TW573061B - Chemical solution for treating magnesium alloy containing aluminum, surface-treated magnesium alloy product of high corrosion resistance, and method for manufacturing the same - Google Patents

Description

573061 Printed by the Consumer Cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs A7 B7 V. Description of the Invention (i) [Technical Field] The present invention relates to a treatment liquid used for chemically treating the surface of a magnesium alloy containing aluminum. A processing method for producing a highly corrosion-resistant surface-treated magnesium alloy product by chemically treating the surface of a magnesium alloy containing aluminum, and the highly corrosion-resistant surface-treated magnesium alloy product. More specifically, the present invention is a harmful chemical treatment solution with a low concentration of hexavalent chromium, which can provide a treatment solution for surface-treated magnesium alloy products with a longer life and higher corrosion resistance than the conventional CHROMATE treatment solution. And a manufacturing method of a highly corrosion-resistant surface-treated magnesium alloy by chemically treating the surface of an aluminum-containing magnesium alloy by using the treatment liquid, and the highly corrosion-resistant surface-treated magnesium alloy product ° [Background Technology] Known for chemical treatment of magnesium alloys, especially for magnesium alloys containing aluminum. There are three types of chromic acid treatment baths described in JISH8561 specifications, Japanese Patent Laid-Open No. 8-225954, and the like. In addition, the Dow22 method ("'92 Magnesium Operation Manual" (1 " 2) Japan Magnesium Association, page 127), JIS H 8651, η, Japanese Unexamined Patent Publication No. 8_35〇73 al., SAE Technical paper Series , 97〇324 pp7 ll l997, Dayid

Hawke, et al., Metal Finishing 93, 10, pp34-38, 1995 and other known chemical conversion treatment baths containing permanganic acid or a water-soluble salt of manganic acid are known, and JP 57-41376 Gazettes, Japanese Unexamined Patent Publication No. 36-82, and the like have already been known as chemical conversion treatment baths containing water-soluble and titanium salts and / or complex salts of nan short acid. Surface formation of light metal products such as aluminum and these alloys ^ " Does the scale apply? iii quasi (CNS) A4 specification ⑽χ tear public love) ------ 1 0110Λ1 (Please read the precautions on the back before filling out this page) Order: 573061 Printed on paper by the Intellectual Property Bureau Staff Consumer Cooperatives Applicable to Zhongguan Jiaxian (CNS) A4 specifications ⑵G χ 挪 Norwegian hair) 2 A7 V. Description of the invention (2) In recent years, due to environmental problems, in recent years, non-chromatization of the 6-valent network without the use of harmful substances has been directed. However, in terms of the corrosion resistance of chemically treated products, a treatment bath and a treatment method that can outperform the conventional chromic acid treatment bath have not yet been developed. It is still expected to develop a complex salt treatment bath with a high residual resistance that better suits the purpose and condition. The subject of this month is to provide a chromic acid treatment bath containing chromic acid ^, which is a harmful substance of 0 valent chromium, but it has a lower hexavalent complex concentration than the conventional chromate treatment baths. Concentration, but still can provide a surface treatment town alloy product treatment liquid with longer life and higher residual resistance than the chromate treatment solution. Another object is to provide a method for manufacturing a high-residue surface-treated town-alloy product that chemically treats the surface of aluminum-containing magnesium gold by using the treatment liquid, and the high-corrosion-resistant surface-treated magnesium alloy product. [Disclosure of the Invention] In order to achieve the above-mentioned problem, as a result of a deliberate study by the present inventors, it was found that by adding a water-soluble salt containing chromic acid, dichromic acid, or the like, manganic acid, ferric acid, or the water-solubility thereof was produced Salt, acid or water-soluble salt of acid: Treatment liquid, add acetic acid or water-soluble salt of acetic acid, and water-soluble salt of phosphoric acid or phosphoric acid to form a treatment liquid, and compare the surface of aluminum-containing magnesium alloy with The treatment temperature and relatively short treatment time can also be used for chemical conversion treatment. 蚀 Corrosion-resistant surface-treated magnesium alloy products, and the life name of the chemical conversion treatment liquid (per unit area can handle aluminum-containing magnesium alloy surface area is large). this invention. That is, the chemical conversion treatment solution for aluminum-containing magnesium alloy of the present invention is characterized by containing chromic acid, dichromic acid, or the concentration conversion of these water-soluble salts — __ 311891

(Please read the notes on the back before filling this page) 573061 V. Description of the invention (3) The amount of chromium trioxide is 3 to 50 g / L, and the concentration of permanganic acid, manganic acid or these water-soluble salts is converted into The amount of potassium permanganate is above 0.5 g / L and the solubility is below. The concentration of nitric acid or a water-soluble salt of nitric acid is converted into a sodium nitrate amount of 3 to 60 g / L, and the concentration of acetic acid or a water-soluble salt of acetic acid is converted. The amount of sodium acetate is 0.5 to 50 g / L, and the concentration of phosphoric acid or a water-soluble salt of phosphoric acid is converted to the amount of sodium phosphate of 0.05 to 8 g / L. In addition, the method for manufacturing a highly corrosion-resistant surface-treated magnesium alloy product according to the present invention is characterized by chemically treating the surface of an aluminum-containing magnesium alloy with a chemical conversion treatment solution of the above-mentioned aluminum-containing magnesium alloy with a liquid temperature of 288 to 368K. To 10 minutes. Furthermore, the high-corrosion-resistant surface-treated magnesium alloy product of the present invention is characterized by being obtained in accordance with the above-mentioned manufacturing method. Eight '[Best Practice of the Present Invention] The aluminum-containing magnesium alloy that is the subject of chemical conversion treatment in the present invention includes all the towns with inscriptions that are practical in various technical fields. M = (AZ) series, Shao Zhong (AM ) Series, Shao Meng (AM) (containing each) series, Shao sulfur series magnesium alloy, so generally these aluminum content is about 2 to i2% by weight. Examples of alloy products include die castings, sand castings, DIECASTING, expanded and forged materials, and the like. Prior to the chemical treatment of the surface of the alloy with inscriptions, the surface of the alloy with inscriptions is dried by solvent dewaxing, pre-treatment or chemical treatment. As for the solvent degreasing, for example, ultrasonic cleaning can be carried out in propidium for 15 minutes. ^ 'S Zhang scale thorns in the family standard (CNS) A4 ^ 721q x 297 public love J 311891-----: ------- installed-(Please read the note on the back? Matters before filling out this page ) • 丨 Order ·

573061

In addition, the pretreatment may be immersed in, for example, a 333K aqueous solution of a potassium pyrophosphate concentration of 35 g / L for 1 minute, followed by water washing and pure water washing. It was then immersed in a 333K solution at a caustic soda concentration of 50 g / L for 3 minutes, and then washed with water and pure water. The above-mentioned solvent degreasing conditions and pretreatment conditions are merely examples of solvent degreasing and mash treatment, and any other solvent degreasing conditions and pretreatment conditions may be used. The chemical conversion treatment solution of the present invention contains chromic acid, dichromic acid, or water-soluble salts thereof, preferably alkali metal salts such as sodium salts, potassium salts, lithium salts, and alkaline earth metal salts such as magnesium salts, and the like. May contain ammonium salts, dibasic salts, and the like. The concentration of chromic acid, dichromic acid or these water-soluble salts in the chemical conversion treatment solution is 3 to 50 g / L, preferably 5 to 50 g / L, when the amount of chromium trioxide is converted. If the concentration of chromic acid, dichromic acid, or these water-soluble salts in the chemical conversion treatment solution is less than 3 g / L, the corrosion resistance of the magnesium alloy surface after chemical conversion treatment tends to be insufficient. In addition, even if the concentration exceeds 50 g / L, the corrosion resistance is not relatively improved. The chemical conversion treatment solution of the present invention contains permanganic acid, manganic acid, or water-soluble salts thereof, preferably alkaline earth metal salts including alkali salts such as sodium salt, potassium salt, lithium salt, and magnesium salt, and the like. May contain ammonium salts and the like. The concentration of permanganic acid, manganic acid, or these water-soluble salts in the chemical conversion treatment solution is 0.5 g / L or more, less than solubility, and preferably 1 to 65 g / L, as the potassium permanganate amount. If the concentration is less than 0.5 g / L, the corrosion resistance of the magnesium alloy surface after the chemical conversion treatment tends to be insufficient. In addition, high-humic acid, shovel acid, or these water-soluble salts may exist in the chemical treatment solution until the solubility, but even if these concentrations in the chemical treatment solution are higher than a certain level, their corrosion resistance is not relatively high. .--- l · ------ (Please read the precautions on the back before filling out this page) Order ------- Printed on paper standards for employees' cooperatives of the Intellectual Property Bureau of the Ministry of Economic Affairs, Chinese paper standards apply (CNS) A4 specification (210 X 297 mm) 4 311891 573061 Printed by the Consumer Cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs A7. 5. Description of the invention (5) Increase 'So the concentration below 65 g / L is sufficient. The chemical conversion treatment liquid of the present invention contains nitric acid or a water-soluble salt of nitric acid, preferably an alkaline earth metal salt such as an alkali metal salt such as sodium salt, potassium salt, lithium salt, and magnesium salt, and the other may also contain an ammonium salt or a salt. Salt and manganese salt. The concentration of the nitric acid or the water-soluble salt of nitric acid in the chemical conversion treatment solution is 3 to 60 g / L, preferably 5 to 50 g / L when converted to the amount of sodium nitrate. If the concentration of nitric acid or a water-soluble salt of nitric acid in the chemical conversion treatment solution is less than 3 g / L, the surface resistance of the magnesium alloy after the chemical conversion treatment tends to be insufficient. In addition, even if the concentration exceeds 60 g / L, the corrosion resistance tends to be insufficient. The chemical conversion treatment solution of the present invention contains acetic acid or a water-soluble salt of acetic acid 'preferably an alkali metal salt including a sodium salt, a potassium salt, a lithium salt, etc., and a metal test salt such as a magnesium salt'. Others may also include an ammonium salt, etc. . The concentration of the acetic acid or the water-soluble salt of acetic acid in the chemical conversion treatment solution is 0.5 to 50 g / L · 'as converted to the amount of sodium acetate, and preferably 1 to 50 g / L. When the concentration of acetic acid or the water-soluble salt of acetic acid in the chemical conversion treatment solution is less than 0.5 g / L, the corrosion resistance of the surface of the magnesium alloy after the chemical conversion treatment tends to be insufficient. In addition, even if the concentration exceeds 50 g / L, the corrosion resistance tends to be insufficient. The chemical conversion treatment solution of the present invention contains phosphoric acid or a water-soluble salt of phosphoric acid, and preferably contains sodium phosphate, sodium hydrogen phosphate, sodium dihydrogen phosphate, ammonium dihydrogen phosphate, monobasic acid, monobasic acid, and the like. The concentration of the water-soluble salt of dishic acid or linoleic acid in the chemical conversion treatment solution is converted into an amount of sodium phosphate of 0,05 to 8 g / L, and more preferably 0.1 to 6 g / L. When the concentration of the water-soluble salt of phosphoric acid or scaly acid in the chemical conversion treatment solution is less than 0.05 g / L, the corrosion resistance of the surface of the magnesium alloy after the chemical conversion treatment tends to be insufficient. In addition, when the concentration exceeds 8g / L, I will produce I ------------------- (Please read the precautions on the back before filling in this page} This paper size applies to China National Standard (CNS) A4 (210 X 297) (Mm) 5 311891 573061 A7 _ B7 V. Description of the invention (6) Dirt (smut) tends to deteriorate the adhesion of the paint. (Please read the note on the back? Matters before filling out this page) The high corrosion resistance of the invention In the method for producing a surface-treated magnesium alloy product, the above-mentioned chemical conversion treatment liquid for the surface of the magnesium alloy containing aluminum is 288 to 368K, preferably 288 to 363K, and the chemical conversion treatment is performed for 0 to 10 minutes. 0.5 to 10 minutes. Once the temperature of the chemical conversion treatment solution is less than 288K, the chemical conversion reaction becomes slower and the required processing time becomes longer. It is not practical. On the other hand, even if the chemical conversion temperature is higher than 3 68K, The corrosion resistance of the magnesium alloy surface has not been improved, so it is not practical in terms of cost. In the manufacturing method of the present invention, if the chemical conversion treatment time is less than 0.3 minutes, the corrosion resistance of the magnesium alloy surface after chemical conversion treatment is insufficient. The tendency. And even if the chemical treatment time exceeds 10 minutes, the corrosion resistance has not been relatively improved, resulting in an increase in production costs. High corrosion resistance surface-treated magnesium alloy products produced by the chemical treatment under the above conditions, followed by water washing and pure water After washing, it is dried. Generally, drying is performed at room temperature to 363K and 10 to 120 minutes. The chemical conversion treatment liquid of the present invention is used under the conditions described above when printed by the Consumer Cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs. The service life is very long. That is, the area of the surface of the aluminum-containing magnesium alloy that can be treated per unit area is very large. In addition, the surface of the highly corrosion-resistant magnesium alloy product obtained by the manufacturing method of the present invention has a good surface. Coating adhesion. The chemical conversion treatment liquid of the present invention can produce a magnesium alloy mouth with reduced hexavalent chromium concentration, longer life and higher corrosion resistance than conventional chromate treatment liquids. In addition, it is prepared by the present invention. The high-resistance # surface-treated town alloy G-scale scale is applicable to China National Standard (CNS) A4 specification (_2ig χ Norwegian public hair) ------ 6 311891 573061 A7 i. Description of the invention (9) Immerse in potassium pyrophosphate solution (35g / L, 3 33K) for 1 minute, and then wash with room temperature tap water for 30 seconds and clean water at room temperature for 3 seconds Second, then immersed in an aqueous caustic soda solution (50g / L, 333K) for 3 minutes, and then washed with room temperature tap water for 30 seconds and room temperature pure water for 30 seconds. Various test pieces treated as described above Then, it was immersed in the chemical conversion treatment solution used in Example 1 for 1 minute in sequence, and then washed with room temperature tap water for 30 seconds and room temperature pure water for 30 seconds, and finally dried at room temperature for 2 hours. Regarding chemical treatment test pieces, the total surface area becomes

The test pieces at 50, 75, 100, 125, 150, 175, and 200 dm2 / L were subjected to a corrosion resistance test in the same manner as in the above examples. The results are shown in Table 2. Comparative Example 4 Most test pieces made of magnesium alloy (AZ91) were subjected to ultrasonic cleaning in acetone at room temperature for 15 minutes, and then dried at room temperature for 5 minutes. Then immersed in potassium pyrophosphate aqueous solution (35g / L, 333K) for 1 minute, and then washed with room temperature tap water for 30 seconds and room temperature pure water for 30 seconds, and then immersed in caustic soda solution (50g / L , 333K) for 3 minutes, and then washed with room temperature tap water for 30 seconds and room temperature pure water for 30 seconds. The various test pieces treated as described above were sequentially immersed in the chemical conversion treatment liquid used in Comparative Example 2 for 丨 minutes, and then washed with room temperature tap water for 30 seconds and room temperature pure water for 30 seconds. Dry at room temperature for 2 hours. With respect to the chemical treatment test pieces, the test pieces when the total surface area was 25, 50, 75, 100, 125, 150, 175, and 200 dm2 / L, respectively, were subjected to a corrosion resistance test in the same manner as in the above examples. The results are shown in Table 2. The paper scale is applicable to the Chinese National Standard (CNS) A4 specification ⑵Q x 297 public hair -------- t pack —— (Please read the precautions on the back before filling this page) Order ---- Wisdom of the Ministry of Economic Affairs Printed by the Consumer Affairs Cooperative of the Property Bureau 311891 573061 A7 B7 V. Description of Invention (10)

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If Yibo® This paper size is in accordance with Chinese National Standard (CNS) A4 (210 x 297 mm) 10 311891 573061 A7 B7 V. Description of the invention (11) Table 2 Total surface area of chemical treatment test piece (dm2 / L) 1 25 50 75 100 125 150 175 200 Example 1 8 9.9 9.8 9.8 9.7 9.7 9.6 9.6 9.5 9.4 Comparative Example 4 9.8 9.3 9.2 9.0 8.8 8.6 8.5 8.5 8.5 dm2 / L = = square inch / liter g / L =: g / Liter | install ------- 1 order ---- (Please read the notes on the back before filling this page) ♦ The paper size printed by the Consumer Cooperatives of the Intellectual Property Bureau of the Ministry of Economic Affairs applies the Chinese national standard (CNS) A4 specifications (210 X 297 mm) 11 311891 Attachment 丄 ▲ Apricot Bundle 1, Date ^ Ί Case No.ονο ^ Α > (Above each block is noted by the Bureau) A4 C4 573061 Feces | Patent Specification Invention New name Chinese containing Shaozhi magnesium alloy chemical conversion treatment solution, high-resistance surface treatment town alloy products and its manufacturing method English name Country CHEMICAL SOLUTION FOR -TREATING MAGNESIUM ALLOY CONTAINING ALUMINUM, SURFACE-TREATED MAGNESIUM AIjLOY PRODUCT OF HIGH CORROSION RES ISTANCE, AND METHOD FOR MANUFACTURI.N ~ G- ΤΗΈ SAME --- 1. Suzuki Mitsuo 3. Matsushita Hideaki 5. Tohashi Makoto 2. Sugawara Shun 4. Inventor and creator of Momotake Masahiro 1. Japan to 5. The address is the same as the one printed by 1333-2, Shimizu, Kamio, Saitama, Japan. Mitsui Metals & Mining Co., Ltd. Printed by the Intellectual Property Bureau of the Ministry of Economic Affairs and Consumer Cooperatives. Name of the person Mitsui Metals Mining Co., Ltd. 1 Osaki, Shinagawa-ku, Tokyo, Japan, Japan No. 1 Miyamura Miramura Paper size applicable to Chinese National Standard (CNS) A4 (210 X 297 mm) 1 (correction page) 311891 573061 A7 B7 V. Description of the invention (7

Printed by the Consumer Cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs, the mouth can achieve good paint adhesion. The present invention will be specifically described based on examples and comparative examples as follows. Example 1 Most test pieces made of magnesium alloy (AZ91) were subjected to ultrasonic cleaning in acetone at room temperature for 15 minutes, and then dried at room temperature for 5 minutes. Then, it was immersed in a potassium pyrophosphate solution (35 g / L, 333K) for 1 minute, and then washed with room temperature tap water for 30 seconds and room temperature pure water for 3 () seconds. Then, it was immersed in a caustic soda solution (50 g / L, 333K) for 3 minutes, and then washed with room temperature tap water for 30 seconds and room temperature pure water for 30 seconds. The various test pieces treated as described above were then immersed in Table 1 as shown in Table 1 each containing chromium trioxide, potassium permanganate, sodium nitrate, sodium acetate, zinc oxide, and sodium phosphate. The liquid temperature (processing temperature) was converted into the processing time shown in Table 1 in the processing liquid, and then left in the air for 1 minute. Then, it was washed with tap water at room temperature for 30 seconds and pure water at room temperature for 3 () seconds, and finally dried at room temperature for 2 hours. The various test pieces subjected to the chemical conversion treatment and drying as described above were subjected to a corrosion test in accordance with JIS Z 237 1 and the state after 24 hours was evaluated by the R.N. method. The evaluation results are shown in Table 1. In addition, 'the surface of various test pieces after being chemically treated and dried as described above' was coated with an acrylic baking paint by a dipping coating method, left to stand for 10 minutes, and then dried by heating at 423K for 20 minutes, and then Jls κ5400 8.5.2 is the standard. The coating adhesion test is performed according to the checkerboard tape method (丨 mni interval). The results are shown in Table 1. Comparative Example 1 This paper size applies the Chinese National Standard (CNS) A4 specification (210 297 mm) 7 (correction page) 311891 (Please read the precautions on the back before filling this page) One SJ · ·; line · 573061

V. Description of the invention (8) The test piece made of magnesium alloy (AZ91) is the same as the above-mentioned example. 2 After the 'mixture removal &, pretreatment and washing, follow IIS Η 8651 (please read the precautions on the back first) (Fill in this page again) Three types, that is, chemical conversion treatment under the treatment conditions shown in Table 丨, post-washing, water washing, and water washing and drying in the same manner as in the above examples. The test pieces were also subjected to the same resistance test and coating adhesion test as in the above examples. The results are shown in Example 2. Example 2. Test pieces made of magnesium a gold (ΑZ91) were performed in the same manner as in the above examples. / The mixture is degreased, pre-treated, and washed with water, and then is processed according to JP-A No .: Reporting, that is, the chemical conversion treatment is performed under the processing conditions shown in Table 1. After that, it is washed and dried in the same manner as the above-mentioned embodiment. Related Comparative Examples The obtained test pieces were also subjected to the same corrosion resistance test and coating adhesion test. The results are shown in Table 1. fe- · fish example 3, ^ test pieces made of magnesium alloy (AZ91) and the above examples Same solvent degreasing Pretreatment and washing. After that, follow the Dow22 method (", 92 Manual for the Printing of Magnesium by the Consumer Cooperatives of the Intellectual Property Bureau of the Ministry of Economic Affairs" (1992) Japan Magnesium Association, the method described on page 127), that is, as shown in Table 1. The chemical conversion treatment was performed under the treatment conditions, and water washing and drying were performed in the same manner as in the above-mentioned Example. The test pieces prepared in Comparative Example 3 were also subjected to the same corrosion resistance test and coating adhesion test. The results are shown in Table 1. 16. Most test pieces made of town alloys (AZ91) are washed at room temperature for 15 minutes, and then dried at room temperature for 5 minutes. Then, the Chinese national standard (CNS) A4 specification ⑵G > < 297 public love) ----- 8 (correction page) 311891

Claims (1)

18 18 573061 Printed by the Staff Welfare Committee of the Central Standards Bureau of the Ministry of Economic Affairs 3. Amendment < I 脒 Supplement No. 89120986 Patent Application Application Amendment of the Patent Scope 1. A chain-containing magnesium alloy chemical conversion treatment solution for aluminum-containing A chemical conversion treatment solution for magnesium alloy in an amount ranging from 2 to 12% by weight, which is characterized by containing chromic acid, dichromic acid, or these water-soluble salts, and its concentration is converted into chromium trioxide (CrO3) in an amount of 3 to 50 g. / L; the concentration of permanganic acid, manganic acid, or these water-soluble salts is converted into potassium permanganate (km〇4) in an amount of 0.5 g / L or more, or less than the degree of valley; nitric acid or acid The concentration of water-soluble salts is 3 to 60 g / L when converted to sodium oleate; the concentration of water-soluble salts of acetic acid or acetic acid is 0.5 to 50 g / L when it is converted to sodium acetate (CH3COONa); the water solubility of phosphoric acid or acid The salt is converted to a concentration of sodium phosphate (Na3po4) of 0.05 to 8 g / L. 2. According to the scope of the patent application, the chemical treatment solution for aluminum-containing magnesium alloys, where the concentration of chromic acid, dichromic acid, or these water-soluble salts is converted into chromium dioxide in an amount of 5 to 50 g / L; the concentration of permanganic acid, manganic acid or the special water-soluble salt is converted into potassium permanganate amount of 1 to 65g / L; the concentration of water-soluble salt of lithic acid or nitric acid is converted to sodium nitrate amount of 5 to 50g / L; the concentration of water-soluble salt of acetic acid or acetic acid is converted into the amount of sodium acetate i to 50g / L; the concentration of water-soluble salt of phosphoric acid or phosphoric acid is converted to the amount of sodium phosphate 0.1 to 6g / L. A method for manufacturing a high-resistance surface-treated magnesium alloy product, which is a chemical conversion treatment solution for magnesium alloys having an aluminum content in the range of 2 to 12% by weight, and is characterized in that the surface temperature of the aluminum-containing magnesium alloy is 288. Ta iii to 7cks to 368κ) (210 x 297 ^ t) 573061 Printed clothes H3 of the Employees Welfare Committee of the Central Standards Bureau of the Ministry of Economic Affairs. Application of the patented chemical treatment solution for alloys with inscriptions No. 丨 or No. 2. A chemical conversion treatment is performed for 0.3 to 10 minutes. As stated in the patent | & manufacturing method of item 3, in which the surface of magnesium-containing aluminum alloys containing aluminum is used for chemical treatment of ingot-containing gold with a liquid temperature of 288 to 363K and the inscription ^ or 2 Alas, those who undergo the chemical conversion treatment for 0.5 to 10 minutes. \ A high-resistance surface-treated ㈣alloy product 'is characterized by being obtained according to the manufacturing method of the patent application scope item 3 or 4. This paper size applies to China National Standard (CNS) Α4 (210 x 297 mm)