JP5860582B2 - 金属表面処理剤及び金属表面処理方法 - Google Patents
金属表面処理剤及び金属表面処理方法 Download PDFInfo
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- JP5860582B2 JP5860582B2 JP2010019605A JP2010019605A JP5860582B2 JP 5860582 B2 JP5860582 B2 JP 5860582B2 JP 2010019605 A JP2010019605 A JP 2010019605A JP 2010019605 A JP2010019605 A JP 2010019605A JP 5860582 B2 JP5860582 B2 JP 5860582B2
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- surface treatment
- compound
- metal surface
- metal
- film
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- 239000002184 metal Substances 0.000 title claims description 141
- 238000004381 surface treatment Methods 0.000 title claims description 82
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- 238000000034 method Methods 0.000 title claims description 33
- 150000001875 compounds Chemical class 0.000 claims description 93
- 239000011651 chromium Substances 0.000 claims description 74
- 229920005989 resin Polymers 0.000 claims description 46
- 239000011347 resin Substances 0.000 claims description 46
- 239000000463 material Substances 0.000 claims description 32
- 239000010935 stainless steel Substances 0.000 claims description 31
- 229910001220 stainless steel Inorganic materials 0.000 claims description 31
- 239000003795 chemical substances by application Substances 0.000 claims description 27
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 26
- -1 phosphate compound Chemical class 0.000 claims description 25
- 239000007769 metal material Substances 0.000 claims description 22
- 238000000576 coating method Methods 0.000 claims description 20
- 239000011248 coating agent Substances 0.000 claims description 19
- 239000000758 substrate Substances 0.000 claims description 19
- 150000002484 inorganic compounds Chemical class 0.000 claims description 15
- 239000003822 epoxy resin Substances 0.000 claims description 11
- 229920000647 polyepoxide Polymers 0.000 claims description 11
- 229910010272 inorganic material Inorganic materials 0.000 claims description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims description 10
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- 125000002091 cationic group Chemical group 0.000 description 4
- PHFQLYPOURZARY-UHFFFAOYSA-N chromium trinitrate Chemical compound [Cr+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PHFQLYPOURZARY-UHFFFAOYSA-N 0.000 description 4
- WMYWOWFOOVUPFY-UHFFFAOYSA-L dihydroxy(dioxo)chromium;phosphoric acid Chemical compound OP(O)(O)=O.O[Cr](O)(=O)=O WMYWOWFOOVUPFY-UHFFFAOYSA-L 0.000 description 4
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- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 3
- 125000001797 benzyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])* 0.000 description 3
- 229910021563 chromium fluoride Inorganic materials 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
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- DCKVFVYPWDKYDN-UHFFFAOYSA-L oxygen(2-);titanium(4+);sulfate Chemical compound [O-2].[Ti+4].[O-]S([O-])(=O)=O DCKVFVYPWDKYDN-UHFFFAOYSA-L 0.000 description 3
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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
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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
- 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
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- 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
- B05D2202/00—Metallic substrate
- B05D2202/10—Metallic substrate based on Fe
- B05D2202/15—Stainless steel
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- 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
- B05D2701/00—Coatings being able to withstand changes in the shape of the substrate or to withstand welding
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- 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
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/50—Multilayers
- B05D7/51—One specific pretreatment, e.g. phosphatation, chromatation, in combination with one specific coating
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B32B2307/00—Properties of the layers or laminate
- B32B2307/30—Properties of the layers or laminate having particular thermal properties
- B32B2307/306—Resistant to heat
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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
- C23C2222/10—Use of solutions containing trivalent chromium but free of hexavalent chromium
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Description
本発明に係る金属表面処理剤は、図1に示すステンレス鋼からなる基材1の表面にラミネート材3(樹脂フィルム又はラミネートフィルム)の下地用の金属表面処理皮膜2を形成するための処理剤である。そして、その特徴は、金属表面処理剤が、Cr(III)化合物(A)と、造膜性を有する有機化合物及び無機化合物から選ばれる少なくとも1種の化合物(B)とを含有し、前記Cr(III)化合物(A)の金属Cr換算質量をMとし、前記化合物(B)の質量をNとしたとき、N/Mが0.005〜1であることにある。
Cr(III)化合物(A)は、6価クロムを含まない3価のクロム化合物である。このCr(III)化合物を含む金属表面処理剤で表面処理皮膜を形成すれば、金属Crが金属基材と反応して基材表面と表面処理皮膜とを強固に密着させることができる。Cr(III)化合物自体でCr化合物層を形成することができるが、さらに化合物(B)を含むことにより、金属表面処理剤は優れた造膜性を示し、その結果、その金属表面処理剤で形成された表面処理皮膜は、耐水性及び耐薬品性が向上し、特に耐食性が飛躍的に向上する。
化合物(B)は、造膜性を有する有機化合物及び無機化合物から選ばれる少なくとも1種の化合物である。造膜性を有する化合物(B)は、Cr(III)リッチとなる表面処理皮膜においてバインダー機能を担い、かつステンレス鋼からなる基材表面に対する優れた密着性を付与することにより、Cr(III)リッチの表面処理皮膜を強加工に耐えさせる役割を有する。さらに、化合物(B)を含む金属表面処理剤で形成された表面処理皮膜は、造膜性が向上することでバリアー性が保持され、耐食性、耐水性、耐溶剤性及び耐薬品性が向上する。
金属表面処理剤を構成する溶媒は、水を主体とするが、皮膜の乾燥性改善等、必要に応じてアルコール系、ケトン系、又はセロソルブ系の水溶性有機溶剤の併用を妨げるものではない。
この他に、界面活性剤、消泡剤、レベリング剤、防菌防ばい剤、着色剤、及び硬化剤等、本発明の趣旨及び皮膜性能を損なわない範囲で添加し得る。また、皮膜の耐食性を向上させるため、メチロール化メラミン、カルボジイミド、及びイソシアネート等の有機架橋剤、及び、密着性向上のため、γ−グリシドキシプロピルトリエトキシシラン、γ−グリシドキシプロピルトリエトキシシラン、γ−アミノプロピルトリエトキシシラン、及びN−β−アミノエチル−γ−アミノプロピルトリメトキシシラン等のシランカップリング剤を、本発明の趣旨及び皮膜性能を損なわない範囲で添加し得る。
本発明に係る金属表面処理剤の処理対象は、ステンレス鋼からなる基材である。本発明に係る金属表面処理剤は、この金属基材を被処理物としてその表面に塗布され、その表面に表面処理皮膜を形成する。ステンレス鋼からなる金属基材1としては、例えば、ステンレス鋼からなる薄板材、包装用箔等を挙げることができる。
本発明に係る金属表面処理方法は、上述した本発明に係る金属表面処理剤をステンレス鋼からなる基材の表面に塗布した後、60〜250℃の温度で加熱乾燥する方法である。金属表面処理剤の液温は、通常、10〜50℃の範囲内である。金属表面処理剤の塗布手段は特に制限はなく、スプレー法、浸漬法等が好適に用いられる。金属表面への金属表面処理剤の接触時間は、通常、0.5〜180秒程度である。
本発明に係る金属材料10は、図1に示すように、上記した金属表面処理方法で処理されてなる表面処理皮膜2を有する。例えば、図1に示すように、被処理物であるステンレス鋼からなる金属基材1上には、上記金属表面処理方法で処理されてなる表面処理皮膜2が形成されており、その表面処理皮膜2上には、樹脂フィルム(3)がラミネートされ又は樹脂塗膜(3)が形成されている。こうして構成された金属材料10には、その後に深絞り加工、しごき加工又はストレッチドロー加工等の厳しい成形加工が施される。なお、図1では、金属基材1の一方の表面に表面処理皮膜2と樹脂フィルム又は樹脂塗膜(3)を形成した例を示しているが、金属基材1の両面に、すなわち他方の表面にも表面処理皮膜を形成し、さらに樹脂フィルム又は樹脂塗膜を設けてもよい。
A1:硫酸クロム
A2:硝酸クロム
A3:フッ化クロム
A4:重リン酸クロム
(ウレタン樹脂:記号b1I)
モノマー組成を、ポリオール成分「イソフタル酸と1,6ヘキサンジオールとからなるポリエステルポリオール(数平均分子量:2000)200部、トリメチロールプロパン(分子量:134)5部、N−メチル−ジエタノールアミン(分子量:119)32部」、イソシアネート成分「イソホロンジイソシアネート(分子量:222)118部」、鎖伸長剤「エチレンジアミン(分子量:60)5部」とした。
成分1「ビスフェノールA系エポキシ樹脂(油化シェルエポキシ株式会社製、エピコート828)(エポキシ当量:187g)235.7部」、成分2「ビスフェノールA 59.4部」、成分3「反応触媒(塩化リチウム)0.1部」、成分4「ジエタノールアミン14部」とした。
モノマー組成として、「メタクリル酸メチル(分子量:100)20部、ブチルアクリレート(分子量:128)40部、2−ヒドロキシプロピルメタクリレート(分子量:144)10部、スチレン(分子量:104)10部、N,N−ジメチルアミノプロピルメタクリレート(分子量:175)20部」を用いた。
下記構造式のビスフェノール型カチオン変性フェノール樹脂b1IVを用いた。下記構造式中、重合度(m+n)は10〜15であり、n/mは40/60である。
ポリビニルアルコール(80質量%)とメタクリル酸(20質量%)との共重合体(平均分子量:20000)を用いた。
下記構造式のグリセリル化キトサン(数平均分子量:1〜10万、グリセリル化1.1)を用いた。
b2I:スノーテックスC(日産化学株式会社製)
b2II:炭酸ジルコニウムアンモニウム
b2III:チタニウムアセチルアセトネート
b2IV:トリポリリン酸
b3I:酒石酸
b3II:アスコルビン酸
b3III:1−ヒドロキシ−エチリデン−1,1−ジホスホン酸
b3IV:ポリアリルアミン
上記した水系樹脂と水溶性金属化合物とを組み合わせ、表1に示す実施例1〜20の金属表面処理剤と、比較例1〜10の金属表面処理剤を準備した。
ステンレス鋼(JIS SUS304、板厚0.26mm)をファインクリーナーE6402(日本パーカライジング株式会社製のアルカリ脱脂剤)の2%水溶液で60℃・30秒間スプレー脱脂した後、水洗して表面を清浄した。続いて、ステンレス鋼板の表面の水分を蒸発させるために、80℃で1分間、加熱乾燥した。脱脂洗浄したステンレス鋼板の表面に、表1に示した実施例1〜20及び比較例1〜10の金属表面処理剤をバーコートによって塗布し、熱風循環式乾燥炉内で200℃、1分間乾燥し、ステンレス鋼板の表面に所定の膜厚の表面処理皮膜を形成した。表面処理皮膜を形成したステンレス鋼板に、ポリエステル系フィルム(膜厚16μm)を250℃で5秒間(到達板温で180℃)、面圧が50kg/cm2になるようにヒートラミネートして「被覆金属板」を作製した。
比較例11として、市販のりん酸クロメート処理剤(AM−K702:日本パーカライジング株式会社製)を50℃で5秒間スプレー処理し、水洗して未反応の薬剤を除去し、80℃で1分間加熱乾燥して試験片(Cr付着量は20mg/m2)を得た。また、比較例12として、市販のりん酸ジルコニウム処理剤(AL−404:日本パーカライジング株式会社製)を40℃で20秒間スプレー処理し、水洗して未反応の薬剤を除去し80℃で1分間加熱乾燥して試験片(Zr付着量は15mg/m2)を得た。また、比較例13として、脱脂のみの試験片も作製した。
被覆金属板を深絞り加工した後の初期密着性、耐久密着性及び耐酸密着性を以下のようにして評価した。その結果を表2に示した。
深絞り加工した後の供試材について、初期密着性を評価した。缶が作製でき、フィルムの剥離がないものを「○」とし、缶は作製できるがフィルムが一部剥離したものを「△」とし、破断して缶が作製できないものを「×」とした。また、「○」の中で、全く剥離が見られず特に外観に優れるものを「◎」とした。
深絞り加工した後の供試材について、加熱加圧蒸気の雰囲気下でレトルト試験を実施した。レトルト試験は、市販の滅菌装置(オートクレーブ)を用い、125℃・1時間で行った。試験後の供試材について、フィルムの剥離がないものを「○」とし、フィルムの一部が剥離したものを「△」とし、フィルムが全面剥離したものを「×」とした。また、「○」の中で、全く剥離が見られず特に外観に優れるものを「◎」とした。
深絞り加工した後の供試材について、50℃の0.5%HF水溶液中に16時間浸漬した後の密着性を評価した。フィルムの剥離がないものを「○」とし、フィルムの一部が剥離したものを「△」とし、フィルムが全面剥離したものを「×」とした。また、「○」の中で、全く剥離が見られず特に外観に優れるものを「◎」とした。
2 表面処理皮膜
3 樹脂フィルム(ラミネートフィルム)又は樹脂塗膜
10 金属材料
Claims (5)
- ステンレス鋼からなる基材表面にラミネート又は樹脂塗膜下地用金属表面処理皮膜を形成するための金属表面処理剤(但し、二酸化ケイ素を含むものを除く。)であって、
6価クロムを含まない3価のクロム化合物であるCr(III)化合物(A)と、
ウレタン樹脂、エポキシ樹脂、ポリオレフィン系樹脂、アクリル樹脂、ビニル樹脂、フェノール樹脂及び天然高分子から選ばれる1種又は2種以上の樹脂化合物(b1)と、ジルコニウム化合物、チタン化合物及びリン酸塩化合物から選ばれる1種又は2種以上の無機化合物(b2)と、水酸基、カルボキシル基、ホスホン酸基、りん酸基、アミノ基及びアミド基から選ばれる少なくとも1種の官能基を一分子内に2個以上有する有機キレート化合物(b3)と、から選ばれる少なくとも1種の化合物(B)と、を含有し、
前記Cr(III)化合物(A)の金属Cr換算質量をMとし、前記化合物(B)として選択された1又は2種以上の化合物を配合したものの固形分換算質量をNとしたとき、N/Mが0.005〜1であることを特徴とする金属表面処理剤。 - 前記金属表面処理剤は、該金属表面処理剤を前記金属基材の表面に塗布した後に乾燥して前記金属表面処理皮膜を形成する、請求項1に記載の金属表面処理剤。
- 請求項1又は2に記載の金属表面処理剤をステンレス鋼からなる基材表面に塗布した後、60〜250℃の温度で加熱乾燥して表面処理皮膜を形成することを特徴とする金属表面処理方法。
- 請求項3に記載の金属表面処理方法で形成されたことを特徴とする金属表面処理皮膜。
- 請求項3に記載の金属表面処理方法で形成された表面処理皮膜を、ステンレス鋼からなる基材表面に設けてなることを特徴とする金属材料。
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