生の有無を観察して評価した。この時、評価基準は以下のとおりである。
〇:良好
×:不良
水溶性ポリウレタン樹脂でポリエステルポリオールの水酸基価が120mgKOH/gであり、重量平均分子量が3,000であるカチオンポリウレタン樹脂、3種のシラン化合物が架橋結合されたシラン系ゾル-ゲル樹脂でメチルトリエトキシシランと3-グリシドキシプロピルトリメトキシシラン及びN-(2-アミノエチル)3-アミノプロピルトリエトキシシランを用いた重合物、硬化剤としてメラミン硬化剤(CYMEL 303)、防錆耐食剤としてバナジウム系防錆剤、モリブデン系化合物としてモリブデン硫化物、シランカップリング剤として2-パーフルオロオクチルエチルトリメトキシシラン、有機金属錯体化合物としてチタン系化合物、酸除去剤としてオキサゾリン系酸除去剤、アルミニウム系化合物としてアルミニウムニトリド、潤滑剤としてポリエチレン-テフロン(登録商標)ワックスを固形分100重量%に対して、表1に示した含有量で用い、上記固形分を溶媒として水81.4重量%及びエタノール3.4重量%と混合して表面処理溶液組成物を製造した。
実施例1と同一組成成分を固形分100重量部基準で表2に示した含有量で用い、上記固形分を溶媒として水81.4重量%及びエタノール3.4重量%と混合して表面処理溶液組成物を製造した。
実施例1と同一組成成分を固形分100重量部基準で表3に示した含有量で用い、上記固形分を溶媒として水81.4重量%及びエタノール3.4重量%と混合して表面処理溶液組成物を製造した。
実施例1と同一組成成分を固形分100重量部基準で表4に示した含有量で用い、上記固形分を溶媒として水81.4重量%及びエタノール3.4重量%と混合して表面処理溶液組成物を製造した。
実施例1と同一組成成分を固形分100重量部基準で表5に示した含有量で用い、上記固形分を溶媒として水81.4重量%及びエタノール3.4重量%と混合して表面処理溶液組成物を製造した。
実施例1と同一組成成分を固形分100重量部基準で表6に示した含有量で用い、上記固形分を溶媒として水81.4重量%及びエタノール3.4重量%と混合して表面処理溶液組成物を製造した。
実施例1と同一組成成分を固形分100重量部基準で表7に示した含有量で用い、上記固形分を溶媒として水81.4重量%及びエタノール3.4重量%と混合して表面処理溶液組成物を製造した。
実施例1と同一組成成分を固形分100重量部基準で表8に示した含有量で用い、上記固形分を溶媒として水81.4重量%及びエタノール3.4重量%と混合して表面処理溶液組成物を製造した。
実施例1と同一組成成分を固形分100重量部基準で表9に示した含有量で用い、上記固形分を溶媒として水81.4重量%及びエタノール3.4重量%と混合して表面処理溶液組成物を製造した。
実施例1と同一組成成分を固形分100重量部基準で表10に示した含有量で用い、上記固形分を溶媒として水81.4重量%及びエタノール3.4重量%と混合して表面処理溶液組成物を製造した。
発明例2の組成物を用いたことを除いては、実施例1と同様の方法で表面処理組成物を製造し、上記表面処理組成物を試験片にコーティングするが、コーティングされた皮膜層の厚さとPMT温度を下記表11に記載された厚さで制御した。
Claims (23)
- 組成物の固形分100重量%に対して、
水溶性ポリウレタン樹脂20~40重量%;
3種のシラン化合物が架橋結合されたシラン系ゾル-ゲル(sol-gel)樹脂40
~60重量%;
硬化剤5~15重量%;
防錆耐食剤0.5~1.5重量%;
モリブデン系化合物0.1~1.0重量%;
シランカップリング剤1.0~3.0重量%;
有機金属錯体化合物1.0~2.0重量%;
酸除去剤(acid scavenger)1.0~2.0重量%;
アルミニウム系化合物0.1~1.0重量%;及び
潤滑剤1.0~2.0重量%を含み、
前記3種のシラン化合物が架橋結合されたシラン系ゾル-ゲル樹脂は、
テトラエチルオルトシリケート、テトラメトキシシラン、メチルトリメトキシシラン、
メチルトリエトキシシラン、ジメチルジメトキシシラン、ジメチルジエトキシシランの中
から選択された1種である第1シラン;2-(3,4エポキシシクロヘキシル)エチルト
リメトキシシラン、3-グリシルオキシプロピルトリメトキシシラン、3-グリシルオキ
シプロピルメチルジエトキシシランの中から選択された1種である第2シラン;3-アミ
ノプロピル-トリエトキシシラン、N-(2-アミノエチル)-3-アミノプロピルメチ
ルジメトキシシラン、N-(2-アミノエチル)-3-アミノプロピルトリメトキシシラ
ン、N-(2-アミノエチル)-3-アミノプロピルトリエトキシシランの中から選択さ
れた1種である第3シランの重合物から得られ、
前記硬化剤は、メラミン系硬化剤、ブロックイソシアネート系硬化剤、及びアジリジン系硬化剤から選択された1種以上であり、
前記防錆耐食剤は、リン酸系化合物、フッ素系化合物、バナジウム系化合物、セリウム
塩系化合物及びセレニウム塩系化合物から選択された1種以上であり、
前記酸除去剤は、カルボジイミド系化合物及びオキサゾリン系化合物から選択された1
種以上であることを特徴とする、表面処理組成物。 - 前記水溶性ポリウレタン樹脂は、ポリエステルポリオールまたはポリカーボネートポリ
オールとポリイソシアネート化合物の反応生成物であることを特徴とする、請求項1に記
載の表面処理組成物。 - 前記ポリエステルポリオールまたはポリカーボネートポリオールは、水酸基価が80~
200mgKOH/gであり、重量平均分子量が1,000~5,000であることを特
徴とする、請求項2に記載の表面処理組成物。 - 前記モリブデン系化合物は、モリブデン酸化物、モリブデン硫化物、モリブデン酢酸塩
、モリブデンリン酸塩、モリブデン炭化物、モリブデン塩化物及びモリブデン窒化物から
選択された1種以上であることを特徴とする、請求項1に記載の表面処理組成物。 - 前記シランカップリング剤は、ビニルトリエトキシシラン、3-グリシルオキシプロピ
ルトリメトキシシラン、3-グリシルオキシプロピルトリエトキシシラン、3-グリシル
オキシプロピルメチルジメトキシシラン、N-2-(アミノエチル))-3-アミノプロ
ピルトリエトキシシラン、3-アミノプロピルトリメトキシシラン、3-アミノプロピル
トリエトキシシラン、及び2-パーフルオロオクチルエチルトリメトキシシランから選択
された1種以上であることを特徴とする、請求項1に記載の表面処理組成物。 - 前記有機金属錯体化合物は、チタン系化合物及びジルコニウム系化合物から選択された
1種以上であることを特徴とする、請求項1に記載の表面処理組成物。 - 前記アルミニウム系化合物は、アルミニウムオキシド、アルミニウムヒドロキシド、ア
ルミニウムクロライド, アルミニウムサルフェート、アルミニウムニトレート、アルミニ
ウムカーボネート、アルミニウムアセテート、アルミニウムシリケート、アルミニウムホ
スフェート、アルミニウムフルオリド及びアルミニウムニトリドから選択された1種以上
であることを特徴とする、請求項1に記載の表面処理組成物。 - 前記潤滑剤は、パラフィン系ワックス、オレフィン系ワックス、カルナバ系ワックス、
ポリエステル系ワックス、ポリエチレン系ワックス、ポリプロピレン系ワックス、ポリエ
チレン-テフロン(登録商標)系ワックス及びポリテフロン(登録商標)系ワックスから
選択された1種以上であることを特徴とする、請求項1に記載の表面処理組成物。 - 前記表面処理組成物は、溶媒をさらに含み、固形分含有量が10~20重量%であり、
残部溶媒であることを特徴とする、請求項1から8のいずれか一項に記載の表面処理組成
物。 - 前記溶媒は、溶媒全重量に対してアルコール3~5重量%及び残部の水を含むことを特
徴とする、請求項9に記載の表面処理組成物。 - 三元系溶融亜鉛合金めっき層が形成された三元系溶融亜鉛合金めっき鋼板上に請求項1
から8のいずれか一項に記載の表面処理組成物をコーティングする段階;及び
前記コーティングされた表面処理組成物を乾燥して表面処理皮膜層を形成する段階を含
む、表面処理された三元系溶融亜鉛合金めっき鋼板の製造方法。 - 前記表面処理組成物を1.5~30μmの厚さでコーティングすることを特徴とする、
請求項11に記載の表面処理された三元系溶融亜鉛合金めっき鋼板の製造方法。 - 前記コーティングは、ロールコーティング、スプレー、浸漬、スプレースクイージング
または浸漬スクイージングによって行われることを特徴とする、請求項11に記載の表面
処理された三元系溶融亜鉛合金めっき鋼板の製造方法。 - 前記乾燥は、素材鋼板の最終到達温度(PMT)基準で70~150℃温度で行われる
ことを特徴とする、請求項11に記載の表面処理された三元系溶融亜鉛合金めっき鋼板の
製造方法。 - 前記乾燥は熱風乾燥炉または誘導加熱炉で行われることを特徴とする、請求項11に記
載の表面処理された三元系溶融亜鉛合金めっき鋼板の製造方法。 - 前記熱風乾燥炉は、内部温度が100~250℃であることを特徴とする、請求項15
に記載の表面処理された三元系溶融亜鉛合金めっき鋼板の製造方法。 - 前記誘導加熱炉は、1000~4500Aの電流が印加されることを特徴とする、請求
項15に記載の表面処理された三元系溶融亜鉛合金めっき鋼板の製造方法。 - 前記表面処理皮膜層を水冷させる段階をさらに含む、請求項11に記載の表面処理され
た三元系溶融亜鉛合金めっき鋼板の製造方法。 - 前記三元系溶融亜鉛合金めっき鋼板の製造方法は連続工程で行われ、前記連続工程の速
度は80~120mpmである、請求項11に記載の表面処理された三元系溶融亜鉛合金
めっき鋼板の製造方法。 - 鋼板;
前記鋼板の少なくとも一面に形成された三元系溶融亜鉛合金めっき層;及び
前記三元系溶融亜鉛合金めっき層上に形成された表面処理皮膜層を含み、
前記表面処理皮膜層は、請求項1から8のいずれか一項に記載の表面処理組成物で形成
された、表面処理された三元系溶融亜鉛合金めっき鋼板。 - 前記三元系溶融亜鉛合金めっき層は、界面に形成されたAl濃化層を含み、前記Al濃
化層の占有面積率は70%以上(100%を含む)であることを特徴とする、請求項20
に記載の表面処理された三元系溶融亜鉛合金めっき鋼板。 - 前記三元系溶融亜鉛合金めっき層は、Al0.2~15重量%、Mg0.5~3.5重
量%、残部Zn及び不可避不純物を含むことを特徴とする、請求項20に記載の表面処理
された三元系溶融亜鉛合金めっき鋼板。 - 前記表面処理皮膜層は、厚さが0.3~3μmであることを特徴とする、請求項20に
記載の表面処理された三元系溶融亜鉛合金めっき鋼板。
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KR1020190117527A KR102314431B1 (ko) | 2019-09-24 | 2019-09-24 | 우수한 내흑변성 및 내알칼리성을 부여하는 삼원계 용융아연합금 도금강판용 표면처리 용액 조성물, 이를 이용하여 표면처리된 삼원계 용융아연합금 도금강판 및 그 제조 방법 |
KR10-2019-0117527 | 2019-09-24 | ||
PCT/KR2020/012844 WO2021060818A1 (ko) | 2019-09-24 | 2020-09-23 | 우수한 내흑변성 및 내알칼리성을 부여하는 삼원계 용융아연합금 도금강판용 표면처리 용액 조성물, 이를 이용하여 표면처리된 삼원계 용융아연합금 도금강판 및 그 제조 방법 |
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CN113289876B (zh) * | 2021-04-30 | 2022-07-29 | 重庆大学 | 一种兼具自修复功能和超双疏功能的金属防护膜制备方法 |
CN114289281A (zh) * | 2021-12-02 | 2022-04-08 | 烨辉(中国)科技材料有限公司 | 制备抗黑变的铝锌镁产品的方法和用该方法制得的产品 |
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EP4036273A1 (en) | 2022-08-03 |
CN114502673B (zh) | 2023-05-26 |
KR20210035955A (ko) | 2021-04-02 |
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