JP6667191B2 - Aluminum surface treatment method - Google Patents
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- JP6667191B2 JP6667191B2 JP2016068725A JP2016068725A JP6667191B2 JP 6667191 B2 JP6667191 B2 JP 6667191B2 JP 2016068725 A JP2016068725 A JP 2016068725A JP 2016068725 A JP2016068725 A JP 2016068725A JP 6667191 B2 JP6667191 B2 JP 6667191B2
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims description 12
- 229910052782 aluminium Inorganic materials 0.000 title claims description 12
- 238000000034 method Methods 0.000 title claims description 12
- 238000004381 surface treatment Methods 0.000 title claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 22
- 238000007789 sealing Methods 0.000 claims description 19
- 239000010407 anodic oxide Substances 0.000 claims description 18
- 238000011282 treatment Methods 0.000 claims description 12
- 239000000377 silicon dioxide Substances 0.000 claims description 9
- 239000007864 aqueous solution Substances 0.000 claims description 7
- 150000002815 nickel Chemical class 0.000 claims description 6
- 238000004040 coloring Methods 0.000 claims description 3
- 239000010419 fine particle Substances 0.000 claims description 3
- 230000015572 biosynthetic process Effects 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 239000002131 composite material Substances 0.000 claims 1
- 238000004043 dyeing Methods 0.000 claims 1
- 239000010408 film Substances 0.000 description 31
- 239000011247 coating layer Substances 0.000 description 15
- 238000000576 coating method Methods 0.000 description 13
- 239000011248 coating agent Substances 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- 238000005260 corrosion Methods 0.000 description 8
- 230000007797 corrosion Effects 0.000 description 8
- 238000012360 testing method Methods 0.000 description 7
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 6
- 125000000217 alkyl group Chemical group 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 230000014759 maintenance of location Effects 0.000 description 4
- 238000003980 solgel method Methods 0.000 description 4
- -1 3-glycidoxypropyl Chemical group 0.000 description 3
- 239000008151 electrolyte solution Substances 0.000 description 3
- 230000002087 whitening effect Effects 0.000 description 3
- 229910000838 Al alloy Inorganic materials 0.000 description 2
- 239000006087 Silane Coupling Agent Substances 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
- 125000004432 carbon atom Chemical group C* 0.000 description 2
- 239000008119 colloidal silica Substances 0.000 description 2
- 238000006482 condensation reaction Methods 0.000 description 2
- 238000010410 dusting Methods 0.000 description 2
- 238000004070 electrodeposition Methods 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- DBJLJFTWODWSOF-UHFFFAOYSA-L nickel(ii) fluoride Chemical compound F[Ni]F DBJLJFTWODWSOF-UHFFFAOYSA-L 0.000 description 2
- 235000006408 oxalic acid Nutrition 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 229920000298 Cellophane Polymers 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 229910001593 boehmite Inorganic materials 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 description 1
- 125000001972 isopentyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])C([H])([H])* 0.000 description 1
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 125000000740 n-pentyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 125000004123 n-propyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 125000001971 neopentyl group Chemical group [H]C([*])([H])C(C([H])([H])[H])(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 125000003538 pentan-3-yl group Chemical group [H]C([H])([H])C([H])([H])C([H])(*)C([H])([H])C([H])([H])[H] 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- WGYKZJWCGVVSQN-UHFFFAOYSA-N propylamine Chemical group CCCN WGYKZJWCGVVSQN-UHFFFAOYSA-N 0.000 description 1
- 230000001012 protector Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 125000001424 substituent group Chemical group 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
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- Other Surface Treatments For Metallic Materials (AREA)
Description
本発明は、アルミニウムの表面に耐食性及び耐白化性に優れた皮膜を形成する表面処理方法に関する。 The present invention relates to a surface treatment method for forming a film having excellent corrosion resistance and whitening resistance on the surface of aluminum.
アルミニウム又はアルミニウム合金(以下、単にアルミニウムと称する)の表面に耐食性向上を目的に陽極酸化皮膜を形成することが一般的に行われている。
陽極酸化皮膜には、バリアー型皮膜とポーラス型皮膜があるが、バリアー型皮膜は厚膜化が難しく、高耐食性が要求される分野では陽極酸化中に内径数十nmの微少の無数の孔が形成されるポーラス型皮膜が採用されている。
このようなポーラス型の陽極酸化皮膜の場合には陽極酸化のままでは耐食性が劣るために各種封孔処理が施されている。
しかし、封孔処理だけでは耐食性が不充分な分野、例えば建材の分野では陽極酸化皮膜を形成後に電着塗装を施している。
ところが自動車等の外装部品の分野では電着塗膜が洗車等によりキズが付きやすく、しかも塗膜の密着性を確保するために下地の陽極酸化皮膜は完全封孔されていなく、塗膜が剥がれた部分は表面が自化しやすい問題があった。
そこで本出願人は、耐アルカリ性の向上に大きな効果を有し、キズが付きにくく耐剥離性に優れた、シロキサンガラス成分からなるコーティング層を有するアルミニウム部材を提案している(特許文献1)。
本技術は充分に実用的であるものの、下地の陽極酸化皮膜が湯洗処理又は半封孔処理されたものであって完全封孔皮膜でないため、仮に強い力でコーティング層に剥がれが生じた場合に、その部分が白化する恐れがある課題が内在していた。
It is common practice to form an anodic oxide film on the surface of aluminum or an aluminum alloy (hereinafter simply referred to as aluminum) for the purpose of improving corrosion resistance.
There are two types of anodic oxide coatings: barrier coatings and porous coatings, but barrier coatings are difficult to increase in thickness, and in fields where high corrosion resistance is required, microscopic countless holes with internal diameters of several tens of nanometers are formed during anodic oxidation. The porous film formed is adopted.
In the case of such a porous type anodic oxide film, various sealing treatments are performed because the corrosion resistance is inferior if anodic oxidation is performed.
However, in a field where corrosion resistance is insufficient only by sealing treatment, for example, in the field of building materials, an electrodeposition coating is applied after forming an anodic oxide film.
However, in the field of exterior parts such as automobiles, the electrodeposition coating film is easily scratched by car washing, etc. In addition, the underlying anodic oxide film is not completely sealed to secure the adhesion of the coating, and the coating peels off There was a problem that the surface was easily self-sustaining.
Therefore, the present applicant has proposed an aluminum member having a coating layer made of a siloxane glass component, which has a great effect on improving alkali resistance, is less likely to be scratched, and has excellent peeling resistance (Patent Document 1).
Although this technology is sufficiently practical, if the underlying anodic oxide film has been washed or semi-sealed and is not a completely sealed film, the coating layer may be peeled off by strong force. However, there is an inherent problem that the part may be whitened.
特許文献2は、陽極酸化皮膜の微細孔中にSiO2を充填させているがコーティング層ではない。
また、完全封孔ではない点で同様の課題を有する。
特許文献3は塗膜の下地としてシランカップリング剤を塗布しているが、塗膜がキズ付きやすく、またシランカップリング剤のみでは耐食性が悪い。
In Patent Document 2, SiO 2 is filled in the micropores of the anodic oxide film, but it is not a coating layer.
In addition, it has a similar problem in that it is not completely sealed.
In Patent Document 3, a silane coupling agent is applied as a base of a coating film. However, the coating film is easily scratched, and the silane coupling agent alone has poor corrosion resistance.
本発明は、充分に封孔処理した陽極酸化皮膜であっても密着性に優れ、高い耐食性と耐白化性を有するアルミニウムの表面処理方法の提供を目的とする。 An object of the present invention is to provide a method for surface treatment of aluminum having excellent adhesion and high corrosion resistance and whitening resistance even with a sufficiently sealed anodic oxide film.
本発明に係るアルミニウムの表面処理方法は、アルミニウムの表面に陽極酸化皮膜を形成するステップと、次に低温のニッケル塩水溶液に浸漬する低温封孔処理ステップと、次に100〜160℃の水蒸気による蒸気封孔処理ステップと、次にゾル−ゲル法によるシリカ質皮膜を形成ステップとを、有することを特徴とする。 The surface treatment method for aluminum according to the present invention includes a step of forming an anodic oxide film on the surface of aluminum, a low-temperature sealing step of immersing the aluminum in a low-temperature nickel salt aqueous solution, and then using steam at 100 to 160 ° C. The method is characterized by having a vapor sealing step and then a step of forming a siliceous film by a sol-gel method.
本発明は、ニッケル塩水溶液による低温封孔処理と100〜160℃の水蒸気による蒸気封孔処理により、陽極酸化皮膜を充分に封孔処理した上に、ゾル−ゲル法によりシリカ質の皮膜からなるコーティング層を形成した点に特徴がある。 The present invention comprises a low-temperature sealing treatment with an aqueous solution of nickel salt and a vapor sealing treatment with steam at 100 to 160 ° C. to sufficiently seal the anodic oxide film and a silica-based film by a sol-gel method. It is characterized in that a coating layer is formed.
ここでシリカ質皮膜とは、二酸化ケイ素を主な成分とする非晶質の透明なガラス質からなる皮膜をいう。
このような二酸化ケイ素を主成分とするシリカガラスからなるコーティング層を陽極酸化皮膜の上に形成する方法としては、ゾル−ゲル法を用いた低温法が好ましい。
例えば、アルコキシシランのゾルを加水分解により縮合反応させてゲル化する方法が挙げられる。
この場合にアルコキシシランを構成するアルキル基は、炭素数1〜6の低級アルキル基であると陽極酸化皮膜に結合する水酸基の密度が高くなり、密着性が向上する。
Here, the siliceous film refers to a film made of an amorphous transparent vitreous material containing silicon dioxide as a main component.
As a method for forming such a coating layer made of silica glass containing silicon dioxide as a main component on the anodic oxide film, a low-temperature method using a sol-gel method is preferable.
For example, there is a method in which a sol of alkoxysilane is subjected to a condensation reaction by hydrolysis to form a gel.
In this case, when the alkyl group constituting the alkoxysilane is a lower alkyl group having 1 to 6 carbon atoms, the density of the hydroxyl group bonded to the anodic oxide film is increased, and the adhesion is improved.
本発明において、低温で透明度が高く1〜10μm程度の薄膜からなるシリカガラス質のコーティング層を形成するのに、例えば、前記ゾル−ゲル法によるシリカ質皮膜を形成ステップは、アルコキシシランとシリカの微粒子との混合ゾルを塗布し、乾燥することでゲル化したものであるのが好ましく、前記アルコキシシランは、Siに官能基を結合していてもよく、Si又はOに結合した置換基は、炭素数1〜6の直鎖又は分岐鎖の低級アルキル基からなる低級アルコキシシランであるのが好ましい。 In the present invention, in order to form a silica glassy coating layer composed of a thin film having a high transparency at a low temperature of about 1 to 10 μm, for example, the step of forming a siliceous film by the sol-gel method includes the step of forming an alkoxysilane and silica. It is preferable that a mixed sol with fine particles is applied and gelled by drying, and the alkoxysilane may have a functional group bonded to Si, and a substituent bonded to Si or O is It is preferably a lower alkoxysilane comprising a linear or branched lower alkyl group having 1 to 6 carbon atoms.
このようにすると、有機−無機ハイブリッド型のシリカ質皮膜となり形成効率が高い。
ここでアルコキシシランは予め、ある程度の縮合反応させた質量平均分子量1,000〜10,000アルコキシシランオリゴマーを用いてもよく、シリカの微粒子は粒子径が10〜200nm程度のシリカ粒子を溶媒に分散させたコロイダルシリカを用いてもよい。
アルコキシシランとコロイダルシリカの配合比率は、固形分としての質量比で1:0.3〜1:1程度が好ましい。
By doing so, an organic-inorganic hybrid type siliceous film is obtained, and the formation efficiency is high.
Here, as the alkoxysilane, a mass average molecular weight of 1,000 to 10,000 alkoxysilane oligomer which has been subjected to a certain degree of condensation reaction in advance may be used, and silica fine particles are dispersed in a solvent by dispersing silica particles having a particle diameter of about 10 to 200 nm. Colloidal silica may be used.
The mixing ratio of alkoxysilane to colloidal silica is preferably about 1: 0.3 to 1: 1 in terms of mass ratio as solids.
本発明に用いるアルコキシシランは(R1)mSi(OR2)4−mで表現でき、m=0,1,2,3のいずれかである。
R1はビニル,3−グリシドキシプロピル,3−アクリロキシプロピル,3−アミノプロピル,3−メルカプトプロピル等の官能基又は、低級アルキル基を示す。
R1又はR2で示される低級アルキル基としては、メチル,エチル,n−プロピル,イソプロピル,n−ブチル,イソブチル,n−ペンチル,1−エチルプロピル,イソペンチル,ネオペンチル等が例として挙げられる。
The alkoxysilane used in the present invention can be represented by (R 1 ) m Si (OR 2 ) 4-m , where m = 0, 1, 2, or 3.
R 1 represents a functional group such as vinyl, 3-glycidoxypropyl, 3-acryloxypropyl, 3-aminopropyl, 3-mercaptopropyl or a lower alkyl group.
Examples of the lower alkyl group represented by R 1 or R 2 include methyl, ethyl, n-propyl, isopropyl, n-butyl, isobutyl, n-pentyl, 1-ethylpropyl, isopentyl, neopentyl and the like.
本発明において、ニッケル塩の水溶液による20〜35℃の低温封孔と100〜160℃の水蒸気(常圧〜高圧蒸気を含む)による蒸気封孔とを組み合せたのは、水蒸気封孔だけでは表面に過度にベーマイト化した粉ふき現象が生じる恐れがあるが、ニッケル塩による低温封孔を組み合せると粉ふきを防止するとともに、コーティング層の密着性が向上する。
ニッケル塩としては、フッ化ニッケルが好ましい。
In the present invention, the combination of low-temperature sealing with an aqueous solution of nickel salt at 20 to 35 ° C. and steam sealing with steam at 100 to 160 ° C. (including normal pressure to high pressure steam) is the only reason that the surface sealing is achieved only with steam sealing. There is a possibility that a dusting phenomenon which is excessively boehmite may occur. However, when low-temperature sealing with a nickel salt is combined, dusting is prevented and the adhesion of the coating layer is improved.
As the nickel salt, nickel fluoride is preferable.
本発明において陽極酸化皮膜は、電解液に硫酸水溶液を用いた硫酸皮膜,シュウ酸を電解液に用いたシュウ酸皮膜等、電解液に制限がなく、膜厚は1〜20μm程度が好ましい。
また、陽極酸化皮膜は、封孔処理前に二次電解着色や染色による着色を施してあってもよい。
また、陽極酸化皮膜の前処理として、バフ研磨,化学研磨,エッチング等の各種前処理が施されていてもよい。
In the present invention, the anodic oxide film is not limited to an electrolytic solution such as a sulfuric acid film using an aqueous solution of sulfuric acid as an electrolytic solution and an oxalic acid film using oxalic acid as an electrolytic solution.
Further, the anodic oxide film may be colored by secondary electrolytic coloring or coloring before the sealing treatment.
Various pretreatments such as buffing, chemical polishing, and etching may be performed as pretreatment of the anodic oxide film.
本発明に用いたシリカ質のコーティング層は、透過率90%以上の高い透明度を示すとともに、密着性に優れる。
そこで、充分に封孔処理した陽極酸化皮膜に対しても密着性に優れ、ガラス質からなるのでキズが付きにくい。
これにより、アルミニウム表面の質感を維持しつつ、高耐食性を付与することができる。
仮に、シリカ質のコーティング層に剥がれが生じても、下地の陽極酸化皮膜が充分に封孔されているので、その部分が白化するのを抑える。
また、シリカ質のコーティング層は密着性がよいので、このコーティング層が剥がれた部分に再コーティングすることも可能である。
The siliceous coating layer used in the present invention exhibits high transparency with a transmittance of 90% or more and excellent adhesion.
Therefore, it has excellent adhesion even to an anodic oxide film that has been sufficiently sealed, and is hardly scratched because it is made of glass.
Thereby, high corrosion resistance can be imparted while maintaining the texture of the aluminum surface.
Even if the silica-based coating layer is peeled off, the underlying anodic oxide film is sufficiently sealed, so that the portion is prevented from whitening.
Further, since the silica-based coating layer has good adhesiveness, it is possible to recoat the portion where the coating layer has been peeled off.
封孔処理の相違による耐水試験を実施したので、以下説明する。
アルミニウム合金の押出材を硫酸水溶液中にて常法に従い、陽極酸化皮膜を形成した。
膜厚は、約10.5μmであった。
次に、図1の表に示すように実施例1は、フッ化ニッケル塩5g/リットルの水溶液を用いて30℃×5〜10分の低温封孔処理を行い、次に水洗後に100〜160℃の水蒸気を用いて15〜30分の蒸気封孔処理をした。
これに対して比較例1は、70〜85℃の温水にて15〜20分の半封孔処理を施した。
次に、実施例1,比較例1とともに、奥野製薬工業株式会社の商品名「Protector」を塗布及び加熱乾燥させ、膜厚約4.8μmのシリカ質のコーティング層を形成した。
次に、故意に上記コーティング層の一部を部分的に強制剥離して、コーティング剥離部分を形成した。
次に、これらのサンプルを純水を用いて40℃×360時間の耐水試験を実施した。
その後に乾燥させ、光沢保持率を計測した。
光沢保持率は、測定器:HORIBA GLOSS CHECKER(IG−410)を用いて、測定角度60°,耐水試験前のグロス値に対する耐水試験後のグロス値の比率として評価した。
この結果、実施例1はコーティング層,コーティング剥離部分とともに高い光沢保持率を維持したのに対して、比較例1はコーティング剥離部分が白化し、低い光沢保持率となり、全体としてまだら模様の表面状態になった。
また、耐水試験後にコーティング層のセロハンテープによるゴバン目剥がれ試験を実施した結果、実施例1,比較例1ともに剥がれ0/100と密着性に差は無かった。
A water resistance test was performed according to the difference in the sealing treatment, and will be described below.
An anodized film was formed on the extruded material of the aluminum alloy in a sulfuric acid aqueous solution according to a conventional method.
The thickness was about 10.5 μm.
Next, as shown in the table of FIG. 1, in Example 1, low-temperature sealing treatment was performed at 30 ° C. for 5 to 10 minutes using an aqueous solution of 5 g / liter of nickel fluoride salt, and then 100 to 160 after water washing. A steam sealing treatment was carried out for 15 to 30 minutes using steam at ℃.
On the other hand, in Comparative Example 1, semi-sealing treatment was performed for 15 to 20 minutes with hot water at 70 to 85 ° C.
Next, together with Example 1 and Comparative Example 1, “Protector” (trade name) of Okuno Pharmaceutical Co., Ltd. was applied and dried by heating to form a siliceous coating layer having a thickness of about 4.8 μm.
Next, a part of the coating layer was intentionally forcibly peeled off partly to form a coating peeling part.
Next, these samples were subjected to a water resistance test at 40 ° C. for 360 hours using pure water.
Then, it was dried and the gloss retention was measured.
The gloss retention was evaluated as a ratio of the gloss value after the water resistance test to the gloss value before the water resistance test at a measurement angle of 60 ° using a measuring device: HORIBA GLOSS CHECKER (IG-410).
As a result, in Example 1, the high gloss retention was maintained together with the coating layer and the coating stripped portion, whereas in Comparative Example 1, the coating stripped portion was whitened and had a low gloss retention, and the surface state of the mottled pattern as a whole was Became.
After the water resistance test, the coating layer was subjected to a peeling test using a cellophane tape. As a result, there was no difference in the adhesion between Example 1 and Comparative Example 1 as 0/100.
Claims (2)
次に低温のニッケル塩水溶液に浸漬する低温封孔処理ステップと、次に100〜160℃の水蒸気による蒸気封孔処理ステップと、
次にゾル−ゲル法によるシリカ質皮膜を形成ステップとを、有し、
前記ゾル−ゲル法によるシリカ質皮膜を形成ステップは、アルコキシシランとシリカの微粒子との混合ゾルを塗布し、乾燥することでゲル化した有機・無機複合皮膜であることを特徴とするアルミニウムの表面処理方法。 Forming an anodized film on the surface of the aluminum;
Next, a low-temperature sealing treatment step of immersing in a low-temperature nickel salt aqueous solution, and then a steam sealing treatment step using steam at 100 to 160 ° C.,
Then the sol - and formation steps siliceous film by gel method, possess,
Before SL sol - forming step a siliceous film by the gel method, the alkoxysilane and the mixed sol of silica fine particles was applied and A is characterized in that an organic-inorganic composite film gelled by drying aluminum Surface treatment method.
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