WO2015093159A1 - アルミニウム材の電解研磨処理方法 - Google Patents
アルミニウム材の電解研磨処理方法 Download PDFInfo
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- WO2015093159A1 WO2015093159A1 PCT/JP2014/079045 JP2014079045W WO2015093159A1 WO 2015093159 A1 WO2015093159 A1 WO 2015093159A1 JP 2014079045 W JP2014079045 W JP 2014079045W WO 2015093159 A1 WO2015093159 A1 WO 2015093159A1
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- treatment
- aluminum material
- electrolytic
- aluminum
- electrolytic polishing
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- 238000011282 treatment Methods 0.000 title claims abstract description 255
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 235
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- OBRBQQWIWWPOPM-UHFFFAOYSA-N NS(O)(=O)=O.OS(O)(=O)=O Chemical compound NS(O)(=O)=O.OS(O)(=O)=O OBRBQQWIWWPOPM-UHFFFAOYSA-N 0.000 description 1
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Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
- C25F3/00—Electrolytic etching or polishing
- C25F3/16—Polishing
- C25F3/18—Polishing of light metals
- C25F3/20—Polishing of light metals of aluminium
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/06—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/18—After-treatment, e.g. pore-sealing
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/18—After-treatment, e.g. pore-sealing
- C25D11/20—Electrolytic after-treatment
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/18—After-treatment, e.g. pore-sealing
- C25D11/24—Chemical after-treatment
Definitions
- the present invention relates to an electrolytic polishing treatment method for an aluminum material made of aluminum or an aluminum alloy, and more particularly to an electrolytic polishing treatment method for an aluminum material suitable for producing an aluminum material having a glossy, uniform and excellent appearance.
- Non-patent Document 1 a vibrating method for vibrating an aluminum material
- Non-patent Document 2 an electrolytic solution stirring method for stirring an electrolytic solution by agitating an aluminum material or a vibrating blade stirrer
- Non-Patent Documents 1 and 2 if the aluminum material has a complicated shape or has a large area, air bubbles are uniformly formed on the entire surface of the aluminum material. It is difficult to completely eliminate the adhesion of air bubbles, and it is difficult to completely remove the adhering bubbles, and the electropolishing process is performed using a concentrated acid, and the apparatus vibrates or perturbs the aluminum material. In addition, it is necessary to make a vibrating blade stirrer with an expensive material excellent in acid resistance, which requires a lot of labor and cost for maintenance and management of the equipment, and is not industrially preferable.
- electrolytic polishing film the anodic oxide film generated during the electrolytic polishing treatment may be intentionally left. However, depending on the application, it may be necessary to remove the electrolytic polishing film remaining on the surface of the aluminum material after electrolytic polishing.
- the electrolytic polishing film remaining on the surface of the aluminum material after the electropolishing has been removed.
- a sodium hydroxide aqueous solution, a mixed aqueous solution of phosphoric acid and chromic acid, sulfuric acid or nitric acid A film peeling treatment is performed in which the aluminum material after electropolishing is immersed in a peeling solution such as an aqueous solution of a fluorine compound, and the anodized film remaining on the surface of the aluminum material is dissolved and removed (Non-patent Document 3).
- the method of film stripping treatment using a stripping solution comprising a mixed aqueous solution of phosphoric acid and chromic acid or an aqueous solution of sulfuric acid or nitric acid and a fluorine compound is an excellent method because it can selectively dissolve and remove the electropolishing film.
- chromic acid and fluorine compounds which are the main components, are harmful substances for environmental hygiene and are currently difficult to use.
- a method of film peeling treatment using a peeling solution comprising an aqueous sodium hydroxide solution is an excellent method because it can selectively dissolve and remove the electropolishing film.
- chromic acid and fluorine compounds which are the main components, are harmful substances for environmental hygiene and are currently difficult to use.
- a method of film peeling treatment using a peeling solution comprising an aqueous sodium hydroxide solution is an excellent method because it can selectively dissolve and remove the electropolishing film.
- chromic acid and fluorine compounds which are the main components, are harmful substances for environmental hygiene and are currently difficult
- the present inventors can solve various problems caused by the above-described electrolytic polishing treatment of an aluminum material, and can easily industrially produce an aluminum material having a glossy, uniform and excellent appearance.
- Regarding the problems associated with the dissolution and removal of the electrolytic polishing film remaining on the surface of the aluminum material, which was performed after the electropolishing of the material the following studies were conducted to develop a method capable of solving the following problems.
- the following examination and development were performed on the problem of point defects caused by bubble adhesion at the start or during the electrolytic polishing of an aluminum material. That is, as a result of detailed examination of the generation mechanism of the point defects generated during the electropolishing process by the present inventors, the point defects generated on the surface of the aluminum material after the electropolishing have been considered so far. It is not a pit (dent) but a protrusion, and the hydrogen gas that causes such point defects is not only generated as a result of an electrolytic reaction during the electropolishing process in the energized state.
- the aluminum material is immersed in the electrolytic treatment solution in a non-energized state before the electropolishing treatment, the aluminum material comes into contact with the electrolytic treatment solution to cause a chemical dissolution reaction. As a result, it was found that the adhering air bubbles adhered to the surface of the aluminum material, which hindered the electrolytic reaction during the subsequent electropolishing process and caused point defects.
- the vibration method of vibrating the aluminum material which is a conventional object to be processed, or the electrolyte solution stirring method using a vibrating blade stirrer of aluminum material compared with the case where it is left without taking any measures, aluminum
- the vibration method and the stirring method for the vibration and the stirring of the electrolyte are adjusted.
- it requires a lot of experience and high level of skill, and it cannot prevent the adhesion of bubbles generated when the aluminum material is immersed in the electrolytic treatment solution in the initial non-energized state during the electrolytic polishing treatment.
- the inventors of the present invention performed an electrolytic reaction in which an electrolytic polishing film is formed on the surface of an aluminum material in an electrolytic processing solution having extremely strong solubility in the aluminum material during the electrolytic polishing treatment of the aluminum material.
- Oxidation treatment is performed, and an anodized film formed in advance on the surface of the aluminum material suppresses generation of hydrogen gas due to chemical dissolution of the surface of the aluminum material at the beginning of the electropolishing process.
- the present inventors further examined how the generation and adhesion of bubbles during the electrolytic polishing treatment of the aluminum material, and during the electrolytic polishing treatment after the start of energization, Almost no generation of hydrogen gas occurs on the aluminum material side serving as the anode, and it has been determined that the generation of hydrogen gas occurs mainly on the cathode side serving as the counter electrode of the aluminum material, and the bubbles of hydrogen gas generated on the cathode side are It diffused to the aluminum material side which is an anode, and it discovered that this diffused bubble adhered to the surface of the aluminum material, and caused the problem of a point-like defect.
- the cathode partition chamber is formed of a liquid permeable material that is permeable (bubble non-permeable) and is permeable to the electrolytic treatment liquid and can ensure conductivity between the electrodes.
- the electropolishing treatment is a method of dissolving the electropolishing film at a high speed while forming a porous type electropolishing film
- the electrolysis solution has a strong solubility in the aluminum material
- chemical dissolution of the surface of the aluminum material starts, so that the electrolytic reaction and chemical dissolution reaction during the electropolishing treatment are kept in a good state to obtain excellent specularity, and immediately after the electropolishing treatment is finished. It is difficult to prevent uniform chemical dissolution.
- an electrolytic polishing film is intentionally left on the surface of the aluminum material after electropolishing, and the electropolishing remaining on this surface after electropolishing. Although the film is dissolved and removed, as described above, there is a problem in dissolving and removing the electrolytic polishing film performed after the electrolytic polishing.
- the present inventors have made further studies on the dissolution removal of the electrolytic polishing film on the surface of the aluminum material after the electrolytic polishing, and the chemical dissolution reaction in which the dissolution of the electrolytic polishing film (oxide) does not involve charge transfer.
- the dissolution of the substrate (metal) is an electrochemical reaction with charge transfer, selective solubility that promotes the chemical dissolution reaction while suppressing the electrochemical reaction.
- a sulfuric acid solution containing sulfuric acid and amines and having a pH of 2 or lower was reached to complete the present invention.
- an object of the present invention is to provide an electrolytic polishing treatment method for an aluminum material, which can easily produce an aluminum material having a glossy, uniform and excellent appearance industrially. That is, the present application provides the following first to fourth inventions, and these first to fourth inventions may be collectively referred to as the present invention.
- an aluminum material made of aluminum or an aluminum alloy is immersed in an electrolytic treatment solution in an electrolytic treatment tank, an electrolytic voltage is applied using the aluminum material as an anode, and the surface of the aluminum material is electropolished.
- It is an electrolytic polishing method, and comprises a polybasic acid aqueous solution having a lower solubility in an aluminum material than the electrolytic treatment liquid in a pretreatment tank provided separately from the electrolytic treatment tank as a pretreatment for the electrolytic polishing treatment.
- Anodizing is performed using a pretreatment liquid and anodizing the aluminum material at a voltage lower than the electrolysis voltage in the electropolishing treatment to form an anodized film on the surface of the aluminum material.
- This is an electrolytic polishing method for an aluminum material.
- an aluminum material made of aluminum or an aluminum alloy is immersed in an electrolytic treatment solution in an electrolytic treatment tank, an electrolytic voltage is applied using the aluminum material as an anode, and the surface of the aluminum material is electropolished.
- the electrolytic treatment tank is formed of a liquid-permeable material that is impermeable to bubbles of hydrogen gas generated at a cathode serving as a counter electrode of the aluminum material, and A cathode partition chamber having an exhaust port for partitioning the cathode from the aluminum material and exhausting the hydrogen gas to the outside of the tank is formed, and during the electrolytic polishing treatment of the aluminum material, the hydrogen gas generated at the cathode in the cathode partition chamber In addition to preventing the bubbles from diffusing to the aluminum material side, a bubble diffusion preventing process for discharging the hydrogen gas from the exhaust port to the outside of the tank is performed.
- an aluminum material made of aluminum or an aluminum alloy is immersed in an electrolytic treatment solution in an electrolytic treatment tank, an electrolytic voltage is applied using the aluminum material as an anode, and the surface of the aluminum material is electropolished.
- An electrolytic polishing method to be processed, and as a post-treatment of the electrolytic polishing treatment an aluminum material after electrolytic polishing is immersed in a post-treatment liquid composed of a sulfuric acid acidic solution containing sulfuric acid and amines and having a pH of 2 or less.
- An electrolytic polishing treatment method for an aluminum material characterized in that a film peeling process for dissolving and removing an electrolytic polishing film present on a surface is performed.
- an aluminum material made of aluminum or an aluminum alloy is immersed in an electrolytic treatment solution in an electrolytic treatment tank, an electrolytic voltage is applied using the aluminum material as an anode, and the surface of the aluminum material is electropolished.
- An electrolytic polishing method to be processed which is performed in the anodizing process as the pretreatment performed in the first invention, the bubble diffusion preventing process in the electrolytic polishing process performed in the second invention, and the third invention.
- An aluminum material electropolishing treatment method comprising performing two or three kinds of treatments selected from film peeling treatment of an electropolishing film as a post-treatment.
- the aluminum material made of aluminum or aluminum alloy to be subjected to electrolytic polishing treatment is not particularly limited, and is intended for various aluminum materials that are required to be mirror-finished by electrolytic polishing treatment.
- Examples include Al-Cu 2000-based materials, Al-Mg 5000-based materials, and Al-Mg-Si 6000-based materials.
- the aluminum material that has a particularly high aluminum purity (Al purity) and is required to have a high degree of mirror finish for example, a high-purity aluminum material having a purity of 99.99% or more, or a pure aluminum-based 1000-based material (for example, A1050 material) etc. can be illustrated.
- the surface of the aluminum material may be preliminarily mirror-finished in advance by means of buffing, cutting, chemical polishing, or the like. It is also effective for aluminum materials that have undergone a specular surface treatment.
- the treatment conditions for electrolytic polishing of the aluminum material in the electrolytic treatment solution in the electrolytic treatment tank are not particularly different from those of the conventional electrolytic polishing treatment of the aluminum material.
- the electrolytic polishing treatment conditions that have been used so far can be employed as they are in terms of the composition of the electrolytic treatment liquid, the electrolytic voltage, the treatment temperature, the treatment time, the inrush current at the start of the electropolishing treatment, and other various conditions.
- examples of the electrolytic treatment liquid include those having a composition of phosphoric acid-sulfuric acid (volume ratio 7: 3) and those having a composition of phosphoric acid-sulfuric acid (volume ratio 1: 1). Can do.
- the solubility in an aluminum material is higher than that of the electrolytic treatment liquid in a pretreatment bath provided separately from the electrolytic treatment bath used in the electrolytic polishing treatment.
- Anodization using a pretreatment solution consisting of a weak polybasic acid aqueous solution and anodizing the aluminum material at a voltage lower than the electrolysis voltage during the electropolishing treatment to form an anodized film on the surface of the aluminum material This is an electrolytic polishing method for an aluminum material to be processed.
- the anodizing treatment is performed in a pretreatment tank provided separately from the electrolytic treatment tank.
- a pretreatment liquid comprising a polybasic acid aqueous solution having a lower solubility in the aluminum material than the electrolytic treatment liquid at the time of anodizing, and anodizing the aluminum material at a voltage lower than the electrolytic voltage in the electrolytic polishing treatment
- a desired anodic oxide film can be easily formed on the surface of the aluminum material during the pretreatment.
- the power supply specifications at the time of electrolytic polishing treatment can be used as they are, so there is no need to prepare a dedicated power source separately, and electrolytic polishing treatment is also possible. Therefore, it is not necessary to form a anodic oxide film on the surface of the aluminum material by flowing a large current in the initial stage, so that it is possible to reduce the capacity of the power source in the electrolytic polishing process, and it is relatively small and inexpensive.
- a power supply device can be employed.
- the pretreatment liquid comprising a polybasic acid aqueous solution having a lower solubility in the aluminum material than the electrolytic treatment liquid used in the electropolishing treatment used in the anodizing treatment as the pretreatment
- examples include sulfuric acid aqueous solution having a composition with a sulfuric acid concentration of 15% by mass, oxalic acid aqueous solution having a composition with an oxalic acid concentration of 2% by mass, and the like.
- a sulfuric acid aqueous solution having a lower sulfuric acid concentration or a higher pH value than the electrolytic treatment liquid is used as the pretreatment liquid.
- the processing conditions for the anodizing treatment as the pretreatment are not different from the processing conditions for the normal anodizing treatment.
- the film thickness of the anodized film formed on the surface of the aluminum material in the anodizing treatment as the pretreatment may be a film thickness formed by a general anodizing treatment, and is not particularly limited. It is about several tens of nm to several tens of ⁇ m.
- the electrolytic treatment tank is formed of a material that is non-permeable to liquid and permeable to bubbles of hydrogen gas generated at a cathode serving as a counter electrode of the aluminum material.
- the cathode partition chamber that partitions the cathode from the aluminum material of the anode is formed of at least a bubble non-permeable material and a liquid permeable material, and a partition wall that partitions the cathode and the aluminum material and hydrogen gas It is sufficient that the hydrogen gas generated in the cathode partition chamber can be discharged from the exhaust port to the outside of the tank, and the material forming the cathode partition chamber is, for example, made of Teflon (registered trademark). Examples thereof include a porous film, for example, a filter medium made of glass such as a sintered glass filter or glass fiber.
- an aluminum material after electropolishing is immersed in a posttreatment solution composed of a sulfuric acid acidic solution containing sulfuric acid and amines and having a pH of 2 or less.
- a posttreatment solution composed of a sulfuric acid acidic solution containing sulfuric acid and amines and having a pH of 2 or less.
- a sulfuric acid solution having a pH of 2 or less containing sulfuric acid and amines is used. It is preferable to be a sulfuric acid solution containing ions and ammonium ions derived from amines, and the pH is usually 2 or less, preferably 1.5 or less. Exceeding this may cause the film to hardly dissolve.
- a post-treatment liquid is a sulfuric acid solution obtained by dissolving a sulfate of amines in water, or a sulfuric acid solution obtained by dissolving sulfuric acid and amines in water.
- amide sulfate such as amide sulfate (sulfamic acid) or its ammonium salt
- an acidic solution of sulfuric acid obtained by dissolving in an aqueous solution more preferably an aqueous solution of amidosulfuric acid.
- examples of amines for preparing an acidic sulfuric acid solution as a post-treatment liquid include ammonia, alkylamines such as methylamine and propylamine, and the like.
- the film peeling treatment performed in the third invention for example, when a 3% by mass-sulfamic acid aqueous solution is used as a post-treatment liquid, a method of immersing under a treatment condition of 70 ° C. and 10 minutes is exemplified.
- the fourth invention of the present application is the anodizing treatment as the pretreatment according to the first invention described above, the bubble diffusion preventing treatment at the time of the electrolytic polishing treatment according to the second invention, and the rear according to the third invention. It is an electrolytic polishing treatment method of an aluminum material for performing two or three kinds of treatments selected from film peeling treatment of an electrolytic polishing film as treatment.
- the treatments according to the first invention, the second invention, and the third invention described above may be combined in any way.
- the polishing treatment for example, the anodizing treatment of the first invention and the bubble diffusion preventing treatment of the second invention may be combined, or the anodizing treatment of the first invention and the film peeling treatment of the third invention.
- the bubble diffusion preventing treatment of the second invention and the film peeling treatment of the third invention may be combined, and when combining three types of treatment, the first invention
- the aluminum material electropolishing treatment is performed by combining the anodizing treatment, the bubble diffusion preventing treatment of the second invention, and the film peeling treatment of the third invention.
- the aluminum material after electropolishing can achieve an excellent appearance with glossiness and uniformity, and at the time of electropolishing treatment There is no need to flow a large current in the initial stage, and the power supply equipment can be downsized.
- hydrogen gas generated at the cathode which is the counter electrode of the aluminum material, does not diffuse to form bubbles on the surface of the aluminum material, thereby preventing point defects due to bubble adhesion.
- the aluminum material after electropolishing can achieve an appearance excellent in gloss and uniformity.
- the electrolytic polishing film remaining on the aluminum material after the electropolishing can be selectively dissolved and removed by the film peeling treatment, and the aluminum material after the electropolishing is glossy and uniform. An excellent appearance can be achieved.
- the aluminum material after electrolytic polishing is excellent in gloss and uniformity by processing in combination with the first invention, the second invention, and the third invention. A good appearance can be achieved.
- FIGS. 1A and 1B are explanatory views for explaining the concept of the first invention, wherein FIG. 1A shows an anodizing treatment step as a pretreatment, and FIG. 1B shows an electropolishing treatment step.
- FIG. 2A and 2B are explanatory views for explaining the concept of the second invention, wherein FIG. 2A shows a conventional electropolishing process, and FIG. 2B shows an electropolishing process of the second invention. .
- FIG. 1 is an explanatory view for explaining the concept of the electrolytic polishing treatment method for an aluminum material according to the first invention, and includes an anodizing treatment step (a) and an electrolytic polishing treatment step (b) as pretreatment.
- the processing steps are shown.
- an anodizing process performed as a pretreatment is performed in a pretreatment tank 2 provided separately from the electrolytic treatment tank 1 in the electrolytic polishing process step (b).
- the pretreatment liquid 3 is loaded, and an aluminum material 4 as an object to be treated is used as an anode, and a direct current voltage is applied between the cathode 5 as a counter electrode of the aluminum material 4 and an anodized film is formed on the surface of the aluminum material. 6 is formed.
- the electrolytic treatment liquid 7 is loaded in the electrolytic treatment tank 1, and then in the electrolytic treatment solution 7 in the pretreatment anodic oxidation treatment step (a).
- An aluminum material 4 as an object to be processed having an anodized film 6 formed on the surface is immersed, and then a DC voltage is applied between the aluminum material 4 as an anode and a cathode 8 which is a counter electrode of the aluminum material 4 to form aluminum. Electrolytic polishing is performed on the surface of the material 4.
- the aluminum material 4 to be treated is immersed in the electrolytic treatment liquid 7 in a non-energized state.
- the metal surface of the aluminum material 4 is in direct contact with the electrolytic treatment solution 7 when immersed in a non-energized state (S 1).
- the anodized film 6 on the surface of the aluminum material 4 that is in direct contact with the electrolytic treatment liquid 7 is gradually dissolved in the electrolytic treatment liquid 7 and does not generate hydrogen gas at that time.
- this electrolytic polishing treatment step (b) when a direct current voltage is applied between the anode aluminum material 4 and the cathode 8 to start the electrolytic polishing treatment, during the electrolytic treatment of this aluminum material 4 (S2).
- the anodic oxide film 6 on the surface of the aluminum material 4 gradually dissolves and disappears in the electrolytic treatment liquid 7, and the formation of the electropolishing film 9 and the chemical dissolution of metal aluminum occur on the surface of the aluminum material 4.
- the anodic oxide film 6 is gradually dissolved and the surface of the aluminum material 4 is electropolished.
- the energization is stopped, and the aluminum material 4 after the electropolishing is immediately lifted from the electrolysis treatment tank 1, washed with pure water, air-dried, and the aluminum material after the electropolishing.
- the electrolytic polishing film 9 is consciously left on the surface of the aluminum material 4 after the electrolytic polishing at the end of energization of the electrolytic polishing treatment (S3), and then this residual electrolytic polishing is left.
- the third invention will be continued.
- the third invention described below is an effective method for selectively dissolving and removing the electrolytic polishing film on the surface of the aluminum material generated by the electrolytic polishing treatment.
- the present invention is not limited to the case where it is subsequently performed, and it is needless to say that it may be performed subsequent to the conventional electrolytic polishing treatment.
- the electrolytically polished aluminum material pulled up from the electrolytic polishing liquid at the end of the electrolytic polishing process is immersed in a post-treatment liquid composed of a sulfuric acid acidic solution having a pH of 2 or less containing sulfuric acid and amines, A film peeling treatment for selectively dissolving and removing the electrolytic polishing film remaining on the surface of the polished aluminum material is performed. After the film peeling treatment is completed, the aluminum material after electrolytic polishing is pulled up from the post-treatment tank, immediately washed with pure water and air-dried to obtain an aluminum material after electrolytic polishing of the product.
- a post-treatment liquid composed of a sulfuric acid acidic solution having a pH of 2 or less containing sulfuric acid and amines
- FIG. 2 is an explanatory view for explaining the concept of the electrolytic polishing treatment method for an aluminum material according to the second invention
- FIG. 2 (A) is an electrolytic polishing treatment step using a conventional electrolytic treatment tank
- FIG. 2 (B) is an explanatory view showing an electrolytic polishing treatment process using the electrolytic treatment tank according to the second invention.
- FIG. 2A showing a conventional electrolytic treatment tank 1
- an electrolytic treatment liquid 7 is loaded in the electrolytic treatment tank 1
- an aluminum material 4 as an object to be treated is immersed therein.
- a DC voltage is applied between the aluminum material 4 and the cathode 8 which is a counter electrode, and the surface of the aluminum material 4 is subjected to electrolytic polishing.
- hydrogen gas bubbles 10 are generated on the cathode 8 side during the electrolytic polishing process and diffused into the electrolytic treatment solution 7, most of which are electrolyzed. Although it scatters from the liquid surface of the treatment liquid 7 into the atmosphere, a part of it diffuses to the aluminum material 4 side of the anode, adheres to the surface of the aluminum material 4, and is dotted on the surface of the aluminum material after electropolishing. It causes a defect.
- FIG. 2 (B) in the electrolytic treatment tank 1, hydrogen gas bubbles 10 generated at the cathode 8, which is the counter electrode of the aluminum material 4.
- a cathode partition chamber 11 is formed which is formed of a material which is impermeable to bubbles and liquid permeable, partitions the cathode 8 from the aluminum material 4 and has an exhaust port 12 for discharging the generated bubbles 10 out of the tank.
- the bubbles 10 generated at the cathode 8 in the cathode compartment 11 are prevented from diffusing to the aluminum material 4 side, and the bubbles 10 are discharged from the exhaust port 12 to the outside of the tank.
- This bubble diffusion preventing process prevents the hydrogen gas bubbles 10 generated at the cathode 8 during the electrolytic polishing process from adhering to the surface of the aluminum material 4.
- Examples 1 to 3 A plate material having an Al purity of 99.99% by mass was used as the aluminum material, and an aluminum piece having a size of 50 mm ⁇ 50 mm ⁇ 10 mm was cut out from the plate material.
- the pretreatment liquid shown in Table 1 was used, and the treatment conditions (voltage) shown in Table 1 were used.
- the amount of electricity and temperature was subjected to an anodizing treatment as a pretreatment, washed with water and dried to obtain pretreated aluminum pieces of Examples 1 to 3.
- Comparative Example 1 The same aluminum pieces as used in Examples 1 to 3 above were used, and the electrolytic treatment solution shown in Table 1 was used without performing the anodic oxidation treatment as a pretreatment, and the treatment conditions (temperature, The electropolishing treatment was performed at a voltage, a time, and an inrush current, immediately washed with water and dried to obtain an aluminum piece (test piece) after electropolishing of Comparative Example 1.
- a tank was constructed.
- As the aluminum material the same aluminum piece having an Al purity of 99.99% by mass as used in Examples 1 to 3 was used.
- the electrolytic treatment solution shown in Table 2 (sulfuric acid-phosphoric acid mass ratio 1: 5 solution) was charged into the electrolytic treatment tank, and the treatment conditions shown in Table 2 (temperature, voltage, time, and inrush current). Then, the aluminum pieces were electropolished while carrying out bubble diffusion prevention treatment in the cathode compartment, and immediately washed with water and dried to obtain aluminum pieces (test pieces) after electropolishing of Examples 4 to 5.
- Example 4 to 5 were evaluated in the same manner as in Examples 1 to 3 by examining the bubble adhesion inhibiting property during processing, the specular gloss, the point defects, and the presence or absence of interference colors. These results are shown in Table 2 together with Comparative Example 1 without the bubble diffusion prevention treatment.
- Examples 6 to 7 and Comparative Examples 2 to 3 After performing electrolytic polishing treatment in the same manner as in Comparative Example 1 above, using the post-treatment liquid shown in Table 3, the film is immersed in the post-treatment liquid under the conditions shown in Table 3 as post-treatment and peels off the electrolytic polishing film Stripping treatment was performed, and aluminum pieces (test pieces) after electropolishing of Examples 6 to 7 and Comparative Examples 2 to 3 were obtained.
- Examples 8 to 11 As the aluminum material, the same aluminum piece having an Al purity of 99.99% by mass as used in Examples 1 to 3 was used, and as shown in Table 4, the pretreatment (anodization treatment) of Example 1 and Example 4 were performed. And / or post-treatment (film peeling treatment) of Example 6 to obtain aluminum pieces (test pieces) after electropolishing of Examples 8 to 11.
- Example 8 to 11 were evaluated in the same manner as in Examples 1 to 3 above by examining the bubble adhesion inhibiting property during processing, the specular gloss, the point defects, and the presence or absence of interference colors. Also, in these evaluation items, if all items are good (no interference color and having a specular gloss that does not show a defect over a wide area), ⁇ , and any 2 or 3 items are good The case was evaluated as ⁇ , and a comprehensive evaluation was performed. These results are shown in Table 4.
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Abstract
Description
すなわち、本発明者らが電解研磨処理時に発生する点状欠陥の生成機構を詳細に検討した結果、電解研磨後のアルミニウム材の表面に発生する点状欠陥は、これまで考えられていたようなピット(窪み)ではなくて突起であることを突き止め、また、このような点状欠陥の原因となる水素ガスは、単に通電状態の電解研磨の処理中に電解反応の結果として発生するだけでなく、電解研磨処理前にアルミニウム材を無通電状態で電解処理液中に浸漬する際に、アルミニウム材が電解処理液と接触して化学的溶解反応を起こし、この際に発生した水素ガスが気泡となってアルミニウム材の表面に付着し、この付着した気泡も後の電解研磨処理時に電解反応を阻害し、点状欠陥の原因となることを突き止めた。
すなわち、本発明者らは、アルミニウム材の電解研磨処理の処理中における気泡の発生及び付着がどのようにして発生するかについて更に検討を行い、通電開始後の電解研磨処理の処理中においては、陽極となるアルミニウム材側ではほとんど水素ガスの発生が起こらず、水素ガスの発生は主としてこのアルミニウム材の対極となる陰極側で起こることを突き止め、また、この陰極側で発生した水素ガスの気泡が陽極であるアルミニウム材側に拡散し、この拡散した気泡がアルミニウム材の表面に付着し、点状欠陥の問題を引き起こすことを突き止めた。
すなわち、アルミニウム材の電解研磨処理の際には、処理終了後にアルミニウム材をそのまま電解処理液中に浸漬しておくとこの電解処理液によりアルミニウム材の表面が化学的に溶解され、この際に不均一な化学的溶解が生じて局部的な凸部が発生し、結果として点状欠陥の原因になることから、処理終了後には直ちに電解処理液中から電解研磨後のアルミニウム材を取り出す必要がある。しかるに、電解研磨処理が多孔質型の電解研磨皮膜を形成しながら高速でこの電解研磨皮膜を溶解する方法であることから、電解処理液はアルミニウム材に対して強い溶解性を有し、通電を停止すると直ちにアルミニウム材の表面の化学的溶解が始まるので、電解研磨処理時の電解反応や化学的溶解反応を良好な状態に保って優れた鏡面性を得つつ、電解研磨処理の終了直後の不均一な化学的溶解を防止するのは困難である。
すなわち、本願は以下の第1の発明から第4の発明を提供するものであり、これら第1の発明から第4の発明までをまとめて本発明ということがある。
この図1において、陽極酸化処理工程(a)では、電解研磨処理工程(b)の電解処理槽1とは別に設けられた前処理槽2内に、前処理として実施する陽極酸化処理のための前処理液3が装填されており、被処理物であるアルミニウム材4を陽極とし、このアルミニウム材4の対極である陰極5との間に直流電圧を印加し、アルミニウム材の表面に陽極酸化皮膜6が形成される。
ここで、図1に示すように、電解研磨処理の通電終了時(S3)に電解研磨後のアルミニウム材4の表面に電解研磨皮膜9を意識的に残存させ、その後にこの残存させた電解研磨皮膜9を除去する場合には、引き続き第3の発明を実施することになる。なお、以下に説明する第3の発明は、電解研磨処理で生成したアルミニウム材表面の電解研磨皮膜を選択的に溶解して除去する上で効果的な方法であることから、第1の発明に引き続いて実施される場合に限られるものではなく、従来の電解研磨処理に引き続いて実施してもよいことは勿論である。
この皮膜剥離処理が終了した後には、電解研磨後のアルミニウム材を後処理槽から引き上げ、直ちに純水で洗浄し風乾させて製品の電解研磨後のアルミニウム材とする。
従来の電解処理槽1を示す図2(A)において、電解処理槽1には電解処理液7が装填されており、被処理物のアルミニウム材4が浸漬され、その後、このアルミニウム材4を陽極としてアルミニウム材4の対極である陰極8との間に直流電圧が印加され、アルミニウム材4の表面に電解研磨処理が施される。そして、この従来の電解処理槽1を用いた電解研磨処理においては、その電解研磨処理中、陰極8側で水素ガスの気泡10が発生し、電解処理液7中に拡散し、その多くが電解処理液7の液面から大気中に飛散するが、その一部は陽極のアルミニウム材4側へと拡散し、このアルミニウム材4の表面に付着し、電解研磨後のアルミニウム材の表面に点状欠陥を発生させる原因になる。
アルミニウム材としてAl純度99.99質量%の板材を用い、この板材から50mm×50mm×10mmの大きさのアルミ片を切り出し、表1に示す前処理液を用い、表1に示す処理条件(電圧、電気量及び温度)で前処理としての陽極酸化処理を行い、水洗し乾燥して実施例1~3の前処理済アルミ片を得た。
上記の実施例1~3で用いたものと同じアルミ片を使用し、前処理としての陽極酸化処理を行うことなく、表1に示す電解処理液を用い、表1に示す処理条件(温度、電圧、時間、及び突入電流)で電解研磨処理を行い、直ちに水洗し乾燥させて比較例1の電解研磨後のアルミ片(試験片)を得た。
上記実施例1~3及び比較例1の電解研磨処理中、ガラス製処理槽外側から目視でアルミ片表面を観察して各実施例及び比較例のアルミ片の表面に付着した水素ガスの気泡を調べ、○:気泡付着なし、△:付着気泡2個以下(1cm2当り)、及び×:付着気泡3個以上(1cm2当り)の基準で電解研磨処理中における気泡付着の抑止効果(処理中気泡付着抑止性)を評価した。
結果を表1に示す。
また、上記実施例1~3及び比較例1で得られた各試験片について、目視により以下の外観観察を行い、鏡面光沢性、点状欠陥、干渉色有無を調べて評価した。
鏡面光沢性については、目視観察でサンプルに写り込む物体の見え方が、○:歪みがなくて明瞭に写り込むもの、△:明瞭に写り込むが、一部に歪みが生じているもの、及び×:歪みがひどくて写り込まないもの、の基準で電解研磨処理中における気泡付着の程度を評価した。
また、点状欠陥については、各試験片の表面を蛍光灯下で目視により観察し、視認された点状欠陥の個数を数え、○:0個/cm2、△:1個/cm2以上3個/cm2未満、及び×:3個/cm2以上の基準で評価した。
干渉色の有無については、蛍光灯下で各試験片を70°傾けてその表面を目視により観察し、電解研磨皮膜による干渉色を確認し、○:干渉色が全く見えないもの、△:試料の一部に干渉色が見えたもの、及び×:試料の全体に干渉模様が見えたもの、の基準で評価した。
これらの結果を表1に示す。
水素ガスに対して気泡非透過性であると共に液透過性の材料であるテフロン(登録商標)製多孔質フィルタ(実施例4)又はガラス繊維製フィルタ(実施例5)を使用し、電解研磨処理のための槽内に、陰極を陽極(アルミニウム材)から仕切ると共に、電解研磨処理中に発生する水素ガスの気泡を窓外に排出するための排気口を有する陰極仕切室を形成し、電解処理槽を構成した。
また、アルミニウム材としては、上記実施例1~3で用いたものと同じAl純度99.99質量%のアルミ片を用いた。
これらの結果を、気泡拡散防止処理無しの上記比較例1と共に、表2に示す。
上記の比較例1と同様にして電解研磨処理を行った後、表3に示す後処理液を用い、後処理として表3に示す条件で後処理液中に浸漬して電解研磨皮膜を剥がす皮膜剥離処理を行い、実施例6~7及び比較例2~3の電解研磨後のアルミ片(試験片)を得た。
これらの結果を表3に示す。
アルミニウム材として上記実施例1~3で用いたものと同じAl純度99.99質量%のアルミ片を用い、表4に示すように、実施例1の前処理(陽極酸化処理)、実施例4の気泡拡散防止処理、及び/又は、実施例6の後処理(皮膜剥離処理)を実施し、実施例8~11の電解研磨後のアルミ片(試験片)を得た。
これらの結果を表4に示す。
Claims (6)
- アルミニウム又はアルミニウム合金からなるアルミニウム材を電解処理槽内の電解処理液中に浸漬し、アルミニウム材を陽極として電解電圧を印加し、アルミニウム材の表面を電解研磨処理する電解研磨方法であり、
前記電解研磨処理の前処理として、前記電解処理槽とは別に設けられた前処理槽内で、前記電解処理液よりもアルミニウム材に対する溶解性の弱い多塩基酸水溶液からなる前処理液を用い、かつ、前記電解研磨処理の際の電解電圧よりも低い電圧で前記アルミニウム材を陽極酸化し、アルミニウム材の表面に陽極酸化皮膜を形成させる陽極酸化処理を行うことを特徴とするアルミニウム材の電解研磨処理方法。 - アルミニウム又はアルミニウム合金からなるアルミニウム材を電解処理槽内の電解処理液中に浸漬し、アルミニウム材を陽極として電解電圧を印加し、アルミニウム材の表面を電解研磨処理する電解研磨方法であり、
前記電解処理槽内には、前記アルミニウム材の対極となる陰極で発生する水素ガスの気泡に対して気泡非透過性であると共に液透過性の材料で形成され、前記陰極をアルミニウム材から仕切ると共に、前記水素ガスを槽外に排出する排気口を有する陰極仕切室を形成し、アルミニウム材の電解研磨処理時には、前記陰極仕切室内の陰極で発生した水素ガスの気泡がアルミニウム材側に拡散するのを防止すると共に、この水素ガスを前記排気口から槽外に排出させる気泡拡散防止処理を行うことを特徴とするアルミニウム材の電解研磨処理方法。 - アルミニウム又はアルミニウム合金からなるアルミニウム材を電解処理槽内の電解処理液中に浸漬し、アルミニウム材を陽極として電解電圧を印加し、アルミニウム材の表面を電解研磨処理する電解研磨方法であり、
前記電解研磨処理の後処理として、硫酸及びアミン類を含むpH2以下の硫酸酸性溶液からなる後処理液中に電解研磨後のアルミニウム材を浸漬し、このアルミニウム材の表面に存在する電解研磨皮膜を溶解させて除去する皮膜剥離処理を行うことを特徴とするアルミニウム材の電解研磨処理方法。 - アルミニウム又はアルミニウム合金からなるアルミニウム材を電解処理槽内の電解処理液中に浸漬し、アルミニウム材を陽極として電解電圧を印加し、アルミニウム材の表面を電解研磨処理する電解研磨方法であり、
前記請求項1に記載された前処理としての陽極酸化処理、前記請求項2に記載された電解研磨処理時の気泡拡散防止処理、及び前記請求項3に記載された後処理としての電解研磨皮膜の皮膜剥離処理から選ばれた2種又は3種の処理を行うことを特徴とするアルミニウム材の電解研磨処理方法。 - 前記後処理液が、アミン類の硫酸塩を水に溶解して得られた硫酸酸性溶液であるか、硫酸とアミン類とを水に溶解して得られた硫酸酸性溶液であるか、硫酸、アミン類、及びアミン類の硫酸塩を水に溶解して得られた硫酸酸性溶液であるか、又は、アミド硫酸又はそのアンモニウム塩を水に溶解して得られた硫酸酸性溶液である請求項3又は4に記載のアルミニウム材の電解研磨処理方法。
- 前記後処理液として用いる硫酸酸性溶液がアミド硫酸の水溶液である請求項4に記載のアルミニウム材の電解研磨処理方法。
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US20180298512A1 (en) * | 2017-04-13 | 2018-10-18 | General Electric Company | Electropolishing and anodizing method for brush holder apparatus |
CN111088503A (zh) * | 2019-12-31 | 2020-05-01 | 中山市皓祥模具五金有限公司 | 一种铝制品的表面处理工艺 |
CN111235579A (zh) * | 2019-12-31 | 2020-06-05 | 南方科技大学 | 金属抛光方法 |
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JP2001107300A (ja) * | 1999-10-08 | 2001-04-17 | Ulvac Japan Ltd | アルミニウム材の電解研磨処理方法 |
JP2002129399A (ja) * | 2000-10-27 | 2002-05-09 | Samsung Techwin Co Ltd | 金属表面処理装置とこれを用いた金属表面処理方法 |
JP2007123433A (ja) * | 2005-10-26 | 2007-05-17 | Nippon Chemicon Corp | アルミニウムエッチング箔の製造方法 |
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CN1006000B (zh) * | 1985-04-23 | 1989-12-06 | 东北工学院 | 铝或铝合金表面乳白色薄膜生成法 |
DE60021140T2 (de) * | 1999-04-22 | 2006-05-04 | Fuji Photo Film Co., Ltd., Minami-Ashigara | Verfahren zur Herstellung eines Aluminiumträgers für lithographische Druckplatten |
DE10149928C1 (de) * | 2001-10-10 | 2002-12-12 | Wkw Erbsloeh Automotive Gmbh | Verfahren zum Glänzen von Aluminium und dessen Verwendung |
CN102649209B (zh) * | 2011-02-23 | 2015-08-12 | 汉达精密电子(昆山)有限公司 | 一种铝合金外观件的制作方法 |
CN103122475B (zh) * | 2011-11-21 | 2015-11-25 | 比亚迪股份有限公司 | 一种铝合金电化学抛光液及一种铝合金电化学抛光方法 |
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2014
- 2014-10-31 WO PCT/JP2014/079045 patent/WO2015093159A1/ja active Application Filing
- 2014-10-31 CN CN201711320047.6A patent/CN108060452A/zh active Pending
- 2014-10-31 CN CN201711318826.2A patent/CN107858743A/zh active Pending
- 2014-10-31 CN CN201480069286.7A patent/CN105829585A/zh active Pending
- 2014-10-31 KR KR1020167019028A patent/KR20160100343A/ko not_active Application Discontinuation
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JP2001107300A (ja) * | 1999-10-08 | 2001-04-17 | Ulvac Japan Ltd | アルミニウム材の電解研磨処理方法 |
JP2002129399A (ja) * | 2000-10-27 | 2002-05-09 | Samsung Techwin Co Ltd | 金属表面処理装置とこれを用いた金属表面処理方法 |
JP2007123433A (ja) * | 2005-10-26 | 2007-05-17 | Nippon Chemicon Corp | アルミニウムエッチング箔の製造方法 |
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JP2015117418A (ja) | 2015-06-25 |
KR20160100343A (ko) | 2016-08-23 |
US20160376725A1 (en) | 2016-12-29 |
TWI636160B (zh) | 2018-09-21 |
TW201538802A (zh) | 2015-10-16 |
CN105829585A (zh) | 2016-08-03 |
JP6078851B2 (ja) | 2017-02-15 |
CN108060452A (zh) | 2018-05-22 |
CN107858743A (zh) | 2018-03-30 |
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