JP5595874B2 - Magnesium alloy surface treatment method - Google Patents
Magnesium alloy surface treatment method Download PDFInfo
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- JP5595874B2 JP5595874B2 JP2010247925A JP2010247925A JP5595874B2 JP 5595874 B2 JP5595874 B2 JP 5595874B2 JP 2010247925 A JP2010247925 A JP 2010247925A JP 2010247925 A JP2010247925 A JP 2010247925A JP 5595874 B2 JP5595874 B2 JP 5595874B2
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- 229910000861 Mg alloy Inorganic materials 0.000 title claims description 43
- 238000000034 method Methods 0.000 title claims description 34
- 238000004381 surface treatment Methods 0.000 title claims description 24
- 238000006243 chemical reaction Methods 0.000 claims description 35
- 239000000126 substance Substances 0.000 claims description 35
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
- -1 Aluminate ion Chemical class 0.000 claims description 21
- 239000000243 solution Substances 0.000 claims description 21
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical group [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 14
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 claims description 12
- 238000000576 coating method Methods 0.000 claims description 11
- 229940085991 phosphate ion Drugs 0.000 claims description 11
- 239000011248 coating agent Substances 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims description 9
- 150000008044 alkali metal hydroxides Chemical class 0.000 claims description 8
- 239000008151 electrolyte solution Substances 0.000 claims description 8
- 229940071182 stannate Drugs 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 7
- ALTWGIIQPLQAAM-UHFFFAOYSA-N metavanadate Chemical compound [O-][V](=O)=O ALTWGIIQPLQAAM-UHFFFAOYSA-N 0.000 claims description 7
- 235000011180 diphosphates Nutrition 0.000 claims description 5
- 238000005530 etching Methods 0.000 claims description 4
- 239000010407 anodic oxide Substances 0.000 claims description 3
- 238000007654 immersion Methods 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 claims 2
- 238000007254 oxidation reaction Methods 0.000 claims 2
- 238000005406 washing Methods 0.000 claims 1
- 238000005260 corrosion Methods 0.000 description 11
- 230000007797 corrosion Effects 0.000 description 11
- 239000003973 paint Substances 0.000 description 11
- 238000007743 anodising Methods 0.000 description 8
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 description 8
- 239000007788 liquid Substances 0.000 description 7
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 6
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 4
- 229910052804 chromium Inorganic materials 0.000 description 4
- 239000011651 chromium Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000011698 potassium fluoride Substances 0.000 description 4
- 235000003270 potassium fluoride Nutrition 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- LWIHDJKSTIGBAC-UHFFFAOYSA-K tripotassium phosphate Chemical compound [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 239000003513 alkali Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- XPPKVPWEQAFLFU-UHFFFAOYSA-J diphosphate(4-) Chemical compound [O-]P([O-])(=O)OP([O-])([O-])=O XPPKVPWEQAFLFU-UHFFFAOYSA-J 0.000 description 3
- ZPWVASYFFYYZEW-UHFFFAOYSA-L dipotassium hydrogen phosphate Chemical compound [K+].[K+].OP([O-])([O-])=O ZPWVASYFFYYZEW-UHFFFAOYSA-L 0.000 description 3
- 229940048084 pyrophosphate Drugs 0.000 description 3
- 239000011775 sodium fluoride Substances 0.000 description 3
- 235000013024 sodium fluoride Nutrition 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 229910001515 alkali metal fluoride Inorganic materials 0.000 description 2
- 150000004645 aluminates Chemical class 0.000 description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 2
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000005266 casting Methods 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 229910000402 monopotassium phosphate Inorganic materials 0.000 description 2
- 235000019796 monopotassium phosphate Nutrition 0.000 description 2
- 229910000403 monosodium phosphate Inorganic materials 0.000 description 2
- 235000019799 monosodium phosphate Nutrition 0.000 description 2
- 235000021317 phosphate Nutrition 0.000 description 2
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 2
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 description 2
- 229910001388 sodium aluminate Inorganic materials 0.000 description 2
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 description 2
- FQENQNTWSFEDLI-UHFFFAOYSA-J sodium diphosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])([O-])=O FQENQNTWSFEDLI-UHFFFAOYSA-J 0.000 description 2
- 239000001488 sodium phosphate Substances 0.000 description 2
- 229940048086 sodium pyrophosphate Drugs 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 235000019818 tetrasodium diphosphate Nutrition 0.000 description 2
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 description 2
- 229910000404 tripotassium phosphate Inorganic materials 0.000 description 2
- 235000019798 tripotassium phosphate Nutrition 0.000 description 2
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 2
- 229910000406 trisodium phosphate Inorganic materials 0.000 description 2
- 235000019801 trisodium phosphate Nutrition 0.000 description 2
- RQALKBLYTUKBFV-UHFFFAOYSA-N 1,4-dioxa-7-thiaspiro[4.4]nonane Chemical compound O1CCOC11CSCC1 RQALKBLYTUKBFV-UHFFFAOYSA-N 0.000 description 1
- PAJMKGZZBBTTOY-UHFFFAOYSA-N 2-[[2-hydroxy-1-(3-hydroxyoctyl)-2,3,3a,4,9,9a-hexahydro-1h-cyclopenta[g]naphthalen-5-yl]oxy]acetic acid Chemical compound C1=CC=C(OCC(O)=O)C2=C1CC1C(CCC(O)CCCCC)C(O)CC1C2 PAJMKGZZBBTTOY-UHFFFAOYSA-N 0.000 description 1
- RSEBUVRVKCANEP-UHFFFAOYSA-N 2-pyrroline Chemical compound C1CC=CN1 RSEBUVRVKCANEP-UHFFFAOYSA-N 0.000 description 1
- 101001108245 Cavia porcellus Neuronal pentraxin-2 Proteins 0.000 description 1
- 229910017855 NH 4 F Inorganic materials 0.000 description 1
- XIHZSTLWURKKRH-UHFFFAOYSA-N [Ca].[Mn].P(O)(O)(O)=O Chemical compound [Ca].[Mn].P(O)(O)(O)=O XIHZSTLWURKKRH-UHFFFAOYSA-N 0.000 description 1
- GJPIVNTZJFSDCX-UHFFFAOYSA-N [V].[Ca] Chemical compound [V].[Ca] GJPIVNTZJFSDCX-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 238000002048 anodisation reaction Methods 0.000 description 1
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 229910001430 chromium ion Inorganic materials 0.000 description 1
- JOPOVCBBYLSVDA-UHFFFAOYSA-N chromium(6+) Chemical compound [Cr+6] JOPOVCBBYLSVDA-UHFFFAOYSA-N 0.000 description 1
- 230000003750 conditioning effect Effects 0.000 description 1
- 238000004512 die casting Methods 0.000 description 1
- XPPKVPWEQAFLFU-UHFFFAOYSA-N diphosphoric acid Chemical compound OP(O)(=O)OP(O)(O)=O XPPKVPWEQAFLFU-UHFFFAOYSA-N 0.000 description 1
- IOUCSUBTZWXKTA-UHFFFAOYSA-N dipotassium;dioxido(oxo)tin Chemical compound [K+].[K+].[O-][Sn]([O-])=O IOUCSUBTZWXKTA-UHFFFAOYSA-N 0.000 description 1
- TVQLLNFANZSCGY-UHFFFAOYSA-N disodium;dioxido(oxo)tin Chemical compound [Na+].[Na+].[O-][Sn]([O-])=O TVQLLNFANZSCGY-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- CCQLOTNQWSBPLX-UHFFFAOYSA-N manganese phosphoric acid Chemical compound [Mn].OP(O)(O)=O CCQLOTNQWSBPLX-UHFFFAOYSA-N 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- KVOIJEARBNBHHP-UHFFFAOYSA-N potassium;oxido(oxo)alumane Chemical compound [K+].[O-][Al]=O KVOIJEARBNBHHP-UHFFFAOYSA-N 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 229940005657 pyrophosphoric acid Drugs 0.000 description 1
- ZVJHJDDKYZXRJI-UHFFFAOYSA-N pyrroline Natural products C1CC=NC1 ZVJHJDDKYZXRJI-UHFFFAOYSA-N 0.000 description 1
- CMZUMMUJMWNLFH-UHFFFAOYSA-N sodium metavanadate Chemical compound [Na+].[O-][V](=O)=O CMZUMMUJMWNLFH-UHFFFAOYSA-N 0.000 description 1
- 229940079864 sodium stannate Drugs 0.000 description 1
- 125000005402 stannate group Chemical group 0.000 description 1
- VKFFEYLSKIYTSJ-UHFFFAOYSA-N tetraazanium;phosphonato phosphate Chemical compound [NH4+].[NH4+].[NH4+].[NH4+].[O-]P([O-])(=O)OP([O-])([O-])=O VKFFEYLSKIYTSJ-UHFFFAOYSA-N 0.000 description 1
- RYCLIXPGLDDLTM-UHFFFAOYSA-J tetrapotassium;phosphonato phosphate Chemical compound [K+].[K+].[K+].[K+].[O-]P([O-])(=O)OP([O-])([O-])=O RYCLIXPGLDDLTM-UHFFFAOYSA-J 0.000 description 1
- LSKHZZSZLMMIMU-UHFFFAOYSA-K tripotassium;hydron;phosphonato phosphate Chemical compound [K+].[K+].[K+].OP([O-])(=O)OP([O-])([O-])=O LSKHZZSZLMMIMU-UHFFFAOYSA-K 0.000 description 1
- MLIKYFGFHUYZAL-UHFFFAOYSA-K trisodium;hydron;phosphonato phosphate Chemical compound [Na+].[Na+].[Na+].OP([O-])(=O)OP([O-])([O-])=O MLIKYFGFHUYZAL-UHFFFAOYSA-K 0.000 description 1
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- Chemical Treatment Of Metals (AREA)
- Other Surface Treatments For Metallic Materials (AREA)
Description
本発明は耐食性及び塗装密着性に優れた表面を有するマグネシウム合金を得るためのマグネシウム合金の表面処理方法に関する。 The present invention relates to a magnesium alloy surface treatment method for obtaining a magnesium alloy having a surface excellent in corrosion resistance and paint adhesion.
マグネシウム合金は実用金属のなかでは密度が最も小さく、比強度が高く、リサイクル性、電磁波シールド性等に優れた特性を有しているため、プラスチックに代わる素材としてデジタルカメラ、ノートパソコン、携帯電話、ビデオカメラ等の筐体や部品、自動車部品に実用されてきている。しかしながら、マグネシウム合金は耐食性が劣るため、従来からマグネシウム合金部材の多くは化学的浸漬処理によって化成皮膜を生成させ、これによって耐食性を付与している。また、この化成皮膜は有機質皮膜との密着性が優れているので、化成処理後に塗装処理を施せば、一般的な腐食環境においても十分に耐食性を維持することができる。 Magnesium alloy has the lowest density among practical metals, high specific strength, and excellent properties such as recyclability and electromagnetic wave shielding, so digital cameras, laptop computers, mobile phones, It has been put into practical use for housings and parts such as video cameras and automobile parts. However, since magnesium alloys are inferior in corrosion resistance, conventionally, many magnesium alloy members have formed chemical conversion films by chemical immersion treatment, thereby imparting corrosion resistance. Moreover, since this chemical conversion film is excellent in adhesiveness with the organic film, if the coating treatment is performed after the chemical conversion treatment, the corrosion resistance can be sufficiently maintained even in a general corrosive environment.
以前には、マグネシウム合金用の化成処理としては、ＪＩＳ Ｈ ８６５１やＭＩＬ−Ｍ−３１７１等のクロム系化成処理が主流であった。しかしながら、これらのクロム系化成処理液は、いずれも６価クロムイオンを含有しており、人体及び地球環境にとって有害性を伴うものであった。このため近年では、ノンクロム系の化成処理液が研究され、実用化されるようになってきた。ノンクロム系化成処理液としてはリン酸−マンガン系化成処理液（例えば、特許文献１参照。）、リン酸−マンガン−カルシウム系化成処理液（例えば、特許文献２参照。）、リン酸−マンガン−カルシウム−バナジウム系化成処理液（例えば、特許文献３参照。）等がある。 Previously, as a chemical conversion treatment for a magnesium alloy, chromium-based chemical conversion treatment such as JIS H8651 and MIL-M-3171 has been mainstream. However, these chromium-based chemical conversion treatment solutions all contain hexavalent chromium ions and are harmful to the human body and the global environment. Therefore, in recent years, non-chromium chemical conversion treatment liquids have been studied and put into practical use. As the non-chromium chemical conversion treatment liquid, a phosphoric acid-manganese chemical conversion treatment liquid (for example, see Patent Document 1), a phosphoric acid-manganese-calcium chemical conversion treatment liquid (for example, see Patent Document 2), and phosphoric acid-manganese- There is a calcium-vanadium chemical conversion treatment solution (for example, see Patent Document 3).
耐食性及び塗装密着性が更に改善された表面を有するマグネシウム合金が引き続き求められている。本発明もまた耐食性及び塗装密着性に優れた表面を有するマグネシウム合金を得るためのマグネシウム合金の表面処理方法を提供することを目的としている。 There is a continuing need for magnesium alloys having surfaces with further improved corrosion resistance and paint adhesion. Another object of the present invention is to provide a surface treatment method of a magnesium alloy for obtaining a magnesium alloy having a surface excellent in corrosion resistance and paint adhesion.
本発明者らは上記の目的を達成するために種々検討した結果、特定組成の電解液を用いて陽極酸化処理し、次いで特定組成の化成処理液を用いて化成処理することにより耐食性及び塗装密着性に優れた表面を有するマグネシウム合金が得られることを見出し、本発明を完成した。 As a result of various investigations to achieve the above object, the present inventors have conducted anodizing treatment using an electrolytic solution having a specific composition, and then performing chemical conversion treatment using a chemical conversion treatment solution having a specific composition. The present invention was completed by finding that a magnesium alloy having a surface with excellent properties can be obtained.
即ち、本発明のマグネシウム合金の表面処理方法は、
マグネシウム合金の表面を
リン酸イオン ３〜１５ｇ／Ｌ
アルミン酸イオン １〜６ｇ／Ｌ
フッ化物イオン １〜１０ｇ／Ｌ
水酸化アルカリ金属 １〜８ｇ／Ｌ（水酸化ナトリウム換算で）
を含む電解液中に浸漬し、好ましくは３０〜６０℃で好ましくは電流密度０．５〜２Ａ／ｄｍ２で好ましくは３〜１０分間、陽極酸化処理して陽極酸化皮膜を形成し、次いで
ピロリン酸イオン １〜１００ｇ／Ｌ
リン酸イオン １〜６０ｇ／Ｌ
フッ化物イオン ０．５〜１０ｇ／Ｌ
スズ酸イオン ０．１〜１０ｇ／Ｌ
メタバナジン酸イオン ０．１〜１０ｇ／Ｌ
を含む化成処理液で、好ましくは２０〜６０℃で好ましくは０．５〜５分間、化成処理して皮膜を形成することを特徴とする。
That is, the surface treatment method of the magnesium alloy of the present invention,
The surface of the magnesium alloy is phosphate ion 3-15g / L
Aluminate ion 1-6g / L
Fluoride ion 1-10g / L
Alkali metal hydroxide 1-8g / L (in terms of sodium hydroxide)
And anodized to form an anodized film , preferably at 30 to 60 ° C., preferably at a current density of 0.5 to 2 A / dm 2 and preferably for 3 to 10 minutes, and then pyrroline Acid ion 1-100g / L
Phosphate ion 1-60g / L
Fluoride ion 0.5-10g / L
Stannate ion 0.1 ~ 10g / L
Metavanadate ion 0.1-10g / L
And a chemical conversion treatment solution, preferably at 20 to 60 ° C., preferably for 0.5 to 5 minutes, to form a film .
また、本発明のマグネシウム合金の表面処理方法は、
マグネシウム合金の表面を
フッ化アンモニウム ０．４〜１０ｇ／Ｌ
を含む溶液中に浸漬して、好ましくは２０〜５０℃で好ましくは２〜１０分間表面調整し、次いで
リン酸イオン ３〜１５ｇ／Ｌ
アルミン酸イオン １〜６ｇ／Ｌ
フッ化物イオン １〜１０ｇ／Ｌ
水酸化アルカリ金属 １〜８ｇ／Ｌ（水酸化ナトリウム換算で）
を含む電解液中に浸漬し、３０〜６０℃で好ましくは電流密度０．５〜２Ａ／ｄｍ２で３〜１０分間陽極酸化処理して陽極酸化皮膜を形成し、更に
ピロリン酸イオン １〜１００ｇ／Ｌ
リン酸イオン １〜６０ｇ／Ｌ
フッ化物イオン ０．５〜１０ｇ／Ｌ
スズ酸イオン ０．１〜１０ｇ／Ｌ
メタバナジン酸イオン ０．１〜１０ｇ／Ｌ
を含む化成処理液で、２０〜６０℃で０．５〜５分間化成処理して皮膜を形成することを特徴とする。
The surface treatment method of the magnesium alloy of the present invention,
The surface of the magnesium alloy is 0.4 to 10 g / L ammonium fluoride.
So that the surface is preferably adjusted at 20 to 50 ° C., preferably for 2 to 10 minutes, and then phosphate ions 3 to 15 g / L
Aluminate ion 1-6g / L
Fluoride ion 1-10g / L
Alkali metal hydroxide 1-8g / L (in terms of sodium hydroxide)
And anodized at 30-60 ° C., preferably at a current density of 0.5-2 A / dm 2 for 3-10 minutes to form an anodized film, and further pyrophosphate ions 1-100 g / L
Phosphate ion 1-60g / L
Fluoride ion 0.5-10g / L
Stannate ion 0.1 ~ 10g / L
Metavanadate ion 0.1-10g / L
The film is formed by chemical conversion treatment at 20 to 60 ° C. for 0.5 to 5 minutes.
本発明のマグネシウム合金の表面処理方法で得られるマグネシウム合金の表面は耐食性及び塗装密着性に優れている。 The surface of the magnesium alloy obtained by the magnesium alloy surface treatment method of the present invention is excellent in corrosion resistance and paint adhesion.
本発明の表面処理方法で処理できるマグネシウム合金はその組成については特に限定されず、産業上使用される何れのマグネシウム合金にも適用できる。そのマグネシウム合金の具体例としては、ＡＺ９２、ＡＺ９１、ＡＺ８０、ＡＺ６３、ＡＺ６１、ＡＺ３１、ＡＭ１００、ＡＭ６０、ＡＭ５０、ＡＭ２０、ＡＳ４１、ＡＳ２１、ＡＥ４２、ＡＣＭ５２２（Ｍｇ−５Ａｌ−２Ｃａ−２ＲＥ）等が挙げられる。また、本発明の表面処理方法の対象となる部材としては、これらのマグネシウム合金の鋳造品、ダイカスト品、射出成形品（半溶融鋳造またはチキソモールド）、展伸材（押出材、圧延材、鍛造材）の板及びプレス品等が挙げられる。 The composition of the magnesium alloy that can be treated by the surface treatment method of the present invention is not particularly limited, and can be applied to any magnesium alloy used in the industry. Specific examples of the magnesium alloy include AZ92, AZ91, AZ80, AZ63, AZ61, AZ31, AM100, AM60, AM50, AM20, AS41, AS21, AE42, ACM522 (Mg-5Al-2Ca-2RE) and the like. Further, as a member to be subjected to the surface treatment method of the present invention, these magnesium alloy castings, die-casting products, injection-molded products (semi-molten casting or thixo mold), wrought materials (extruded materials, rolled materials, forged materials) Material) plates and pressed products.
本発明の表面処理方法で用いる化成処理液はピロリン酸イオン、リン酸イオン、フッ化物イオン、スズ酸イオン及びメタバナジン酸イオンを含む。ピロリン酸イオン源としてピロリン酸や、ピロリン酸ナトリウム、ピロリン酸水素ナトリウム、ピロリン酸カリウム、ピロリン酸水素カリウム、ピロリン酸アンモニウム等の水溶性ピロリン酸塩を用いることができる。リン酸イオン源としてリン酸や、リン酸二水素ナトリウム、リン酸水素二ナトリウム、リン酸三ナトリウム、リン酸二水素カリウム、リン酸水素二カリウム、リン酸三カリウム等の水溶性リン酸塩を用いることができる。フッ化物イオン源としてフッ化水素酸や、アルカリ金属フッ化物であるフッ化ナトリウム、フッ化カリウム等やフッ化アンモニウム等の水溶性フッ化水素酸塩を用いることができる。スズ酸イオン源としてスズ酸や、スズ酸ナトリウム、スズ酸カリウム、スズ酸アンモニウム等の水溶性スズ酸塩を用いることができる。また、メタバナジン酸イオン源としてメタバナジン酸や、メタバナジン酸ナトリウム、メタバナジン酸カリウム、メタバナジン酸アンモニウム等の水溶性メタバナジン酸塩を用いることができる。 The chemical conversion treatment solution used in the surface treatment method of the present invention contains pyrophosphate ions, phosphate ions, fluoride ions, stannate ions, and metavanadate ions. As the pyrophosphate ion source, pyrophosphoric acid, or a water-soluble pyrophosphate such as sodium pyrophosphate, sodium hydrogen pyrophosphate, potassium pyrophosphate, potassium hydrogen pyrophosphate, or ammonium pyrophosphate can be used. Phosphoric acid as a phosphate ion source and water-soluble phosphates such as sodium dihydrogen phosphate, disodium hydrogen phosphate, trisodium phosphate, potassium dihydrogen phosphate, dipotassium hydrogen phosphate, tripotassium phosphate Can be used. As the fluoride ion source, hydrofluoric acid or water-soluble hydrofluoric acid salt such as sodium fluoride, potassium fluoride or ammonium fluoride which is an alkali metal fluoride can be used. As a stannate ion source, water-soluble stannates such as stannic acid, sodium stannate, potassium stannate, and ammonium stannate can be used. Moreover, water-soluble metavanadates, such as metavanadate, sodium metavanadate, potassium metavanadate, ammonium metavanadate, can be used as a metavanadate ion source.
本発明の表面処理方法で用いる化成処理液においては、ピロリン酸イオン濃度は１〜１００ｇ／Ｌ、好ましくは５〜５０ｇ／Ｌであり（ピロリン酸ナトリウム濃度として１．５〜１５３ｇ／Ｌ、好ましくは７．６〜７６ｇ／Ｌ、他の成分についての同様）、リン酸イオン濃度は１〜６０ｇ／Ｌ、好ましくは３〜３０ｇ／Ｌであり、フッ化物イオン濃度は０．５〜１０ｇ／Ｌ、好ましくは１〜８ｇ／Ｌであり、スズ酸イオン濃度は０．１〜１０ｇ／Ｌ、好ましくは０．５〜８ｇ／Ｌであり、メタバナジン酸イオン濃度は０．１〜１０ｇ／Ｌ、好ましくは０．５〜８ｇ／Ｌである。 In the chemical conversion treatment solution used in the surface treatment method of the present invention, the pyrophosphate ion concentration is 1 to 100 g / L, preferably 5 to 50 g / L (sodium pyrophosphate concentration is 1.5 to 153 g / L, preferably 7.6 to 76 g / L, the same for other components), the phosphate ion concentration is 1 to 60 g / L, preferably 3 to 30 g / L, and the fluoride ion concentration is 0.5 to 10 g / L, Preferably, it is 1-8 g / L, the stannate ion concentration is 0.1-10 g / L, preferably 0.5-8 g / L, and the metavanadate ion concentration is 0.1-10 g / L, preferably 0.5 to 8 g / L.
本発明の表面処理方法で採用する化成処理として上記の化成処理液を用い、化成処理液のｐＨをＮａＯＨ等のアルカリで好ましくは９〜１１、実際には９．５程度に調整し、化成処理液の温度を好ましくは２０〜６０℃、より好ましくは３０〜５５℃に維持し、好ましくは０．５〜５分間、より好ましくは１〜４分間処理する。化成処理液の温度が２０℃よりも低い場合には反応速度が小さく、皮膜生成までに長時間を要し、また６０℃よりも高い場合には皮膜の生成速度は大きいが、皮膜に肌ムラが発生し易くなる傾向がある。 As the chemical conversion treatment employed in the surface treatment method of the present invention, the chemical conversion treatment solution is used, and the pH of the chemical conversion treatment solution is preferably adjusted to 9 to 11, preferably about 9.5 with an alkali such as NaOH. The temperature of the liquid is preferably maintained at 20 to 60 ° C., more preferably 30 to 55 ° C., preferably 0.5 to 5 minutes, more preferably 1 to 4 minutes. When the temperature of the chemical conversion treatment liquid is lower than 20 ° C., the reaction rate is low, and it takes a long time until the film is formed. Tends to occur.
マグネシウム合金の表面を上記のように化成処理することにより耐食性及び塗装密着性が改善された表面を有するマグネシウム合金を得ることができる。しかしながら、上記のような化成処理に先立ってマグネシウム合金の表面を陽極酸化処理することにより、即ち、表面を陽極酸化処理したマグネシウム合金の表面を上記のように化成処理することにより、耐食性及び塗装密着性に一層優れた表面を有するマグネシウム合金を得ることができる。 By subjecting the surface of the magnesium alloy to chemical conversion treatment as described above, a magnesium alloy having a surface with improved corrosion resistance and paint adhesion can be obtained. However, by anodizing the surface of the magnesium alloy prior to the chemical conversion treatment as described above, that is, by subjecting the surface of the magnesium alloy anodized to the chemical conversion treatment as described above, the corrosion resistance and paint adhesion A magnesium alloy having a surface with even better properties can be obtained.
本発明の表面処理方法で用いる陽極酸化処理のための電解液はリン酸イオン、アルミン酸イオン、フッ化物イオン及び水酸化アルカリ金属を含む。リン酸イオン源としてリン酸や、リン酸二水素ナトリウム、リン酸水素二ナトリウム、リン酸三ナトリウム、リン酸二水素カリウム、リン酸水素二カリウム、リン酸三カリウム等の水溶性リン酸塩を用いることができる。アルミン酸イオン源としてアルミン酸や、アルミン酸ナトリウム、アルミン酸カリウム等の水溶性アルミン酸塩を用いることができる。フッ化物イオン源としてフッ化水素酸や、アルカリ金属フッ化物であるフッ化ナトリウム、フッ化カリウム等やフッ化アンモニウム等の水溶性フッ化水素酸塩を用いることができる。水酸化アルカリ金属として水酸化ナトリウム、水酸化カリウム等の水溶性水酸化アルカリ金属を用いることができる。 The electrolytic solution for anodizing treatment used in the surface treatment method of the present invention contains phosphate ions, aluminate ions, fluoride ions, and alkali metal hydroxide. Phosphoric acid as a phosphate ion source and water-soluble phosphates such as sodium dihydrogen phosphate, disodium hydrogen phosphate, trisodium phosphate, potassium dihydrogen phosphate, dipotassium hydrogen phosphate, tripotassium phosphate Can be used. As the aluminate ion source, aluminate, water-soluble aluminate such as sodium aluminate and potassium aluminate can be used. As the fluoride ion source, hydrofluoric acid or water-soluble hydrofluoric acid salt such as sodium fluoride, potassium fluoride or ammonium fluoride which is an alkali metal fluoride can be used. As the alkali metal hydroxide, a water-soluble alkali metal hydroxide such as sodium hydroxide or potassium hydroxide can be used.
本発明の表面処理方法で陽極酸化処理に用いる電解液においては、リン酸イオン濃度は３〜１５ｇ／Ｌ、好ましくは５〜１２ｇ／Ｌであり、アルミン酸イオン濃度は１〜６ｇ／Ｌ、好ましくは２〜５ｇ／Ｌであり、フッ化物イオン濃度は１〜１０ｇ／Ｌ、好ましくは３〜８ｇ／Ｌであり、水酸化アルカリ金属濃度は水酸化ナトリウム換算で１〜８ｇ／Ｌ、好ましくは２〜６ｇ／Ｌである。 In the electrolytic solution used for the anodizing treatment in the surface treatment method of the present invention, the phosphate ion concentration is 3 to 15 g / L, preferably 5 to 12 g / L, and the aluminate ion concentration is 1 to 6 g / L, preferably Is 2 to 5 g / L, fluoride ion concentration is 1 to 10 g / L, preferably 3 to 8 g / L, and alkali metal hydroxide concentration is 1 to 8 g / L in terms of sodium hydroxide, preferably 2 ~ 6 g / L.
本発明の表面処理方法で採用する陽極酸化処理は上記の電解液を用い、電解液のｐＨをＮａＯＨ等のアルカリで好ましくは１０〜１３．５、実際には１２〜１３前後に調整し、電解液の温度を好ましくは３０〜６０℃、より好ましくは３５〜５５℃に維持し、電流密度を好ましくは０．５〜２Ａ／ｄｍ２に維持して、好ましくは３〜１０分間、より好ましくは４〜８分間処理する。 The anodizing treatment employed in the surface treatment method of the present invention uses the above-described electrolytic solution, and the pH of the electrolytic solution is preferably adjusted to 10 to 13.5 with an alkali such as NaOH, and actually adjusted to about 12 to 13 for electrolysis. The temperature of the liquid is preferably maintained at 30 to 60 ° C., more preferably 35 to 55 ° C., and the current density is preferably maintained at 0.5 to 2 A / dm 2 , preferably 3 to 10 minutes, more preferably Process for 4-8 minutes.
マグネシウム合金の表面を上記のように陽極酸化処理し、次いで化成処理することにより、耐食性及び塗装密着性に一層優れた表面を有するマグネシウム合金を得ることができる。 By subjecting the surface of the magnesium alloy to anodization treatment as described above and then chemical conversion treatment, a magnesium alloy having a surface with further excellent corrosion resistance and coating adhesion can be obtained.
マグネシウム合金の表面への陽極酸化皮膜の密着性、耐剥離性を改善するために陽極酸化処理に先立ってマグネシウム合金の表面をフッ化アンモニウム含む溶液中に浸漬して表面調整する（ＭｇＦ２の膜を形成させる）ことが好ましい。即ち、表面にＭｇＦ２の膜を形成させたマグネシウム合金の表面を上記のように陽極酸化処理することが好ましい。 In order to improve the adhesion and peel resistance of the anodic oxide film to the surface of the magnesium alloy, the surface of the magnesium alloy is dipped in a solution containing ammonium fluoride prior to the anodizing treatment (MgF 2 film) Is preferably formed). That is, it is preferable to anodize the surface of the magnesium alloy having the MgF 2 film formed on the surface as described above.
本発明の表面処理方法で表面調整（ＭｇＦ２膜の形成）に用いる溶液はフッ化アンモニウムを含む。フッ化アンモニウムの代わりにフッ化ナトリウムやフッ化カリウムを用いた場合には目的とする効果が得られない。表面調整に用いる溶液中のフッ化アンモニウム濃度は０．４〜１０ｇ／Ｌ、好ましくは０．７〜８ｇ／Ｌである。 The solution used for surface adjustment (formation of MgF 2 film) in the surface treatment method of the present invention contains ammonium fluoride. When sodium fluoride or potassium fluoride is used instead of ammonium fluoride, the intended effect cannot be obtained. The ammonium fluoride concentration in the solution used for the surface adjustment is 0.4 to 10 g / L, preferably 0.7 to 8 g / L.
本発明の表面処理方法で採用する表面調整処理においては、上記の溶液を用い、溶液のｐＨをＮＨ４ＦやＮＨ３などの弱酸や弱アルカリで好ましくは６〜８、実際には６．５前後に調整し、溶液の温度を好ましくは２０〜５０℃、より好ましくは３０〜５０℃に維持し、好ましくは２〜１０分間、より好ましくは３〜８分間処理する。 In the surface conditioning treatment employed in the surface treatment method of the present invention, the above solution is used, and the pH of the solution is preferably 6 to 8, preferably 6.5 to 8 with a weak acid or weak alkali such as NH 4 F or NH 3. The temperature of the solution is preferably maintained at 20 to 50 ° C., more preferably 30 to 50 ° C., and preferably 2 to 10 minutes, more preferably 3 to 8 minutes.
本発明の表面処理方法においては、表面をエッチング処理し、スマット除去処理したマグネシウム合金を用いることが好ましい。このエッチング処理及びスマット除去処理は周知の技術であり、本発明においては周知のエッチング処理及びスマット除去処理をそのまま採用することができる。 In the surface treatment method of the present invention, it is preferable to use a magnesium alloy obtained by etching the surface and removing the smut. This etching process and smut removal process are well-known techniques, and in the present invention, a well-known etching process and smut removal process can be employed as they are.
本発明の表面処理方法においては、化成処理した後、純水で洗浄し、乾燥することが好ましい。この純水での洗浄処理、乾燥処理は周知の技術であり、本発明においては周知の純水での洗浄処理、乾燥処理をそのまま採用することができる。 In the surface treatment method of the present invention, after the chemical conversion treatment, it is preferable to wash with pure water and dry. The cleaning process and the drying process with pure water are well-known techniques. In the present invention, the well-known cleaning process and drying process with pure water can be employed as they are.
本発明の表面処理方法においては、乾燥した後、塗装することができる。マグネシウム合金表面の塗装技術は周知であり、本発明においては周知の塗装方法をそのまま採用することができる。塗装は、例えば、溶剤型塗料、水溶性塗料、粉体塗料等一般的な塗料を用いて行うことができる。具体的には、水溶性カチオン電着塗料を用い、電解電圧１００〜１５０Ｖ、処理時間３分、塗膜厚１０〜２０μｍ、乾燥条件１５０℃、３０分で塗布し、その上にトップコートとして、アクリル系塗料を用いて塗膜厚１０〜２５μｍ，乾燥条件１５０℃、３０分で塗装する。 In the surface treatment method of the present invention, the coating can be performed after drying. The coating technique of the magnesium alloy surface is well known, and in the present invention, a well-known coating method can be employed as it is. The coating can be performed using a common paint such as a solvent-type paint, a water-soluble paint, or a powder paint. Specifically, using a water-soluble cationic electrodeposition coating, applied at an electrolysis voltage of 100 to 150 V, a treatment time of 3 minutes, a coating thickness of 10 to 20 μm, a drying condition of 150 ° C. for 30 minutes, and a top coat thereon. Using an acrylic paint, coating is performed at a coating thickness of 10 to 25 μm and drying conditions of 150 ° C. for 30 minutes.
以下に実施例及び比較例によって本発明を具体的に説明する。 The present invention will be specifically described below with reference to examples and comparative examples.
実施例１〜５、比較例１〜３
マグネシウム合金（ＡＺ９１Ｄ）製の長さ１０ｃｍ、幅５ｃｍ、厚さ２ｍｍの試験片を複数個用意し、各々の試験片をエタノールで脱脂し、水洗した。次いで硫酸１１ｍＬ／Ｌ及びクエン酸二水素カリウム１８．４ｇ／Ｌを含有する６０℃の溶液中に１分間浸漬してエッチングし、水洗した。その後、ＮａＯＨを５０ｇ／Ｌ含有する６０℃の溶液中に３分間浸漬してスマット除去し、水洗した。
Examples 1-5, Comparative Examples 1-3
A plurality of test pieces made of magnesium alloy (AZ91D) having a length of 10 cm, a width of 5 cm, and a thickness of 2 mm were prepared. Each test piece was degreased with ethanol and washed with water. Subsequently, it was immersed in a 60 ° C. solution containing 11 mL / L sulfuric acid and 18.4 g / L potassium dihydrogen citrate for 1 minute, etched, and washed with water. Then, it was immersed in a 60 ° C. solution containing 50 g / L of NaOH for 3 minutes to remove smut, and washed with water.
上記のように処理した複数の試験片の一部について、フッ化アンモニウムを１ｇ／Ｌ含有するｐＨ６．５、温度４０℃の溶液中に５分間浸漬して表面調整（ＭｇＦ２幕の形成）を行った。表面調整の実施の有無は第１表に示す通りであった。 A portion of the plurality of test pieces treated as described above was immersed in a solution containing 1 g / L of ammonium fluoride at pH 6.5 and temperature of 40 ° C. for 5 minutes for surface adjustment (formation of MgF 2 curtain). went. The presence / absence of surface adjustment was as shown in Table 1.
陽極酸化処理については
リン酸水素二カリウム ８ｇ／Ｌ
アルミン酸ナトリウム ３ｇ／Ｌ
フッ化カリウム ４ｇ／Ｌ
水酸化ナトリウム ５ｇ／Ｌ
を含むｐＨ１３．０、温度５０℃（スタート時）の電解液中に試験片を浸漬し、電流密度（定電流）１Ａ／ｄｍ２で１５分間陽極酸化処理した。陽極酸化処理の有無は第１表に示す通りであった。
About anodizing treatment Dipotassium hydrogen phosphate 8g / L
Sodium aluminate 3g / L
Potassium fluoride 4g / L
Sodium hydroxide 5g / L
The test piece was immersed in an electrolyte solution having a pH of 13.0 and a temperature of 50 ° C. (starting time), and anodized at a current density (constant current) of 1 A / dm 2 for 15 minutes. The presence or absence of anodizing treatment was as shown in Table 1.
化成処理については、第１表に記載の組成を有するｐＨ９．５、温度４５℃の化成処理液中に２分間浸漬して化成処理した。その後、水洗し、純水で洗浄し、乾燥した。 Regarding the chemical conversion treatment, chemical conversion treatment was performed by immersing in a chemical conversion treatment solution having a composition shown in Table 1 at pH 9.5 and a temperature of 45 ° C. for 2 minutes. Thereafter, it was washed with water, washed with pure water, and dried.
実施例１〜５及び比較例１〜３に従って処理したマグネシウム合金（ＡＺ９１Ｄ）製の試験片について、ＪＩＳ Ｚ ２３７１に従って塩水噴霧試験を実施した。第１表に記載の時間塩水噴霧した後の表面の腐食状態をレイティングナンバー標準図表と照合して評価した。その結果は第１表に記載の通りであった。 About the test piece made from the magnesium alloy (AZ91D) processed according to Examples 1-5 and Comparative Examples 1-3, the salt spray test was implemented according to JISZ2371. The corrosion state of the surface after spraying with salt water for the time indicated in Table 1 was evaluated against the rating number standard chart. The results were as shown in Table 1.
実施例６
ＡＺ９１Ｄ製の試験片の代わりにＡＣＭ５２２（Ｍｇ−５Ａｌ−２Ｃａ−２ＲＥ）製の試験片を用いた以外は実施例３と同様に処理し、実施例３と同様に塩水噴霧試験を実施した。その結果は塩水噴霧時間１６８ｈｒ後及び２４０ｈｒ後のレイティングナンバーは１０であり、３６０ｈｒ後のレイティングナンバーは９．５であった。
Example 6
A salt spray test was conducted in the same manner as in Example 3 except that a test piece made of ACM522 (Mg-5Al-2Ca-2RE) was used instead of the test piece made of AZ91D. As a result, the rating number after salt spraying time 168 hr and 240 hr was 10, and the rating number after 360 hr was 9.5.
Claims (5)
リン酸イオン ３〜１５ｇ／Ｌ
アルミン酸イオン １〜６ｇ／Ｌ
フッ化物イオン １〜１０ｇ／Ｌ
水酸化アルカリ金属 １〜８ｇ／Ｌ（水酸化ナトリウム換算で）
を含む電解液中に浸漬し、陽極酸化処理して陽極酸化皮膜を形成し、次いで
ピロリン酸イオン １〜１００ｇ／Ｌ
リン酸イオン １〜６０ｇ／Ｌ
フッ化物イオン ０．１〜１０ｇ／Ｌ
スズ酸イオン ０．１〜１０ｇ／Ｌ
メタバナジン酸イオン ０．１〜１０ｇ／Ｌ
を含む化成処理液で化成処理して皮膜を形成することを特徴とするマグネシウム合金の表面処理方法。 The surface of the magnesium alloy is phosphate ion 3-15g / L
Aluminate ion 1-6g / L
Fluoride ion 1-10g / L
Alkali metal hydroxide 1-8g / L (in terms of sodium hydroxide)
Soaked in an electrolytic solution containing anodic oxidation to form an anodic oxide film, and then pyrophosphate ions 1 to 100 g / L
Phosphate ion 1-60g / L
Fluoride ion 0.1 ~ 10g / L
Stannate ion 0.1 ~ 10g / L
Metavanadate ion 0.1-10g / L
A surface treatment method for a magnesium alloy, characterized by forming a film by chemical conversion treatment with a chemical conversion treatment solution containing
フッ化アンモニウム ０．４〜１０ｇ／Ｌ
を含む溶液中に浸漬して表面調整し、次いで
リン酸イオン ３〜１５ｇ／Ｌ
アルミン酸イオン １〜６ｇ／Ｌ
フッ化物イオン １〜１０ｇ／Ｌ
水酸化アルカリ金属 １〜８ｇ／Ｌ（水酸化ナトリウム換算で）
を含む電解液中に浸漬し、陽極酸化処理して陽極酸化皮膜を形成し、更に
ピロリン酸イオン １〜１００ｇ／Ｌ
リン酸イオン １〜６０ｇ／Ｌ
フッ化物イオン ０．１〜１０ｇ／Ｌ
スズ酸イオン ０．１〜１０ｇ／Ｌ
メタバナジン酸イオン ０．１〜１０ｇ／Ｌ
を含む化成処理液で化成処理して皮膜を形成することを特徴とするマグネシウム合金の表面処理方法。 The surface of the magnesium alloy is 0.4 to 10 g / L ammonium fluoride.
Surface adjustment by immersion in a solution containing 3 to 15 g / L phosphate ion
Aluminate ion 1-6g / L
Fluoride ion 1-10g / L
Alkali metal hydroxide 1-8g / L (in terms of sodium hydroxide)
Soaked in an electrolyte solution containing anodic oxidation to form an anodic oxide film, and further pyrophosphate ions 1 to 100 g / L
Phosphate ion 1-60g / L
Fluoride ion 0.1 ~ 10g / L
Stannate ion 0.1 ~ 10g / L
Metavanadate ion 0.1-10g / L
A surface treatment method for a magnesium alloy, characterized by forming a film by chemical conversion treatment with a chemical conversion treatment solution containing
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| JP6083020B2 (en) * | 2012-10-24 | 2017-02-22 | 株式会社正信 | Surface treatment method of magnesium or magnesium alloy, acid detergent and chemical conversion treatment agent, and chemical conversion treatment structure of magnesium or magnesium alloy |
| JP6083562B2 (en) * | 2013-03-27 | 2017-02-22 | 株式会社正信 | Surface treatment method, chemical conversion treatment agent, and chemical conversion treatment structure |
| CN104651908B (en) * | 2013-11-25 | 2017-09-29 | 中国兵器科学研究院宁波分院 | The preparation method and method for sealing of a kind of Mg alloy surface ceramic film |
| JP2016113676A (en) * | 2014-12-16 | 2016-06-23 | 富士通株式会社 | Method for manufacturing housing having chemical conversion coating, housing having chemical conversion coating and tool for holding housing |
| WO2019059255A1 (en) * | 2017-09-20 | 2019-03-28 | ミリオン化学株式会社 | Magnesium-lithium alloy and surface-treatment method thereof |
| JP6553268B2 (en) * | 2017-09-20 | 2019-07-31 | ミリオン化学株式会社 | Magnesium-lithium alloy and surface treatment method thereof |
| JP7235254B2 (en) * | 2021-04-09 | 2023-03-08 | 三菱重工業株式会社 | Method for modifying surface of Mg-Al-Ca alloy |
| KR102339453B1 (en) * | 2021-09-02 | 2021-12-14 | 박중수 | Magnesium etching treatment method |
| CN113774462B (en) * | 2021-10-22 | 2023-03-28 | 上海康德莱医疗器械股份有限公司 | Magnesium alloy surface treatment method and treated magnesium alloy |
| CN114875396B (en) * | 2022-04-28 | 2023-03-14 | 厦门大学 | Surface treatment method of magnesium or magnesium alloy |
| CN115305552A (en) * | 2022-08-05 | 2022-11-08 | 河南大学 | Electrolyte formula and method for preparing high-corrosion-resistance magnesium alloy micro-arc oxidation coating based on electrolyte formula |
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| JPS6134200A (en) * | 1984-07-26 | 1986-02-18 | Matsufumi Takatani | Surface treatment of magnesium and its alloy |
| EP0573585B1 (en) * | 1991-02-26 | 1994-12-14 | Technology Applications Group, Inc. | Two-step chemical/electrochemical process for coating magnesium |
| JPH0770759A (en) * | 1993-08-31 | 1995-03-14 | Kobe Steel Ltd | Mg or mg alloy material having high corrosion resistance |
| JP4223088B2 (en) * | 1998-02-23 | 2009-02-12 | 三井金属鉱業株式会社 | Corrosion-resistant magnesium material product exhibiting metallic substrate gloss and method for producing the same |
| JP2002322567A (en) * | 2001-04-24 | 2002-11-08 | Chiyoda Chemical Kk | Surface treatment method for casting and cast article |
| JP2002371380A (en) * | 2001-06-15 | 2002-12-26 | Fujitsu Ltd | Magnesium material product having corrosion resistance and manufacturing method therefor |
| US6887320B2 (en) * | 2002-02-11 | 2005-05-03 | United Technologies Corporation | Corrosion resistant, chromate-free conversion coating for magnesium alloys |
| US6692583B2 (en) * | 2002-02-14 | 2004-02-17 | Jon Bengston | Magnesium conversion coating composition and method of using same |
| US20040256030A1 (en) * | 2003-06-20 | 2004-12-23 | Xia Tang | Corrosion resistant, chromate-free conversion coating for magnesium alloys |
| JP2005281717A (en) * | 2004-03-26 | 2005-10-13 | Kurimoto Ltd | Method for forming chemical conversion-treated film of magnesium alloy |
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