JP2019510886A - ニッケルなしで金属表面をリン酸処理するための改良された方法 - Google Patents
ニッケルなしで金属表面をリン酸処理するための改良された方法 Download PDFInfo
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- JP2019510886A JP2019510886A JP2018553121A JP2018553121A JP2019510886A JP 2019510886 A JP2019510886 A JP 2019510886A JP 2018553121 A JP2018553121 A JP 2018553121A JP 2018553121 A JP2018553121 A JP 2018553121A JP 2019510886 A JP2019510886 A JP 2019510886A
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- phosphating
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- 229910052751 metal Inorganic materials 0.000 title claims abstract description 45
- 239000002184 metal Substances 0.000 title claims abstract description 45
- 238000000034 method Methods 0.000 title claims abstract description 30
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title description 28
- 229910052759 nickel Inorganic materials 0.000 title description 14
- 239000000203 mixture Substances 0.000 claims abstract description 72
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims abstract description 37
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 32
- 239000010452 phosphate Substances 0.000 claims abstract description 32
- -1 iron (III) ions Chemical class 0.000 claims abstract description 17
- 238000004140 cleaning Methods 0.000 claims abstract description 9
- 229910001437 manganese ion Inorganic materials 0.000 claims abstract description 7
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 claims abstract description 6
- 230000003213 activating effect Effects 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract 2
- 239000002253 acid Substances 0.000 claims description 31
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 24
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 claims description 18
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 claims description 12
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- 238000010306 acid treatment Methods 0.000 claims description 8
- 230000002378 acidificating effect Effects 0.000 claims description 6
- 229910021645 metal ion Inorganic materials 0.000 claims description 4
- 229910002651 NO3 Inorganic materials 0.000 claims description 3
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- 229910052782 aluminium Inorganic materials 0.000 description 8
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 8
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- 229910001335 Galvanized steel Inorganic materials 0.000 description 7
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 7
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- 239000011572 manganese Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 239000010959 steel Substances 0.000 description 6
- 238000000151 deposition Methods 0.000 description 5
- 230000008021 deposition Effects 0.000 description 5
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- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
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- 229910001453 nickel ion Inorganic materials 0.000 description 4
- 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 description 4
- 229910000165 zinc phosphate Inorganic materials 0.000 description 4
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 3
- 150000001768 cations Chemical class 0.000 description 3
- 238000010790 dilution Methods 0.000 description 3
- 239000012895 dilution Substances 0.000 description 3
- 150000002222 fluorine compounds Chemical class 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- 229910052748 manganese Inorganic materials 0.000 description 3
- 150000002823 nitrates Chemical class 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 229910052725 zinc Inorganic materials 0.000 description 3
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 230000004913 activation Effects 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
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- 238000006243 chemical reaction Methods 0.000 description 2
- 239000003599 detergent Substances 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- 229940085991 phosphate ion Drugs 0.000 description 2
- 238000005554 pickling Methods 0.000 description 2
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- JUWGUJSXVOBPHP-UHFFFAOYSA-B titanium(4+);tetraphosphate Chemical compound [Ti+4].[Ti+4].[Ti+4].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O JUWGUJSXVOBPHP-UHFFFAOYSA-B 0.000 description 2
- 238000004448 titration Methods 0.000 description 2
- 150000003751 zinc Chemical class 0.000 description 2
- IDCPFAYURAQKDZ-UHFFFAOYSA-N 1-nitroguanidine Chemical compound NC(=N)N[N+]([O-])=O IDCPFAYURAQKDZ-UHFFFAOYSA-N 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-L Phosphate ion(2-) Chemical compound OP([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-L 0.000 description 1
- 229920000388 Polyphosphate Polymers 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 239000012190 activator Substances 0.000 description 1
- 239000002318 adhesion promoter Substances 0.000 description 1
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- 229910045601 alloy Inorganic materials 0.000 description 1
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- 150000001860 citric acid derivatives Chemical class 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
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- 229910001610 cryolite Inorganic materials 0.000 description 1
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- 238000005238 degreasing Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-M dihydrogenphosphate Chemical compound OP(O)([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-M 0.000 description 1
- 235000011180 diphosphates Nutrition 0.000 description 1
- IRXRGVFLQOSHOH-UHFFFAOYSA-L dipotassium;oxalate Chemical compound [K+].[K+].[O-]C(=O)C([O-])=O IRXRGVFLQOSHOH-UHFFFAOYSA-L 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000000383 hazardous chemical Substances 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 229910000159 nickel phosphate Inorganic materials 0.000 description 1
- 150000002826 nitrites Chemical class 0.000 description 1
- 208000014451 palmoplantar keratoderma and congenital alopecia 2 Diseases 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 239000001205 polyphosphate Substances 0.000 description 1
- 235000011176 polyphosphates Nutrition 0.000 description 1
- 239000001103 potassium chloride Substances 0.000 description 1
- 235000011164 potassium chloride Nutrition 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000011775 sodium fluoride Substances 0.000 description 1
- 235000013024 sodium fluoride Nutrition 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
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- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 150000003892 tartrate salts Chemical class 0.000 description 1
- 238000004876 x-ray fluorescence Methods 0.000 description 1
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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
- 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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- 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
- C23C22/82—After-treatment
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D13/00—Electrophoretic coating characterised by the process
- C25D13/12—Electrophoretic coating characterised by the process characterised by the article coated
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D13/00—Electrophoretic coating characterised by the process
- C25D13/20—Pretreatment
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/48—After-treatment of electroplated surfaces
-
- 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
Abstract
Description
本発明の方法は、被覆されていない金属表面、またはその代わりに既に化成処理されている金属表面を処理するのに使用することができる。したがって、以下で「金属表面」というときは常に既に化成処理された金属表面も含むと考えられる。
遊離酸の決定には、10mlのリン酸処理用組成物を300mlの三角フラスコのような適切な容器にピペットで移す。リン酸処理用組成物が錯体のフッ化物を含有するならば、追加の2〜3gの塩化カリウム(KCl)を試料に加える。次いで、pH計および電極を用いて、0.1MのNaOHでpH3.6まで滴定を行う。この滴定で消費される0.1MのNaOHの量(リン酸処理用組成物10ml当たりのml)が遊離酸(FA)の値を点で与える。
遊離酸(希釈)の決定には、10mlのリン酸処理用組成物を300mlの三角フラスコのような適切な容器にピペットで移す。その後150mlのDI水を加える。pH計および電極を用いて、0.1MのNaOHでpH4.7まで滴定を行う。この滴定で消費される0.1MのNaOHの量(希釈リン酸処理用組成物10ml当たりのml)が遊離酸(希釈)(FA(dil.))の値を点で与える。遊離酸(FA)に対する差から錯体のフッ化物の量を決定することが可能である。この差に0.36の係数をかけると、結果がSiF6 2−としての錯体のフッ化物の量g/lである。
遊離酸(希釈)の決定後、希釈リン酸処理用組成物を、シュウ酸カリウム溶液を添加した後、pH計および電極を用いて、0.1MのNaOHでpH8.9まで滴定する。この手順での、希釈リン酸処理用組成物10ml当たりのmlとしての0.1MのNaOHの消費量が総酸、Fischer(TAF)を点で与える。この数字に0.71をかけると、結果はP2O5として計算したホスフェートイオンの総量である(W. Rausch:「Die Phosphatierung von Metallen」 Eugen G. Leuze−Verlag 2005、第3版、332ページ以降参照)。
総酸(TA)は、存在する二価のカチオンならびに遊離および結合したリン酸(後者がホスフェートである)の合計である。これは、pH計および電極を用いて0.1MのNaOHの消費量によって決定される。このためには、10mlのリン酸処理用組成物を300mlの三角フラスコのような適切な容器にピペットで移し、25mlのDI水で希釈する。この後0.1MのNaOHでpH9まで滴定する。この手順中の、希釈リン酸処理用組成物10ml当たりのmlとしての消費量が総酸(TA)の点数に対応する。
酸価(A値)は比FA:TAFを表し、遊離酸(FA)の値を総酸、Fischer(TAF)の値で割ることによって得られる。
溶融亜鉛メッキ鋼(EA)、電解亜鉛メッキ鋼(G)またはアルミニウム(AA6014S)で作成された試験プレートを、1.3g/lのZn、1g/lのMnおよび13g/lのPO4 3−(P2O5として計算)を含有するニッケル不含リン酸処理用溶液を用いて45℃で被覆した。
溶融亜鉛メッキ鋼(EA)、電解亜鉛メッキ鋼(G)またはアルミニウム(AA6014S)で作成された試験プレートを、1.3g/lのZn、1g/lのMn、13mg/lのFe(III)および13g/lのPO4 3−(P2O5として計算)を含有するニッケル不含リン酸処理用溶液を用いて45℃で被覆した。
溶融亜鉛メッキ鋼(EA)、電解亜鉛メッキ鋼(G)またはアルミニウム(AA6014S)で作成された試験プレートを、1.3g/lのZn、1g/lのMn、14g/lのPO4 3−(P2O5として計算)、3g/lのNO3 −およびさらに1g/lのニッケルを含有するリン酸処理用溶液を用いて53℃で被覆した。
鉄を添加してない浴は初めスラッジを含まなかった。浴値は:FA(KCl)=1.3、Zn含有量=1.2g/lであった。
10mg/lのFe(III)を他のニッケル不含浴に加えた。その後、FA(KCl)を約1.3に調節した。Zn含有量に変化はなく、1.3g/lで安定なままであった。
Claims (15)
- 金属表面をリン酸処理する方法であって、金属表面を、任意に浄化および/または活性化した後、亜鉛イオン、マンガンイオン、鉄(III)イオンおよびホスフェートイオンを含む酸性の水性で実質的にニッケルなしのリン酸処理用組成物で処理し、その後任意に濯ぎおよび/または乾燥する、方法。
- 金属表面を少なくとも部分的に亜鉛メッキする、請求項1に記載の方法。
- リン酸処理用組成物中の鉄(III)イオンの含有量が1〜200mg/l、好ましくは5〜100mg/l、より好ましくは5〜20mg/lの範囲である、請求項1または2に記載の方法。
- リン酸処理用組成物が0.3〜3.0g/lの亜鉛イオン、0.3〜2.0g/lのマンガンイオン、8〜25g/lのホスフェートイオン(P2O5として計算)を含む、請求項1から3のいずれか一項に記載の方法。
- リン酸処理用組成物が30〜250mg/lの遊離のフッ化物を含む、請求項1から4のいずれか一項に記載の方法。
- リン酸処理用組成物が0.5〜3g/lの錯体のフッ化物を含む、請求項1から5のいずれか一項に記載の方法。
- 錯体のフッ化物がテトラフルオロボレート(BF4 −)および/またはヘキサフルオロシリケート(SiF6 2−)である、請求項6に記載の方法。
- リン酸処理用組成物が、0.3〜2.0の範囲の遊離酸、0.5〜8の範囲の遊離酸(希釈)、12〜28の範囲の総酸、Fischer、12〜45の範囲の総酸、および0.01〜0.2の範囲の酸価を有する、請求項1から7のいずれか一項に記載の方法。
- リン酸処理用組成物がH2O2を促進剤として含む、請求項1から8のいずれか一項に記載の方法。
- リン酸処理用組成物が1g/l未満、好ましくは0.1g/l未満、より好ましくは0.05〜0.1g/lの硝酸塩を含有する、請求項1から9のいずれか一項に記載の方法。
- 鉄(III)イオンが遊離酸の確立に先立ってリン酸処理用組成物に添加されている、請求項1から10のいずれか一項に記載の方法。
- 既にリン酸処理用組成物で処理された、即ち既にホスフェートで被覆された金属表面を、任意に濯ぎおよび/または乾燥するが、その後水性の後濯ぎ組成物で処理しない、殊に少なくとも1種の金属イオンおよび/または少なくとも1種のポリマーを含む組成物で処理しない、請求項1から11のいずれか一項に記載の方法。
- 請求項1から12のいずれか一項の方法により金属表面をリン酸処理するための、酸性の水性で実質的にニッケルなしのリン酸処理用組成物。
- 適切な溶媒で1〜100倍に希釈し、必要な場合にはpH調整物質を添加することにより、請求項13に記載のリン酸処理用組成物を得ることができる、濃縮物。
- 請求項1から12のいずれか一項に記載の方法により得られる、ホスフェートで被覆された金属表面。
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PCT/EP2017/050993 WO2017174222A1 (de) | 2015-04-07 | 2017-01-18 | Verbessertes verfahren zur nickelfreien phosphatierung von metallischen oberflächen |
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JP2017553120A Active JP6804464B2 (ja) | 2015-04-07 | 2016-04-07 | ニッケルを用いないで金属表面をリン酸塩処理するための方法 |
JP2018553121A Active JP6986028B2 (ja) | 2015-04-07 | 2017-01-18 | ニッケルなしで金属表面をリン酸塩処理するための改良された方法 |
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