WO2018043603A1 - Procédé de production d'un corps poreux en aluminium - Google Patents

Procédé de production d'un corps poreux en aluminium Download PDF

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Publication number
WO2018043603A1
WO2018043603A1 PCT/JP2017/031262 JP2017031262W WO2018043603A1 WO 2018043603 A1 WO2018043603 A1 WO 2018043603A1 JP 2017031262 W JP2017031262 W JP 2017031262W WO 2018043603 A1 WO2018043603 A1 WO 2018043603A1
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Prior art keywords
producing
precursor
phase
aluminum
capacitor
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PCT/JP2017/031262
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English (en)
Japanese (ja)
Inventor
雅司 坂口
小沼　博
西森　秀樹
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Resonac Holdings Corp
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Showa Denko KK
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/08—Alloys with open or closed pores

Definitions

  • the present invention relates to a method for producing an aluminum porous body suitably used as a material for an electrode material in, for example, an aluminum electrolytic capacitor or an aluminum solid electrolytic capacitor, and related technology.
  • Aluminum electrolytic capacitors and aluminum solid electrolytic capacitors are widely used for home appliances such as personal computers and television sets and on-vehicle electrical products because they are relatively inexpensive and have a high capacity.
  • An aluminum electrolytic capacitor is generally manufactured by winding an anode foil and a cathode foil with a separator interposed therebetween to form a capacitor element, impregnating the capacitor element with an electrolytic solution, storing the case in a case, and sealing. ing.
  • an anode foil is subjected to a surface expansion treatment by chemical or electrochemical etching on a valve action metal foil such as aluminum, and an oxide film layer is formed by subjecting the surface of the surface expansion treatment to chemical conversion. Is formed.
  • Patent Document 4 for the purpose of significantly increasing the capacity of an aluminum electrolytic capacitor, as shown in Patent Document 4, as shown in Patent Document 4, in order to arrange the etching positions regularly, the technique of injecting the powder of valve action metal onto the anode foil is shown in Patent Document 5.
  • Patent Document 6 A technique using a printing method and a technique using lithography as shown in Patent Document 6 have been proposed.
  • any of the techniques in Patent Documents 4 to 6 has a problem such as high cost. Not reached.
  • An object of the present invention is to provide a method for producing a porous aluminum body and its related technology capable of greatly improving the capacitance when used as an anode body of a capacitor.
  • an aluminum alloy cast body having a solidified structure having an ⁇ -Al phase and a second phase formed in a continuous manner with the ⁇ -Al phase is produced as a precursor.
  • Process By contacting the precursor with an eluent that dissolves the second phase, the second phase of the solidified tissue in the precursor is eluted to produce an aluminum porous body having a large number of voids communicating from the surface to the inside.
  • the aluminum alloy as a precursor is composed of an Al—X alloy in which “X” as an additive component is added to “Al” as a main component, “X” is an element that exhibits a eutectic reaction with respect to “Al”, and an Al—X alloy as a precursor has a hypoeutectic composition in which the amount of “X” added is less than the eutectic point on an Al basis.
  • an aluminum alloy cast body having a solidified structure having an ⁇ -Al phase and a second phase formed in a continuous manner with the ⁇ -Al phase is produced as a precursor.
  • Process By contacting the precursor with an eluent that dissolves the second phase, the second phase of the solidified tissue in the precursor is eluted to produce an aluminum porous body having a large number of voids communicating from the surface to the inside.
  • the aluminum alloy as a precursor is composed of an Al—X alloy in which “X” as an additive component is added to “Al” as a main component, “X” is an element that exhibits a eutectic reaction with respect to “Al”, and an Al—X alloy as a precursor has a hypoeutectic composition in which the amount of “X” added is less than the eutectic point on an Al basis.
  • Capacitor electrode material characterized in that a capacitor electrode material is manufactured by subjecting the porous aluminum body obtained by the manufacturing method according to any one of items 1 to 8 to a chemical conversion treatment. Manufacturing method.
  • a method for manufacturing a capacitor characterized in that a capacitor is manufactured using the capacitor electrode material obtained by the manufacturing method according to any one of items 9 to 16.
  • a method for manufacturing a capacitor characterized in that a capacitor is manufactured using the capacitor electrode material obtained by the manufacturing method according to item 17 above as an anode material.
  • an aluminum porous body having a sufficient surface area can be obtained easily and at low cost.
  • the porous body thus obtained is used as the anode body of an aluminum capacitor, the capacitance can be greatly improved.
  • the residual amount in the porous body of the component added to aluminum when casting an aluminum alloy cast body as a precursor for obtaining the porous body can be reduced.
  • FIG. 1 is an optical micrograph showing a cross section of a solidified structure in an aluminum porous body obtained in an example of the present invention.
  • an aluminum electrolytic capacitor is formed by sandwiching a dielectric film made of aluminum oxide formed on an anode material made of aluminum between an anode and a cathode facing the anode.
  • porous aluminum body of the present invention As an anode material, a dielectric film is formed on the anode material, and a separator infiltrated with an electrolyte solution serving as a cathode is placed on the dielectric film, whereby an aluminum electrolytic capacitor is obtained. Can be formed.
  • the separator may not be used depending on the structure of the capacitor.
  • a known separator such as a porous cellulose membrane can be used as the separator.
  • the electrolytic solution generally comprises a cation component, an anion component, and a solvent.
  • the anion component include weak acids such as boric acid and carboxylic acid
  • examples of the cation component include organic bases such as ammonia and amines.
  • examples of the solvent include ethylene glycol and ⁇ -butyrolactone.
  • a conventional surface-expanded Al foil or the like can be used.
  • the anode material obtained by the present invention is composed of an aluminum porous body (porous material).
  • This aluminum porous body has an aluminum alloy cast body formed by casting solidification as a precursor. Then, by eluting (etching) a required portion of the precursor, an aluminum porous body having a large number of voids (pores) open to the surface and communicating from the surface to the inside is obtained.
  • An aluminum alloy as a precursor is expressed as an Al—X alloy in which “X” as an additive component (additive element) is added to Al (aluminum) as a main component (main element) as described later. it can.
  • the solidification structure of the precursor has an ⁇ phase composed of primary crystals (that is, an ⁇ -Al phase) and a second phase having a eutectic formed continuously with the ⁇ phase.
  • the primary crystal refers to a crystal that is first formed from a molten metal during casting solidification.
  • the second phase has a eutectic of Al and the additive element “X”. The second phase is virtually all connected. However, the isolated second phase may remain as long as the effects of the present invention are not impaired.
  • the casting method for obtaining the precursor is not particularly limited, and may be casting into a mold or continuous casting method.
  • a continuous casting method for example, a DC casting method, a horizontal continuous casting method, an electromagnetic field casting method, a roll type continuous casting method, a belt casting method, or the like can be applied.
  • a directional solidification casting method can be suitably used as casting for obtaining a precursor.
  • a precursor having a uniform structure can be obtained, and a porous body having a large surface area can be obtained by elution of the second phase of the precursor.
  • the unidirectional solidification casting method it is preferable to apply the unidirectional solidification casting method.
  • the porous body having a large surface area is more reliably obtained by leaving the ⁇ -Al phase of the precursor having a structure extending in one direction and dissolving the second phase with the eluent. Is obtained.
  • the unidirectional solidification casting method is not particularly limited.
  • continuous casting in which the ingot surface is solidified right outside the mold outlet end using a heating mold.
  • Reference 2 a closed mold placed on a cooling plate is filled with molten metal without voids, and the molten metal is unidirectionally solidified by cooling from the cooling plate, Reference 3, a twin roll continuous casting method or the like can be applied.
  • the content (mass%) of the additive component “X” in the second phase is the content in the ⁇ phase. More than
  • the additive component “X” When the precursor is brought into contact with a solution that dissolves the additive component “X”, the additive component “X” is preferentially eluted, and as a result, the ⁇ phase remains and at least a part, preferably all, of the second phase remains.
  • a large number of continuous voids (pores) are formed in the precursor from the surface to the inside, and the porous aluminum body of the present embodiment is obtained.
  • Mg can be suitably used because it has a melting point close to that of Al.
  • the additive component “X” is not limited to one type, and two or more types may be added.
  • the Al—X-based alloy constituting the precursor can be regarded as having a hypoeutectic composition with an Al-based addition amount of “X” below the eutectic point.
  • an Al-rich alloy phase is crystallized inside the solidification cell constituting the ⁇ phase, while being added to the final solidification portion of the solidification cell formed on the outer periphery of the ⁇ phase. Since the alloy phase (second phase) containing a large amount of the component “X” is crystallized, the second phase is preferentially eluted by the eluent. Therefore, a desired gap can be formed reliably.
  • the ⁇ phase may also be eluted slightly, but this is not a problem as long as a continuous void is formed and the shape of the porous body is maintained.
  • the precursor has a hypereutectic composition in which the addition amount of “X” exceeds the eutectic point, a crystallized product whose primary crystal is composed of the additive component “X” or an alloy containing a large amount of the additive component “X” Since it becomes a crystallized product of the phase, many parts of the primary crystal are eluted by the eluent. In this case, the voids are too large, and the surface area cannot be sufficiently expanded or the porous structure cannot be maintained.
  • an element other than “X” may be added to the Al—X-based alloy as the precursor within the range of the eutectic composition as necessary or unavoidable.
  • the general addition amount of “X” in the precursor is not more than the eutectic composition and is 1% by mass or more, desirably 5% by mass or more, and more desirably 10% by mass or more. That is, when “X” is added in this amount, as described above, an alloy phase containing a large amount of the additive component “X” crystallizes on the outer periphery of the ⁇ phase. When the preferential elution is performed and the second phase is eluted, a porous structure having a desired void can be formed.
  • the eutectic composition in the present invention is 35% by mass with the smallest amount of Mg in the phase diagram in the case of an Al—Mg alloy, and 36% by mass in the case of an Al—Zn alloy.
  • the surface area can be increased as the solidification cell composed of the ⁇ phase during casting is smaller. Therefore, it is preferable to reduce the solidification cell during casting solidification.
  • the cooling rate in the vicinity of the freezing point may be adjusted to 1 ° C./sec or higher, preferably 5 ° C./sec or higher, more preferably 10 ° C./sec or higher.
  • dendrites in at least a part of the ⁇ -phase solidification cell, and it is more preferable to form all of them into dendrites.
  • the primary ⁇ phase 1 (the light gray portion in the figure) is composed of dendritic crystals, and between the ⁇ phases 1,
  • the void 2 (the dark gray portion in the figure) formed by the elution of the second phase is continuously formed.
  • the photograph in FIG. 1 is a porous body based on an aluminum alloy casting obtained by a continuous casting method using a heating mold, and an axial cross section of the aluminum alloy casting is observed. It is a thing.
  • the precursor may be subjected to a drawing process or a rolling process for shaping the outer shape.
  • the precursor is processed with a high deformation rate, the solidified structure collapses, and the crystallized product as the second phase is divided, and when the crystallized product is eluted, the porous material has a desired void. There is a possibility that the structure cannot be obtained.
  • the surface of the precursor may be left as it is or may be cut to a size that facilitates the next process. Further, the cast solidified surface may be cut (deleted) so that the etching (elution) of the second phase can be performed quickly and uniformly.
  • the additive component “X” in order to reduce the residual amount of “X” in the porous body, heat treatment is performed in a process after the aluminum alloy cast body is manufactured. By this heat treatment, “X” evaporates, and the residual amount of “X” in the porous body finally obtained can be reduced.
  • the atmosphere of the heat treatment is preferably performed in a vacuum in order to promote evaporation of “X”.
  • the degree of vacuum in the heat treatment in vacuum is preferably 0.1 Pa or less, more preferably 1 ⁇ 10 ⁇ 2 Pa or less, and particularly preferably 5 ⁇ 10 ⁇ 3 Pa or less.
  • the heat treatment is a temperature at which “X” evaporates in the heat treatment atmosphere, and is preferably 550 ° C. or less. If the heat treatment temperature is too low, “X” does not evaporate, and if the heat treatment temperature is too high, the aluminum surface is oxidized inhomogeneously.
  • the heat treatment temperature is preferably from 400 ° C. to 550 ° C., more preferably from 450 ° C. to 550 ° C.
  • an acid aqueous solution can be exemplified as an eluent for dissolving the additive component “X” of the precursor.
  • an acid contained in the acid aqueous solution hydrochloric acid, sulfuric acid, nitric acid and the like can be used.
  • the heat treatment when the heat treatment is performed in a state where the additive component “X” is dissolved from the precursor and the area is expanded, evaporation of “X” is promoted. Therefore, the heat treatment is performed by contact with the eluate. It is preferable to carry out after dissolution of “X”.
  • the precursor may be made into a porous body by performing at least one of contact with the eluate and heat treatment a plurality of times.
  • the contact with the eluate is performed after the first contact with the eluate, heat treatment is performed, and then the second eluate is contacted. If it is possible, the second contact with the eluate may be performed in such a short time that the oxide film can be removed.
  • An aluminum porous body obtained by treating the precursor with an eluent can be used as a capacitor electrode material.
  • a dielectric coating is formed on the anode body.
  • the method for forming the dielectric film is not particularly limited, but it is preferable to apply a chemical conversion treatment by anodic oxidation.
  • Hydration treatment is generally performed in pure water as pre-chemical treatment.
  • Other pretreatment methods include immersion in hydrogen peroxide, cleaning with an acid or alkaline treatment solution, vacuum or atmospheric heat treatment, dechlorination treatment, hydration treatment in an aqueous solution to which an amine is added, thermal oxide film It can be applied alone or in combination from known pretreatment methods including treatment with an acid or alkali solution after formation, and hydration treatment performed after electrolytic etching is applied to the aluminum foil.
  • the chemical conversion treatment solution known ones can be used, and examples include aqueous solutions in which one or more of boric acid, ammonium borate, adipic acid, ammonium adipate, phosphoric acid and its salt, citric acid and its salt, etc. are mixed. it can.
  • the EIAJ method can be exemplified, but is not limited thereto.
  • the chemical conversion treatment may be performed a plurality of times, the chemical conversion liquid may be changed for each chemical conversion treatment according to a known method, and heat treatment or washing may be performed between the chemical conversion treatment and the chemical conversion treatment.
  • the conversion voltage may be set to different values in a plurality of conversion processes.
  • the precursor may be formed in any shape such as a columnar shape, a cylindrical shape, an elliptical columnar shape, an elliptical cylindrical shape, a prismatic shape, a rectangular cylindrical shape, a flat shape such as a plate shape, and the like.
  • a columnar shape a cylindrical shape, an elliptical columnar shape, an elliptical cylindrical shape, a prismatic shape, a rectangular cylindrical shape, a flat shape such as a plate shape, and the like.
  • a flat shape such as a plate shape, and the like.
  • an aluminum electrolytic capacitor can be formed by sequentially laminating and placing a semiconductor layer and a conductor layer on the dielectric coating.
  • the semiconductor layer can be formed of an inorganic semiconductor such as manganese dioxide or an organic semiconductor such as a conductive polymer, and these can be generally produced by a known method. In the case of forming with a conductive polymer, it can be formed using, for example, a chemical polymerization method and / or an electrolytic polymerization method.
  • the solution for forming the semiconductor layer is not particularly limited as long as the solution can form a semiconductor by dipping and / or energization. For example, a solution containing aniline, thiophene, pyrrole, and substituted derivatives thereof (for example, 3,4-ethylenedioxythiophene) can be used. Further, a dopant may be added to this solution.
  • arylsulfonic acid or its salt alkylsulfonic acid or its salt, various polymeric sulfonic acid or its salt, etc.
  • conductive polymer for example, polyaniline, polythiophene, polypyrrole, polymethylpyrrole, and derivatives thereof
  • a semiconductor layer can be formed.
  • the conductor layer can be made of, for example, highly conductive carbon or silver, and can be produced by solidifying pasty carbon or silver. These may be laminated.
  • Example 1 Using a molten 670 ° C. alloy having the composition shown in Table 1 and passing it through a heated mold as shown in Table 2 at a casting rate of 150 mm ⁇ min ⁇ 1 , cooling at a cooling rate of 100 ° C./sec or more, A cylindrical (round bar) aluminum alloy casting having a diameter of 12 mm was obtained. As shown in Table 3, the cast body was cut to a thickness of 1.0 mm perpendicularly in the axial direction, degreased with ethanol, immersed in a 5N hydrochloric acid solution at a liquid temperature of 10 ° C. for 24 hours, and in vacuum (1 Heat treatment at 500 ° C.
  • Example 1 An aluminum porous body of Example 1.
  • the mass reduction rate of the cast body by the first immersion in the eluate was 28%.
  • the specific surface area was 0.50 m 2 / g, and the ratio of pores of 1 ⁇ m or more and 10 ⁇ m or less was 90% or more of all pores in terms of volume. It was.
  • the obtained aluminum porous body was immersed in pure water in a boiling state for 5 minutes for chemical conversion pretreatment.
  • the aluminum porous body subjected to the chemical conversion pretreatment was immersed in 11 L of pure water to which 1100 g of boric acid and 9.9 g of ammonium pentaborate octahydrate were added, and the initial current value was 500 mA / cm 2 at 90 ° C., constant voltage. Chemical conversion treatment was carried out by holding at 150 V for 10 minutes.
  • the aluminum porous body subjected to chemical conversion treatment is immersed in 360 ml of pure water to which 28.8 g of ammonium pentaborate octahydrate is added, and below the surface of the stainless steel container (area: bottom diameter 60 mm ⁇ height 150 mm)
  • As a counter electrode 30 ° C., measurement frequency 120 Hz, measurement voltage 0.5 Vr. m. s.
  • the capacitance measurement was performed, it was 80 ⁇ F.
  • Examples 2 to 7, Comparative Example 1 As shown in Table 2, the molten alloy of the composition shown in Table 1 is cast by the heating mold type continuous casting method in Examples 2 to 5, and in Examples 6 and 7 and Comparative Example 1, casting into the mold is performed. To obtain cylindrical (round bar) aluminum alloy castings. In addition, the temperature of the casting_mold
  • FIG. 1 shows an optical micrograph of a cross-section of a solidified structure in the precursor of the porous aluminum body of Example 5.
  • ⁇ -phase 1 of the primary crystal (light gray portion in the figure) is formed in dendritic crystals, and is formed by elution of the second phase between the ⁇ -phases 1.
  • the void 2 (the dark gray portion in the figure) is continuously formed.
  • the ratio of pores of 1 ⁇ m or more and 10 ⁇ m or less was 90% or more of the total pores in terms of volume. It was confirmed by blowing air into the porous body in water that the aluminum porous body penetrated in the axial direction.
  • porous bodies of Examples 2 to 7 obtained by performing the heat treatment had less residual Mg than the porous body of Comparative Example 1 that was not subjected to the heat treatment.
  • the ⁇ -Al phase and the ⁇ -Al phase are intricately and continuously formed by the directional solidification casting of the aluminum alloy.
  • An aluminum alloy cast body with a solidified structure having a phase is manufactured as a precursor, and the cast body is brought into contact with the eluate to elute the second phase of the solidified structure, while heat treatment is performed in the process after the precursor is manufactured.
  • an aluminum porous body having a large number of voids communicating from the surface to the inside can be formed, and it can be used as an electrode material having a high electrostatic capacity.
  • the residual amount in the porous body of the component added to aluminum when casting an aluminum alloy casting as a precursor for obtaining a porous body can be reduced.
  • the method for producing an aluminum porous body of the present invention can be suitably used when producing an anode material for an aluminum electrolytic capacitor or an aluminum solid electrolytic capacitor.
  • phase 2 void

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
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  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
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Abstract

L'invention concerne un procédé de production d'un corps poreux en aluminium présentant une grande surface. Le procédé de production d'un corps poreux en aluminium selon la présente invention comprend : une étape consistant à produire, en tant que précurseur, un corps coulé en alliage d'aluminium présentant une structure solidifiée doté d'une phase 1 d'α-Al et d'une deuxième phase formée en continu et de manière intriquée avec la phase d'α-Al, par solidification du produit coulé d'un alliage d'aluminium ; une étape consistant à produire un corps poreux en aluminium présentant un grand nombre de vides 2 dont les intérieurs sont reliés à la surface, par mise en contact du précurseur avec un éluant pour dissoudre la deuxième phase et à éluer ainsi la deuxième phase de la structure solidifiée dans le précurseur ; et une étape consistant à effectuer un traitement thermique après l'étape de production du précurseur.
PCT/JP2017/031262 2016-09-02 2017-08-30 Procédé de production d'un corps poreux en aluminium Ceased WO2018043603A1 (fr)

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JP2016172146A JP2018035432A (ja) 2016-09-02 2016-09-02 アルミニウム多孔質体の製造方法
JP2016-172146 2016-09-02

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001006985A (ja) * 1999-06-17 2001-01-12 Showa Alum Corp 電解コンデンサ電極用アルミニウム箔の製造方法
JP2009170618A (ja) * 2008-01-16 2009-07-30 Sanyo Electric Co Ltd コンデンサの製造方法及びコンデンサ
JP2011249175A (ja) * 2010-05-28 2011-12-08 Honda Foundry Co Ltd マグネシウム電池用電極材料とその製造方法、および該電極材料を用いた電極を用いる電池

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001006985A (ja) * 1999-06-17 2001-01-12 Showa Alum Corp 電解コンデンサ電極用アルミニウム箔の製造方法
JP2009170618A (ja) * 2008-01-16 2009-07-30 Sanyo Electric Co Ltd コンデンサの製造方法及びコンデンサ
JP2011249175A (ja) * 2010-05-28 2011-12-08 Honda Foundry Co Ltd マグネシウム電池用電極材料とその製造方法、および該電極材料を用いた電極を用いる電池

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