WO2011099115A1 - Filtre à membrane en alumite et procédé de production d'un filtre à membrane en alumite - Google Patents

Filtre à membrane en alumite et procédé de production d'un filtre à membrane en alumite Download PDF

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Publication number
WO2011099115A1
WO2011099115A1 PCT/JP2010/051857 JP2010051857W WO2011099115A1 WO 2011099115 A1 WO2011099115 A1 WO 2011099115A1 JP 2010051857 W JP2010051857 W JP 2010051857W WO 2011099115 A1 WO2011099115 A1 WO 2011099115A1
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Prior art keywords
aluminum
membrane filter
alumite
film
composition
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PCT/JP2010/051857
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English (en)
Japanese (ja)
Inventor
中井　真澄
清弘 黒川
蓮尾　俊治
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九州三井アルミニウム工業株式会社
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Priority to PCT/JP2010/051857 priority Critical patent/WO2011099115A1/fr
Publication of WO2011099115A1 publication Critical patent/WO2011099115A1/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
    • B01D67/0039—Inorganic membrane manufacture
    • B01D67/0053—Inorganic membrane manufacture by inducing porosity into non porous precursor membranes
    • B01D67/006—Inorganic membrane manufacture by inducing porosity into non porous precursor membranes by elimination of segments of the precursor, e.g. nucleation-track membranes, lithography or laser methods
    • B01D67/0065—Inorganic membrane manufacture by inducing porosity into non porous precursor membranes by elimination of segments of the precursor, e.g. nucleation-track membranes, lithography or laser methods by anodic oxidation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
    • B01D71/02—Inorganic material
    • B01D71/024—Oxides
    • B01D71/025—Aluminium oxide
    • 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
    • C25D11/045—Anodisation of aluminium or alloys based thereon for forming AAO templates
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2325/00—Details relating to properties of membranes
    • B01D2325/02—Details relating to pores or porosity of the membranes
    • B01D2325/0283—Pore size

Definitions

  • the present invention relates to an anodized membrane filter and an alumite membrane filter manufacturing method. Specifically, the present invention relates to an alumite membrane filter used for a microfiltration membrane and a method for producing an alumite membrane filter used for a microfiltration membrane.
  • Membrane filters that have been put to practical use in the field of microfiltration are specifically used for, for example, protein adsorbents, water purification, air purification, structures for deodorized exhaust gas equipment, ozone removal, and various virus removal.
  • the membrane filter includes an organic membrane filter and an inorganic membrane filter.
  • Many organic membrane filters do not have independent pores and have a relatively wide pore size distribution. For this reason, the separation accuracy of a specific object, which is the most important function of a filter, is inferior, and research for improving the accuracy is being promoted in various fields.
  • a filter made by a so-called track etching method that forms pores by irradiating an organic film made of a polymer with high-energy particles generated from a nuclear reactor and etching the tracks where the particles have passed through the organic film. Proposed.
  • this method can form independent pores with a narrow pore size distribution upright with respect to the organic film, but in order to avoid the generation of double holes due to the incidence of particles overlapping during track formation, the pore density There is a problem that the so-called porosity cannot be increased.
  • a porous alumina membrane filter using an anodized aluminum film As an inorganic membrane filter, a porous alumina membrane filter using an anodized aluminum film is known.
  • the porous alumina membrane filter is prepared by anodizing aluminum in an acidic electrolyte and peeling the anodized film from the material. Since the independent pores having a narrow pore size distribution are formed with a high porosity, the amount of filtration per hour is high, and it can be produced at low cost.
  • the micropores are arranged at regular intervals, a method of arranging them more regularly has been proposed.
  • Patent Document 1 a silicon substrate in which protrusions having a diameter of about 25 nm and a height of 60 nm are regularly arranged with a period of 0.1 ⁇ m is placed on an aluminum plate having a purity of 99.99%, and pressure is applied to the aluminum plate.
  • a method is described in which a depression is formed on the surface, and an anodization of the aluminum plate on which the depression is formed is performed.
  • a porous anodized alumina film having a regular hexagonal shape with respect to each pore and an equal spacing between the pores is obtained with a pore spacing of 100 nm.
  • the filter produced by such a method has a problem of hydration reaction such that pores contract and clog when hot water or boiling water is filtered, and a problem of strength due to lack of a hydrated film.
  • a film made of a high-purity aluminum material has a phenomenon that deformation or cracks occur, and it is difficult to obtain an alumite membrane filter that suppresses the hydration reaction and has improved strength.
  • the present invention has been made in view of the above points, and aims to provide an alumite membrane filter having excellent heat resistance and a method for producing such an alumite membrane filter.
  • the anodized membrane filter of the present invention for achieving the above object is an aluminum anodic oxide film having fine pores, the composition of which includes Al, O, and Mg, and the balance is inevitable impurities.
  • the aluminum membrane filter has an Mg composition of 0.01% to 5.0% by mass.
  • the Mg composition is 0.01% or more, the composition is different from that of the conventional aluminum membrane filter.
  • the reason why the composition is 5% or less is that the Mg component dissolves in the electrolyte during anodizing of anodized aluminum This is because the Mg composition in the aluminum membrane filter does not exceed 5% even with an aluminum alloy having a composition of Mg solid solubility limit.
  • the composition of the aluminum material for forming the alumite membrane filter of the present invention is mass%, Mg: 0.03 to 14.9%, and Mg: 0.03 to 2.8% is preferable in actual use. .
  • the content is limited to 0.03% or more, if less than 0.03%, the Mg component dissolves in the electrolytic solution during anodizing of anodized aluminum, and the Mg in the aluminum membrane filter disappears, and the effect is lost.
  • the reason for limiting to 9% or less is that it is possible to suppress the precipitation of Mg 2 Al 3 which is an intermetallic compound in the aluminum material, and to easily suppress the formation of discontinuous micropores during the anodizing treatment.
  • Mg 2 Al 3 may be precipitated in the aluminum material. Therefore, it is preferable to set Mg to 2.8% or less.
  • the crystal structure of Al 2 O 3 is ⁇ -Al 2 O 3 , ⁇ -Al 2 O 3 , ⁇ -Al 2 O 3 and ⁇ -Al 2 O 3.
  • the phase is transformed, the strength is improved.
  • the method for producing an alumite membrane filter of the present invention has a composition of mass%, Mg: 0.03% to 14.9%, and more preferably Mg: 0.03 to
  • the aluminum base material containing Mg 0.03-14.9%, it contains 0.03% or more of Mg, so that it can have a composition different from that of aluminum having a purity of 99.99%, Since Mg is limited to 14.9% or less of the solid solution limit, precipitation of Mg 2 Al 3 which is an intermetallic compound is suppressed, and formation of discontinuous fine pores is suppressed during anodizing treatment. It becomes easy. Moreover, the reason why 2.8% or less is preferable is that Mg 2 Al 3 may be precipitated depending on the cooling rate after heat treatment such as solution treatment.
  • the method for producing an alumite membrane filter of the present invention includes a step of heating the aluminum anodized film to about 800 ° C. or higher, the aluminum anodized film can be at least ⁇ -ized.
  • the method for producing an alumite membrane filter of the present invention includes a step of heating the aluminum anodic oxide film to about 1200 ° C. or more, the aluminum anodic oxide film can be ⁇ -ized.
  • the anodized membrane filter according to the present invention is excellent in heat resistance.
  • the method for producing an alumite membrane filter according to the present invention can produce an alumite membrane filter having excellent heat resistance.
  • the alumite membrane filter of the present invention is an aluminum anodized film having fine pores, the composition of which includes Al, O, and Mg, and the balance is inevitable impurities. Also, if the composition of the aluminum anodized film constituting the alumite membrane filter does not contain Mg, it becomes the same component as the aluminum anodized film made of aluminum with a purity of 99.99%, and cracking occurs when heated at high temperatures, which is not preferable. . Moreover, the Mg concentration in the aluminum anodic oxide film constituting the anodized membrane filter was limited to 5.0% or less because the Mg component was dissolved in the electrolytic solution during anodizing of the anodized aluminum and 1/3 of the aluminum base material. This is because, for example, an Mg alloy in the aluminum membrane filter does not exceed 5% even in an aluminum alloy (14.9% Mg) having a composition of Mg solid solubility limit.
  • the Mg concentration in the aluminum base material for forming the aluminum anodic oxide film constituting the anodized membrane filter is less than 0.03 mass%, the Mg component is dissolved in the electrolytic solution during anodizing of the anodized aluminum. Since the Mg composition in the membrane filter becomes 0 and the effect is lost, 0.03% by mass or more is good, and when it exceeds 14.9% by mass, Mg 2 Al 3 precipitates in the aluminum base material, and as a result In the process of forming the aluminum anodic oxide film, discontinuous (that is, not straight) partial pores are likely to be formed at positions where Mg 2 Al 3 is present, which is not preferable as a filter. Depending on the cooling rate after heat treatment such as solution treatment, Mg 2 Al 3 may be precipitated, so Mg is preferably 2.8% or less.
  • the anodized aluminum membrane filter of the present invention has different Al 2 O 3 in the aluminum anodized film before and after being heated. That is, Al 2 O 3 of the aluminum anodic oxide film is amorphous before being heated, but ⁇ -Al 2 O 3 , ⁇ -Al 2 O 3 , or ⁇ after being heated. As a mixture of -Al 2 O 3 and ⁇ -Al 2 O 3 , phase transformations such as ⁇ (gamma) and ⁇ (alpha) transformations occur, improving strength and preventing pore hydration (clogging) it can. Among these, it is desirable that the remaining Al 2 O 3 is only ⁇ -Al 2 O 3 .
  • an example of the manufacturing method of the alumite membrane filter of this invention is demonstrated.
  • an aluminum base material having a composition of mass%, Mg: 0.03% to 14.9%, and the balance being Al and inevitable impurities is prepared.
  • the surface of the aluminum substrate is chemically polished.
  • any method may be used as long as the unevenness on the surface of the aluminum base material can be eliminated. Examples of methods other than the above include a method of electrolytic polishing. .
  • a chemically polished aluminum substrate is immersed as an anode in a treatment solution at a constant temperature
  • a carbon plate is immersed as a cathode
  • a voltage is applied to these anode and cathode.
  • an aluminum anodic oxide film is formed and grown on the surface of the anode, that is, the surface of the aluminum substrate, by the mechanism shown in FIG. That is, by applying a voltage to the aluminum base material 2, first, as shown in FIG. 1A, a barrier layer film 6 grows on the aluminum base 4.
  • FIG. 1B an aluminum anodic oxide film 3 including the barrier layer film 6 is formed on the barrier layer film 6, and fine holes 5 are formed in the aluminum anodic oxide film 3.
  • the alumite membrane filter 1 having fine pores 5 as shown in FIG. 2 is obtained. If necessary, the obtained alumite membrane filter is heated to 800 ° C. or higher, preferably 1200 ° C. or higher for about 30 minutes or longer using, for example, an electric furnace.
  • a voltage lower than the applied current is applied to decrease the current value, and the voltage is continuously applied to gradually increase the current. Increase the value.
  • a voltage lower than the applied voltage is applied to form a finer fine hole.
  • hydrogen gas is generated between the aluminum substrate and the aluminum anodized film by applying a voltage with the aluminum substrate as the cathode and the carbon plate as the anode, thereby peeling the anodized film from the aluminum substrate.
  • the peeled aluminum anodic oxide film is immersed in an acidic solution, and the barrier layer film is removed to obtain an alumite membrane filter having fine pores penetrating therethrough.
  • dissolving aluminum is mentioned, for example.
  • the aluminum substrate chemically polished in a treatment solution having a bath temperature of about 20 ° C. and an oxalic acid concentration of about 3% by mass was immersed as an anode. As dipped carbon plate. Then, a voltage of about 50 V was applied to these anode and cathode to form fine holes in the aluminum anodic oxide film. After forming the micropores, a voltage lower than the applied voltage was applied to decrease the current value, and the voltage was continuously applied to gradually increase the current value. When the current value became constant, a voltage lower than the applied voltage was applied to form finer fine holes, and an aluminum anodic oxide film having a thin barrier layer film was formed.
  • an aluminum substrate on which an aluminum anodized film is formed is used as a cathode and a carbon plate is used as an anode in a treatment solution having a bath temperature of about 20 ° C. and a sulfuric acid concentration of about 15% by volume.
  • a voltage to the cathode hydrogen gas was generated between the aluminum substrate and the aluminum anodized film, and the aluminum anodized film was peeled from the aluminum substrate.
  • the peeled aluminum anodic oxide film was immersed in 5 volume% phosphoric acid liquid, the barrier layer film was removed, and the alumite membrane filter which has the fine hole penetrated was obtained.
  • a test body of the obtained alumite membrane filter (test body size: 40 ⁇ 10 mm, thickness: 85 ⁇ m) was prepared, and this test body was heat-treated at temperatures of 800 ° C., 900 ° C., 1100 ° C., and 1200 ° C.
  • the amount of strain of the specimen at each heat treatment temperature was measured.
  • the amount of strain is a value obtained by fixing one end of the test body to the surface of the desk and measuring the length from the surface of the desk to the other end of the test body. The results are shown in Table 2.
  • An alumite membrane filter was produced in the same manner as in Example 1 except that the aluminum base material having the composition B in Table 1 was used, and the Mg component and the strain amount were similarly examined. The results are shown in Table 2.
  • An alumite membrane filter was produced in the same manner as in Example 1 except that the aluminum base material having the composition C in Table 1 was used, and the Mg component and the strain amount were similarly examined. The results are shown in Table 2.
  • Example 2 After chemically polishing the aluminum substrate having the composition B of Table 1, the aluminum substrate chemically polished in a treatment solution having a bath temperature of about 20 ° C. and a phosphoric acid concentration of about 5% by mass was immersed as an anode.
  • a treatment solution having a bath temperature of about 20 ° C. and a phosphoric acid concentration of about 5% by mass was immersed as an anode.
  • an alumite membrane filter was manufactured in the same manner as in Example 1 except that a carbon plate was immersed, a voltage of about 100 V was applied to the anode and the cathode, and fine pores were formed in the aluminum anodized film. The amount was investigated. The results are shown in Table 2.
  • An alumite membrane filter was produced in the same manner as in Example 1 except that an aluminum substrate having the composition D in Table 1 was used, and the Mg component and the strain amount were measured in the same manner. The results are shown in Table 2.
  • An alumite membrane filter was produced in the same manner as in Example 4 except that the aluminum base material having the composition D in Table 1 was used, and the Mg component and the amount of strain were measured in the same manner. The results are shown in Table 2.
  • composition D is the same composition as aluminum having a purity of 99.99%.
  • the unit of Mg is mass%, and the unit of strain is mm.
  • the alumite membrane filter of the present invention had a smaller distortion amount than the alumite membrane filter not containing Mg at a heat treatment temperature of 800 ° C. Moreover, although the alumite membrane filter not containing Mg was cracked at a heat treatment temperature of 900 ° C. or higher, the alumite membrane filter of the present invention was not cracked at all.
  • Example 4 and Comparative Example 2 even in an alumite membrane filter prepared with another electrolyte, the product of the present invention had a smaller strain than an alumite membrane filter containing no Mg at a heat treatment temperature of 800 ° C. .
  • the alumite membrane filter not containing Mg was cracked at a heat treatment temperature of 900 ° C. or higher, the alumite membrane filter of the present invention was not cracked at all. This is presumably because magnesia spinel (MgAl 2 O 4 ) is generated because the aluminum anodized film constituting the alumite membrane filter of the present invention contains Mg and is heated.
  • MgAl 2 O 4 magnesia spinel
  • the anodized membrane filter of the present invention is made of an aluminum anodic oxide film having fine pores, and the composition thereof includes Mg. That is, the composition is mass%, and Mg: 0.01% to 5%. Unlike the alumite membrane filter made from aluminum with a purity of 99.99%, cracks do not occur even when heated at high temperatures because the film is 0.0% and the balance is Al, O and inevitable impurities. Therefore, the alumite membrane filter of the present invention is excellent in heat resistance.
  • the method for producing an alumite membrane filter according to the present invention can produce an anodized membrane filter having excellent heat resistance.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Optics & Photonics (AREA)
  • Manufacturing & Machinery (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)

Abstract

L'invention concerne un filtre à membrane en alumite comprenant un film d'oxyde anodique d'aluminium comprenant des trous traversants fins formés dans celui-ci, le film d'oxyde comprenant de l'Al, de l'O et du Mg, le reste étant constitué d'impuretés inévitables. Lorsque le filtre à membrane en alumite est chauffé, l'Al2O3 prend la forme de α-Al2O3, γ-Al2O3 ou d'un mélange de α-Al2O3 et γ-Al2O3. Lorsque le filtre à membrane en alumite est chauffé, le filtre à membrane en alumite se compose de MgAl2O4.
PCT/JP2010/051857 2010-02-09 2010-02-09 Filtre à membrane en alumite et procédé de production d'un filtre à membrane en alumite WO2011099115A1 (fr)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2018145477A (ja) * 2017-03-06 2018-09-20 栗田工業株式会社 金属材表面の酸化皮膜を除去する方法
JP2021113346A (ja) * 2020-01-20 2021-08-05 東洋アルミニウム株式会社 ポーラスアルミナシートおよびその製造方法

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6171804A (ja) * 1984-09-17 1986-04-12 Toyo Soda Mfg Co Ltd 多孔性酸化アルミニウム膜
JPS62129106A (ja) * 1985-12-02 1987-06-11 Fuji Electric Co Ltd アルミニウムフイルタ−
JPH02149698A (ja) * 1988-10-05 1990-06-08 Alcan Internatl Ltd 陽極酸化アルミニウム膜の耐薬品性向上方法
JP2005232487A (ja) * 2004-02-17 2005-09-02 Kanagawa Acad Of Sci & Technol 陽極酸化ポーラスアルミナおよびその製造方法
WO2006134737A1 (fr) * 2005-06-17 2006-12-21 Tohoku University Film d'oxyde metallique, lamine, element en metal et son procede de fabrication
JP2009074133A (ja) * 2007-09-20 2009-04-09 Fujifilm Corp 微細構造体

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6171804A (ja) * 1984-09-17 1986-04-12 Toyo Soda Mfg Co Ltd 多孔性酸化アルミニウム膜
JPS62129106A (ja) * 1985-12-02 1987-06-11 Fuji Electric Co Ltd アルミニウムフイルタ−
JPH02149698A (ja) * 1988-10-05 1990-06-08 Alcan Internatl Ltd 陽極酸化アルミニウム膜の耐薬品性向上方法
JP2005232487A (ja) * 2004-02-17 2005-09-02 Kanagawa Acad Of Sci & Technol 陽極酸化ポーラスアルミナおよびその製造方法
WO2006134737A1 (fr) * 2005-06-17 2006-12-21 Tohoku University Film d'oxyde metallique, lamine, element en metal et son procede de fabrication
JP2009074133A (ja) * 2007-09-20 2009-04-09 Fujifilm Corp 微細構造体

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2018145477A (ja) * 2017-03-06 2018-09-20 栗田工業株式会社 金属材表面の酸化皮膜を除去する方法
JP2021113346A (ja) * 2020-01-20 2021-08-05 東洋アルミニウム株式会社 ポーラスアルミナシートおよびその製造方法
JP7426835B2 (ja) 2020-01-20 2024-02-02 東洋アルミニウム株式会社 ポーラスアルミナシートおよびその製造方法

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