JP2008214701A - Method for forming chemical conversion-treated film of magnesium alloy - Google Patents
Method for forming chemical conversion-treated film of magnesium alloy Download PDFInfo
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本発明はマグネシウム合金の化成処理被膜の形成方法に関し、より詳しくは、マグネシウム合金の表面をリン酸イオン含有水溶液中で化成処理する化成処理被膜の形成方法に関する。 The present invention relates to a method for forming a chemical conversion coating on a magnesium alloy, and more particularly to a method for forming a chemical conversion coating on the surface of a magnesium alloy in a phosphate ion-containing aqueous solution.
エネルギー問題、環境問題、省資源対策、リサイクル問題等の観点から、軽量であり、比強度に優れ、且つリサイクル性にも優れているマグネシウム合金が注目を浴び、家電製品あるいはＩＴ関連機器、更には自動車部品等へと応用が広まってきている。 From the viewpoints of energy problems, environmental problems, resource saving measures, recycling problems, etc., magnesium alloys that are lightweight, excellent in specific strength, and excellent in recyclability have attracted attention, and are used for home appliances or IT-related equipment, Application to automobile parts is spreading.
しかしながら、マグネシウム合金はアルミニウム、鉄等に比べて耐食性に劣るという問題点がある。それで、マグネシウム合金の耐食性を改善するために様々な表面処理法や塗装法が提案されている。 However, magnesium alloys have a problem that they are inferior in corrosion resistance compared to aluminum, iron and the like. Therefore, various surface treatment methods and coating methods have been proposed to improve the corrosion resistance of magnesium alloys.
例えば、マグネシウム合金の化成処理方法としてノンクロム系化成処理方法がある（例えば、特許文献１、特許文献２参照）。また、エッチング処理した後、有機リン化合物を含有するアルカリ性水溶液で表面処理する方法（例えば、特許文献３参照）、オルトリン酸と、Ｚｎ、ＭｎおよびＣａから選ばれる少なくとも１種の金属イオンとを含有する酸性水溶液で表面処理する方法（例えば、特許文献４参照）、カルシウムイオン、マンガンイオン及びリン酸イオンを含有する溶液で化成処理する方法（例えば、特許文献５参照）がある。更に、エッチング処理なしで又はエッチング処理した後、リン酸イオン及び過マンガン酸イオンを含有する処理液で化成処理する方法（例えば、特許文献６参照）、リン酸と、カルシウム化合物と、チタン化合物、ジルコニウム化合物、ストロンチウム化合物から選ばれる少なくとも１種の金属化合物を含有する処理液で化成処理する方法（例えば、特許文献７参照）、リン酸及び／又はリン酸塩化合物、並びに過マンガン酸塩化合物を含有する処理液で化成処理する方法（例えば、特許文献８参照）がある。 For example, as a chemical conversion treatment method for a magnesium alloy, there is a non-chromium chemical conversion treatment method (see, for example, Patent Document 1 and Patent Document 2). In addition, after etching treatment, a surface treatment with an alkaline aqueous solution containing an organophosphorus compound (see, for example, Patent Document 3), orthophosphoric acid, and at least one metal ion selected from Zn, Mn and Ca are contained. There are a method of surface treatment with an acidic aqueous solution (for example, see Patent Document 4) and a method of chemical conversion treatment with a solution containing calcium ions, manganese ions and phosphate ions (for example, see Patent Document 5). Further, after etching treatment or after etching treatment, a chemical conversion treatment with a treatment liquid containing phosphate ions and permanganate ions (for example, see Patent Document 6), phosphoric acid, calcium compound, titanium compound, A method of chemical conversion treatment with a treatment liquid containing at least one metal compound selected from a zirconium compound and a strontium compound (see, for example, Patent Document 7), phosphoric acid and / or phosphate compound, and permanganate compound There exists a method (for example, refer patent document 8) of performing a chemical conversion treatment with the containing processing liquid.
一般に、ＡＺ３１Ｂ等に代表される押し出し材や圧延材に用いられるアルミニウム含有マグネシウム合金は、ＡＺ９１Ｄ等に代表される鋳造品のアルミニウム含有マグネシウム合金に比較してアルミニウム含有量が少ないため、酸等による溶解性がかなり大きい。従って、アルミニウム含有マグネシウム合金について酸化膜の除去や、表面に潜り込んだ離型剤や潤滑剤の除去を目的として必ず行われるエッチング工程において、ＡＺ９１材等で行われるエッチングと同じ処理をＡＺ３１材等で行うとエッチング過剰となり、表面が過剰に荒れた状態となる。このように過剰に荒れた状態の表面に化成被膜形成処理を実施すると、化成被膜が過剰に析出し、被膜質量が過大となるばかりでなく、過剰析出成分が微粉となって表面に残留した状態となる。また、そのような化成被膜表面に塗装を行った場合には、塗膜種によっては密着性、特に耐水密着性が著しく低下する。 Generally, aluminum-containing magnesium alloys used for extruded materials and rolled materials typified by AZ31B have a lower aluminum content than cast magnesium-containing magnesium alloys typified by AZ91D. Sex is quite big. Therefore, in the etching process that is always performed for the purpose of removing the oxide film and removing the release agent and lubricant that have entered the surface of the aluminum-containing magnesium alloy, the same process as that performed with the AZ91 material is performed with the AZ31 material. If it is performed, the etching becomes excessive and the surface becomes excessively rough. When the chemical conversion film forming treatment is performed on the surface in such an excessively rough state, the chemical conversion film is excessively deposited, and not only the film mass becomes excessive, but also the excessively deposited component remains as a fine powder on the surface. It becomes. Moreover, when coating is performed on the surface of such a chemical conversion coating, the adhesion, particularly the water-resistant adhesion, is significantly lowered depending on the type of coating.
本発明は、エッチング処理を行う必要なしで、マグネシウム合金、特に少量のアルミニウムを含有するマグネシウム合金の表面に、耐食性、塗膜密着性に優れた化成処理被膜を形成し得る、マグネシウム合金の化成処理被膜の形成方法を提供することを目的としている。 The present invention provides a chemical conversion treatment of a magnesium alloy that can form a chemical conversion treatment film having excellent corrosion resistance and coating adhesion on the surface of a magnesium alloy, particularly a magnesium alloy containing a small amount of aluminum, without the need for performing an etching treatment. It aims at providing the formation method of a film.
本発明者等は上記の目的を達成するために鋭意検討した結果、エッチング処理していないマグネシウム合金の表面を、リン酸又は水溶性リン酸塩をリン酸イオン濃度換算で１〜１０質量％含有する水溶液で処理することにより上記の目的が達成されることを見出し、本発明を完成した。 As a result of intensive studies to achieve the above object, the inventors of the present invention contain 1-10% by mass of phosphoric acid or water-soluble phosphate in terms of phosphate ion concentration on the surface of the magnesium alloy that has not been etched. The present invention was completed by finding that the above-mentioned object was achieved by treating with an aqueous solution.
即ち、本発明のマグネシウム合金の化成処理被膜の形成方法は、リン酸又は水溶性リン酸塩をリン酸イオン濃度換算で１〜１０質量％含有する水溶液をマグネシウム合金の表面に接触させて表面処理することを特徴とする。 That is, in the method for forming a chemical conversion treatment film of a magnesium alloy according to the present invention, an aqueous solution containing phosphoric acid or a water-soluble phosphate in an amount of 1 to 10% by mass in terms of phosphate ion concentration is brought into contact with the surface of the magnesium alloy. It is characterized by doing.
また、本発明のマグネシウム合金の化成処理被膜の形成方法は、マグネシウム合金の表面を脱脂処理した後、リン酸又は水溶性リン酸塩をリン酸イオン濃度換算で１〜１０質量％含有する水溶液を該マグネシウム合金の表面に接触させて表面処理することを特徴とする。 Moreover, the formation method of the chemical conversion treatment film of the magnesium alloy of this invention is the method of degreasing the surface of a magnesium alloy, Then, the aqueous solution which contains phosphoric acid or water-soluble phosphate 1-10 mass% in conversion of a phosphate ion density | concentration The surface treatment is performed by contacting the surface of the magnesium alloy.
本発明のマグネシウム合金の化成処理被膜の形成方法により、エッチング処理を行う必要なしで、マグネシウム合金の表面に耐食性、塗膜密着性に優れた化成処理被膜を形成することができる。 According to the method for forming a chemical conversion coating of a magnesium alloy of the present invention, a chemical conversion coating excellent in corrosion resistance and coating film adhesion can be formed on the surface of the magnesium alloy without the need for etching treatment.
以下に、本発明の化成処理被膜の形成方法を具体的に説明する。本発明においては、表面に化成処理被膜を形成するマグネシウム合金の種類は特には限定されず、例えば、ＡＺ２１、ＡＺ３１Ｂ、ＡＺ３１Ｃ、ＡＺ６１Ａ、ＡＺ８０Ａ等の展伸用マグネシウム合金及びＡＺ６３Ａ、ＡＺ８１Ａ、ＡＺ９１Ｃ、ＡＺ９２Ａ、ＡＭ６０Ａ、ＡＭ１００Ａ等の鋳造用マグネシウム合金を挙げることができる。しかし、本発明のマグネシウム合金の化成処理被膜の形成方法は少量のアルミニウムを含有するマグネシウム合金、特に、アルミニウム含有量が１〜５質量％のマグネシウム合金、具体的にはＡＺ２１、ＡＺ３１Ｂ、ＡＺ３１Ｃ等の表面に耐食性、塗膜密着性に優れた化成処理被膜を形成するのに特に適している。 Below, the formation method of the chemical conversion treatment film of this invention is demonstrated concretely. In the present invention, the type of the magnesium alloy that forms the chemical conversion coating on the surface is not particularly limited. , AM60A, AM100A, and other magnesium alloys for casting. However, the method for forming a chemical conversion treatment film of a magnesium alloy according to the present invention is a magnesium alloy containing a small amount of aluminum, particularly a magnesium alloy having an aluminum content of 1 to 5% by mass, specifically AZ21, AZ31B, AZ31C, etc. It is particularly suitable for forming a chemical conversion film having excellent corrosion resistance and coating film adhesion on the surface.
また、本発明において表面に化成処理被膜を形成するマグネシウム合金部材の成形方法も特には限定されず、押し出し加工、圧延加工、引き抜き加工、ダイカスト法、チクソモールド法、プレス成形法、鍛造法、鋳造法等を挙げることができる。 In addition, the method for forming the magnesium alloy member for forming the chemical conversion coating on the surface in the present invention is not particularly limited. Extrusion processing, rolling processing, drawing processing, die casting method, thixo molding method, press molding method, forging method, casting The law etc. can be mentioned.
本発明においては、マグネシウム合金表面のエッチング処理は不要であるが、化成処理の前に脱脂処理することが好ましい。脱脂処理はマグネシウム合金の表面に脱脂液を接触させることにより行われる。マグネシウム合金の表面に脱脂液を接触させる方法としては、従来から公知の浸漬法、スプレー法等が挙げられ、本発明においてはいずれの方法も適用することができる。 In the present invention, the etching treatment of the magnesium alloy surface is not necessary, but it is preferable to perform a degreasing treatment before the chemical conversion treatment. The degreasing treatment is performed by bringing a degreasing solution into contact with the surface of the magnesium alloy. Examples of methods for bringing the degreasing solution into contact with the surface of the magnesium alloy include conventionally known dipping methods and spray methods, and any method can be applied in the present invention.
脱脂液としては、有機汚れを除去できるものであれば組成は特には限定されないが、界面活性剤を含むアルカリ性水溶液を用いるのが好ましい。かかる脱脂液のアルカリビルダーとしては、アルカリ金属の水酸化物、リン酸塩、ケイ酸塩、炭酸塩等が適用できる。また、界面活性剤としてはノニオン系、カチオン系、アニオン系のいずれも適用できる。さらに、脱脂効率を上げるためにキレート剤を配合してもよい。 The composition of the degreasing liquid is not particularly limited as long as it can remove organic stains, but an alkaline aqueous solution containing a surfactant is preferably used. As the alkali builder for such a degreasing solution, alkali metal hydroxides, phosphates, silicates, carbonates and the like can be applied. As the surfactant, any of nonionic, cationic and anionic can be applied. Furthermore, a chelating agent may be added to increase the degreasing efficiency.
脱脂液をマグネシウム合金の表面に接触させる際の温度と時間は特には限定されないが、マグネシウム合金表面の汚染の程度によって３５〜７０℃、３０秒〜１０分の範囲内で接触させるのが好ましい。また、脱脂液の濃度は、マグネシウム合金表面の汚染の程度、脱脂液成分等により適宜設定される。 The temperature and time when the degreasing solution is brought into contact with the surface of the magnesium alloy are not particularly limited, but it is preferable that the degreasing solution is brought into contact within a range of 35 to 70 ° C. for 30 seconds to 10 minutes depending on the degree of contamination of the magnesium alloy surface. Further, the concentration of the degreasing liquid is appropriately set depending on the degree of contamination of the magnesium alloy surface, the degreasing liquid component, and the like.
本発明で用いるリン酸又は水溶性リン酸塩として、オルトリン酸、ホスホン酸、ピロリン酸、トリポリリン酸及びそれらのアルカリ金属塩を挙げることができる。リン酸又は水溶性リン酸塩をリン酸イオン濃度換算で１〜１０質量％含有する水溶液とは、リン酸又は水溶性リン酸塩中のＰＯ4 ---の重量を全溶液の量で割って１００倍した値であり、例えば、リン酸を用いる場合には１．０３〜１０．３質量％となる量で用い、リン酸カリウムを用いる場合には２．２３〜２２．３質量％となる量で用いる。 Examples of phosphoric acid or water-soluble phosphate used in the present invention include orthophosphoric acid, phosphonic acid, pyrophosphoric acid, tripolyphosphoric acid, and alkali metal salts thereof. An aqueous solution containing 1 to 10% by mass of phosphoric acid or water-soluble phosphate in terms of phosphate ion concentration is obtained by dividing the weight of PO 4 --- in phosphoric acid or water-soluble phosphate by the amount of the total solution. For example, when phosphoric acid is used, it is used in an amount of 1.03 to 10.3 mass%, and when potassium phosphate is used, 2.23 to 22.3 mass%. Is used in an amount of
本発明において、マグネシウム合金の表面に化成処理液を接触させる方法としては、従来から公知の浸漬法、スプレー法等が挙げられ、本発明においてはいずれの方法も適用することができる。 In the present invention, examples of the method for bringing the chemical conversion treatment liquid into contact with the surface of the magnesium alloy include conventionally known dipping methods, spraying methods, and the like, and any method can be applied in the present invention.
化成処理液をマグネシウム合金の表面に接触させる際の温度と時間はリン酸又は水溶性リン酸塩の種類、水溶液の濃度、ｐＨ、被処理物たるマグネシウム合金の種類等により異なる。一般論としては、化成処理液の濃度が高ければ、比較的低い温度で且つ比較的短時間で所望程度の化成処理が完了し、化成処理液の温度が高ければ、比較的低い化成処理液濃度で且つ比較的短時間で所望程度の化成処理が完了し、また、処理時間が長ければ、比較的低い化成処理液濃度で且つ比較的低い温度で化成処理が完了する。例えば、常温〜７０℃の温度で１０秒間〜１０分間接触させる。 The temperature and time at which the chemical conversion solution is brought into contact with the surface of the magnesium alloy vary depending on the type of phosphoric acid or water-soluble phosphate, the concentration of aqueous solution, pH, the type of magnesium alloy to be processed, and the like. Generally speaking, if the concentration of the chemical conversion treatment liquid is high, a desired degree of chemical conversion treatment is completed at a relatively low temperature in a relatively short time. If the temperature of the chemical conversion treatment liquid is high, the concentration of the chemical conversion treatment liquid is relatively low. In addition, a desired degree of chemical conversion treatment is completed in a relatively short time, and if the treatment time is long, the chemical conversion treatment is completed at a relatively low chemical conversion solution concentration and at a relatively low temperature. For example, the contact is performed at a temperature of room temperature to 70 ° C. for 10 seconds to 10 minutes.
本発明においては、各工程の間に水洗工程を設けることが望ましい。該水洗工程による水洗は、水に被処理物たるマグネシウム合金を接触させることにより行われる。水洗の程度（接触時間、水の純度・温度、水洗の段数、希釈倍率等）は、特には制限がなく、各処理液の濃度、次工程に混入した際の影響度等を考慮の上、適宜設定すればよい。 In the present invention, it is desirable to provide a water washing step between each step. The water washing in the water washing step is performed by bringing a magnesium alloy, which is an object to be treated, into contact with water. The degree of water washing (contact time, water purity / temperature, number of stages of water washing, dilution rate, etc.) is not particularly limited, taking into account the concentration of each processing solution, the degree of influence when mixed in the next process, etc. What is necessary is just to set suitably.
本発明による化成処理被膜の形成の後、表面に残存する水分を蒸散させるべく、乾燥させることが望ましい。もちろん水系の塗料により塗装を施す場合には、表面に水分が残存していても塗装そのものは可能であるため乾燥は必須ではない。しかし、水分が塗料に混入し、塗料の濃度に影響を与える場合があるため、この場合にも乾燥工程を設けることが望ましい。乾燥は、特に制限はなく、例えば自然乾燥でもよいが、熱風ヒーターや赤外線ヒーター等によるオーブン乾燥とすることが望ましい。 After the formation of the chemical conversion coating according to the present invention, it is desirable to dry in order to evaporate water remaining on the surface. Of course, when applying with a water-based paint, drying is not essential since the coating itself is possible even if moisture remains on the surface. However, since moisture may enter the paint and affect the concentration of the paint, it is desirable to provide a drying step in this case as well. The drying is not particularly limited and may be natural drying, for example, but is preferably oven drying with a hot air heater or an infrared heater.
本発明の化成処理被膜の形成方法によって得られるマグネシウム合金部材は、そのままでも優れた耐食性を有するが、更なる耐食性の向上を企図して、あるいは、マグネシウム合金部材の美観性の向上を企図して、必要に応じて塗装が為される。塗装に供される塗料は、特に制限されず、水系、溶剤系のいずれでもよい。また、塗装方法についても特に制限されず、スプレー塗装、浸漬塗装、電着塗装等従来公知のいずれの塗装方法であっても適用できる。 Although the magnesium alloy member obtained by the method for forming a chemical conversion coating of the present invention has excellent corrosion resistance as it is, it is intended to further improve the corrosion resistance or to improve the aesthetics of the magnesium alloy member. If necessary, painting is done. The paint used for coating is not particularly limited, and may be either water-based or solvent-based. The coating method is not particularly limited, and any conventionally known coating method such as spray coating, dip coating, or electrodeposition coating can be applied.
以下に、実施例及び比較例に基づいて本発明を更に具体的に説明する。 Hereinafter, the present invention will be described more specifically based on examples and comparative examples.
実施例１〜２及び比較例１
処理対象部材として、ＡＳＴＭ ＡＺ３１Ｂのアルミニウム含有マグネシウム合金押し出し部材から作製した５ｍｍ×７０ｍｍ×１５０ｍｍの部材を用いた。脱脂処理においては、脱脂剤としてキシレンを用い、部材表面の油分を刷毛で洗い落とし、風乾させた。
Examples 1-2 and Comparative Example 1
A 5 mm × 70 mm × 150 mm member produced from an aluminum-containing magnesium alloy extruded member of ASTM AZ31B was used as the processing target member. In the degreasing treatment, xylene was used as a degreasing agent, and the oil on the surface of the member was washed away with a brush and allowed to air dry.
実施例１〜２においては、化成処理液としてリン酸濃度５質量％のリン酸水溶液（化成処理液Ａ）又はリン酸濃度１質量％のリン酸水溶液（化成処理液Ｂ）を用い、それらの液温を２３℃に保持し、それらの中に上記の部材を１分間浸漬して化成処理を実施した。比較例１においては化成処理は実施しなかった。実施例１〜２及び比較例１についての化成処理の条件は第１表に示す通りであった。 In Examples 1-2, phosphoric acid aqueous solution (chemical conversion liquid A) having a phosphoric acid concentration of 5 mass% or phosphoric acid aqueous solution (chemical conversion liquid B) having a phosphoric acid concentration of 1 mass% was used as the chemical conversion liquid. The liquid temperature was kept at 23 ° C., and the above-mentioned members were immersed in them for 1 minute to carry out a chemical conversion treatment. In Comparative Example 1, no chemical conversion treatment was performed. The conditions of chemical conversion treatment for Examples 1-2 and Comparative Example 1 were as shown in Table 1.
塗装例
実施例１〜２及び比較例１で得た各々の化成処理被膜付き部材の表面に、エアースプレー法によりエポキシ樹脂系塗料（大日本塗料株式会社製ＭＧ−ＰＲ−Ｅ）を膜厚２０μｍとなるように塗布し、２０分間静置した後、更にエアースプレー法によりウェットオンウェットでアクリル−メラミン樹脂系塗料（大日本塗料株式会社製ＭＧ−トップ）を膜厚２０μｍとなるように塗布し、これを１８０℃で２０分間焼付処理した。
Coating Example An epoxy resin paint (MG-PR-E, manufactured by Dainippon Paint Co., Ltd.) is formed on the surface of each member with a chemical conversion coating obtained in Examples 1 and 2 and Comparative Example 1 by a film thickness of 20 μm. After being allowed to stand for 20 minutes, an acrylic-melamine resin-based paint (MG-Top, manufactured by Dainippon Paint Co., Ltd.) is applied to a film thickness of 20 μm by wet-on-wet by an air spray method. This was baked at 180 ° C. for 20 minutes.
塗装例で得た各々の塗膜について、下記の塗膜性能を下記の方法で評価した。それらの結果は第２表に示す通りであった。 About each coating film obtained by the coating example, the following coating film performance was evaluated by the following method. The results were as shown in Table 2.
（イ）塗膜外観
塗膜外観を下記の基準で目視により評価した。
○：良好である。
△：はじきがわずかに認められる。
×：はじきが甚だ多い。
(A) Coating film appearance The coating film appearance was visually evaluated according to the following criteria.
○: Good.
Δ: Slight repellency is observed.
X: There are many repellents.
（ロ）塗膜密着性
ＪＩＳ Ｋ ５４００ ８．５．２の碁盤目テープ法に準拠して、塗膜にナイフで碁盤目模様を描き、１００個の部分に区分した後、粘着テープにより塗膜の剥離を試みた。塗膜の剥離の有無及びその程度を下記の基準で目視により評価した。
○：全く異常が認められない。
△：塗膜の剥離が２０％以下。
×：塗膜の剥離が２０％を越える。
(B) Coating film adhesion In accordance with the cross-cut tape method of JIS K 5400 8.5.2, a cross-cut pattern is drawn on the coating film with a knife and divided into 100 parts. I tried to peel off. The presence or absence and degree of peeling of the coating film were visually evaluated according to the following criteria.
○: No abnormality is observed at all.
(Triangle | delta): Peeling of a coating film is 20% or less.
*: Peeling of a coating film exceeds 20%.
（ハ）耐塩水噴霧性
塗膜表面にナイフでクロスカットを入れ、ＪＩＳ Ｚ ２３７１に準拠して塩水噴霧試験（ＳＳＴ）を５００時間行い、クロスカット部分の塗膜の剥離幅を測定し、下記の基準により評価した。
○：剥離幅が±２．５ｍｍ以下。
△：剥離幅が±５ｍｍ以下。
×：剥離幅が±５ｍｍを越える。
(C) Salt spray resistance A cross-cut is made on the surface of the coating film with a knife, a salt spray test (SST) is performed for 500 hours in accordance with JIS Z 2371, and the peeling width of the coating film at the cross-cut portion is measured. It was evaluated according to the criteria.
○: Peel width is ± 2.5 mm or less.
Δ: Peel width is ± 5 mm or less.
X: The peeling width exceeds ± 5 mm.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104451631A (en) * | 2014-12-04 | 2015-03-25 | 常州大学 | Simple coating method for magnesium and magnesium alloy surfaces |
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| CN104451631A (en) * | 2014-12-04 | 2015-03-25 | 常州大学 | Simple coating method for magnesium and magnesium alloy surfaces |
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