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WO2018139072A1 - Composition d'agent de gravure électrolytique, procédé de gravure électrolytique, substrat gravé par électrolyse, matériau d'électrode pour condensateurs électrolytiques en aluminium et condensateur - Google Patents

Composition d'agent de gravure électrolytique, procédé de gravure électrolytique, substrat gravé par électrolyse, matériau d'électrode pour condensateurs électrolytiques en aluminium et condensateur Download PDF

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Publication number
WO2018139072A1
WO2018139072A1 PCT/JP2017/044281 JP2017044281W WO2018139072A1 WO 2018139072 A1 WO2018139072 A1 WO 2018139072A1 JP 2017044281 W JP2017044281 W JP 2017044281W WO 2018139072 A1 WO2018139072 A1 WO 2018139072A1
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WO
WIPO (PCT)
Prior art keywords
electrolytic
aluminum
electrolytic etching
base material
mass
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/JP2017/044281
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English (en)
Japanese (ja)
Inventor
鈴木　陽介
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Adeka Corp
Original Assignee
Adeka Corp
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Filing date
Publication date
Application filed by Adeka Corp filed Critical Adeka Corp
Publication of WO2018139072A1 publication Critical patent/WO2018139072A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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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
    • C25F3/02—Etching
    • C25F3/04—Etching of light metals
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
    • H01G9/004—Details
    • H01G9/04—Electrodes or formation of dielectric layers thereon

Definitions

  • the present invention relates to an electrolytic etching solution composition used for forming pits by electrochemical etching on a substrate containing aluminum.
  • the present invention also provides an electrolytic etching method using the electrolytic etching solution composition, a base material electrolytically etched using the electrolytic etching solution composition, and an aluminum electrolytic capacitor manufactured using the base material.
  • the present invention relates to an electrode material and a capacitor.
  • a base material containing aluminum is used as an electrode material for an aluminum electrolytic capacitor.
  • an effective area of a base material containing aluminum is increased by performing an electrochemical or chemical etching treatment.
  • Patent Document 1 discloses an aqueous solution containing chlorine ions, an aqueous solution containing chlorine ions and sulfate ions, and an aqueous solution containing nitrate ions or chlorine ions as an electrolytic etching solution used in the method for etching an aluminum foil for electrolytic capacitors. ing.
  • Patent Document 2 discloses an aqueous solution containing hydrochloric acid and sulfuric acid as an etching solution used in the method for producing an aluminum foil for electrolytic capacitors.
  • an object of the present invention is to provide an electrolytic etching solution composition that is suitable as an electrode material for an aluminum electrolytic capacitor and that can produce a substrate having a large capacitance and containing aluminum.
  • the present invention also provides an electrolytic etching method using the above electrolytic etching solution composition.
  • the present invention intends to provide a base material electrolytically etched with the above electrolytic etching solution composition, and an electrode material and a capacitor for an aluminum electrolytic capacitor manufactured using the base material subjected to the electrolytic etching. .
  • the inventors of the present invention contain an aluminum having a large electrostatic capacity suitable as an electrode material for an aluminum electrolytic capacitor by an electrolytic etching solution composition containing a specific component in an amount within a specific range. It was found that a base material to be obtained was obtained, and the present invention was achieved.
  • the present invention is an electrolytic etchant composition used to form pits in the substrate by electrochemically etching the substrate containing aluminum, and is selected from the group consisting of acetic acid and lactic acid
  • An electrolytic etching solution composition containing at least one of a total of 10 to 70% by mass, aluminum chloride of 0.1 to 10% by mass, and water is provided.
  • the present invention also provides an electrolytic etching method including a step of electrochemically etching a base material containing aluminum using the electrolytic etching solution composition.
  • the present invention provides a substrate in which an aluminum-containing substrate is electrolytically etched with the electrolytic etching solution composition, and an electrode material for an aluminum electrolytic capacitor and a capacitor manufactured using the electrolytically etched substrate. provide.
  • an electrolytic etching solution composition that is suitable as an electrode material for an aluminum electrolytic capacitor and that can produce a substrate having a large capacitance and containing aluminum.
  • the electrolytic etching method using the said electrolytic etching liquid composition can be provided.
  • the electrolytic etching solution composition of one embodiment of the present invention is used for electrochemically etching a base material containing aluminum to form pits on the base material.
  • the “base material containing aluminum” may contain aluminum, and its shape is not limited. Suitable materials for the base material include, for example, pure aluminum (aluminum having a purity of 99% or more), an aluminum alloy mainly composed of aluminum, and the like. As a shape of a base material, foil, a board, a molded object provided with these, etc. can be mentioned, for example.
  • the “pit” in the present specification includes a hole and a hole, and does not ask for penetration or non-penetration, and its shape is not limited.
  • the electrolytic etching solution composition of one embodiment of the present invention contains at least one selected from the group consisting of acetic acid and lactic acid in total 10 to 70% by mass, aluminum chloride 0.1 to 10% by mass, and water. .
  • the concentration of at least one selected from the group consisting of acetic acid and lactic acid in the electrolytic etching solution composition is 10 to 70% by mass in total.
  • the concentration of at least one of acetic acid and lactic acid is preferably 30 to 60% by mass in total because the effect of increasing the capacitance of the substrate is high, and is preferably 40 to 60% by mass in total. More preferably, the total amount is more preferably 45 to 55% by mass.
  • acetic acid and lactic acid it is preferable to use acetic acid as an essential component, and it is more preferable to use only acetic acid because the effect of increasing the capacitance of the substrate is high.
  • the concentration of aluminum chloride in the electrolytic etching solution composition is 0.1 to 10% by mass. Since the linear pits can be formed on the substrate and the effect of increasing the capacitance is high, the concentration of aluminum chloride is preferably 0.3 to 8% by mass, and 0.3 to 5% by mass. % Is more preferable, and 0.5 to 2% by mass is even more preferable.
  • the electrolytic etching solution composition of one embodiment of the present invention contains water as an essential component in addition to at least one of acetic acid and lactic acid and aluminum chloride.
  • This electrolytic etching solution composition is preferably an aqueous solution containing at least one of acetic acid and lactic acid, and aluminum chloride in a concentration in the specific range described above.
  • the content of water in the electrolytic etching solution composition is preferably 20% by mass or more and less than 90% by mass, more preferably 30% by mass or more and less than 70% by mass, and more preferably 30% by mass or more and less than 60% by mass. More preferably, it is 40 mass% or more and less than 55 mass%.
  • the electrolytic etching solution composition of one embodiment of the present invention can contain other additives as necessary within a range not impairing the object of the present invention.
  • other additives include stabilizers, antifoaming agents, pH adjusting agents, specific gravity adjusting agents, viscosity adjusting agents, wettability improving agents, chelating agents, oxidizing agents, reducing agents, and surfactants. be able to.
  • One or more of these additives can be used.
  • the content of other additives in the electrolytic etching solution composition is preferably 0.01 to 10% by mass per one type of additive.
  • the shape of the pit formed on the substrate by the electrolytic etching solution composition of one embodiment of the present invention can be changed depending on the configuration and conditions of the electrolytic etching solution composition. For example, when a pit having a pit diameter or diagonal length of 1 nm to 10 ⁇ m is formed, a substrate having a large capacitance can be obtained, and the pit diameter or diagonal length is preferably 100 nm to 5 ⁇ m. The range is more preferable.
  • the electrolytic etching method of one embodiment of the present invention includes a step of electrochemically etching a base material containing aluminum using the above-described electrolytic etching solution composition. Thereby, a pit can be formed in a base material and, thereby, the effective surface area of a base material can be expanded.
  • the method of electrolytic etching is not particularly limited, and a known electrolytic etching method can be used.
  • the substrate can be electrochemically etched by immersing the substrate in an electrolytic etching bath with an electrolytic etching solution composition and applying a direct current or an alternating current in the electrolytic etching bath.
  • an electrolytic etching bath of the above-described electrolytic etching solution composition can be used, and the temperature of the electrolytic etching bath is preferably in the range of 40 to 90 ° C., and 50 to 80 More preferably, the temperature is in the range of ° C.
  • the current density in electrolytic etching is preferably in the range of 0.01 to 1.0 A / cm 2 , and more preferably in the range of 0.05 to 0.5 A / cm 2 .
  • the electrolytic etching time is preferably in the range of 10 to 3000 seconds, and more preferably in the range of 50 to 500 seconds.
  • the electrolytic etching method of one embodiment of the present invention preferably includes a step of pretreating the surface of the base material before electrochemically etching the base material. In this pretreatment step, degreasing of the surface of the substrate, removal of the natural oxide film, washing, and the like can be performed.
  • the electrolytically etched base material containing aluminum can be manufactured by the electrolytic etching method of one embodiment of the present invention. That is, the base material in which the base material containing aluminum was electrolytically etched with the above-described electrolytic etching solution composition can be provided.
  • This electrolytically etched substrate can be provided with pits formed by electrolytic etching using the aforementioned electrolytic etching solution composition.
  • an electrode material for an aluminum electrolytic capacitor can be manufactured. Specifically, an electrode for an aluminum electrolytic capacitor in which an oxide film is formed on the surface of a base material by electrochemically etching a base material containing aluminum by the above-described electrolytic etching method and then undergoing a chemical conversion treatment step. The material can be manufactured. What is necessary is just to implement the said chemical conversion treatment process on the conditions similar to the general process employ
  • an aqueous solution of ammonium borate, ammonium phosphate, organic acid ammonium, or the like is used as a chemical electrolyte for chemical conversion, and the electrolytically etched base material is immersed in the chemical electrolyte for chemical conversion.
  • An oxide film (aluminum oxide) can be formed.
  • manufacture of a cathode material it is not necessary to perform a chemical conversion treatment.
  • a capacitor can be manufactured by using the above-mentioned electrolytically etched base material.
  • the electrode material for an aluminum electrolytic capacitor described above is manufactured using an electrolytically etched base material, and the aluminum electrolytic capacitor can be manufactured using the electrode material.
  • the manufacturing method of the electrolytic capacitor using the electrode material for aluminum electrolytic capacitors is not particularly limited, and a known method can be used.
  • the capacitor can include an electrode material (anode material and cathode material), an electrolytic solution, electrolytic paper, and the like.
  • Examples 1 to 5 Each component was mixed so that it might become the mixing
  • each component was mixed so as to have the composition shown in Table 2 to produce an electrolytic etching solution composition (comparative compositions 1 to 4).
  • water was mix
  • An aluminum foil (manufactured by UACJ) having a length of 20 mm, a width of 50 mm and a thickness of 0.12 mm was prepared as a base material containing aluminum, which is an object to be subjected to electrolytic etching.
  • This aluminum foil is immersed in a 0.2% by mass hexafluorosilicic acid aqueous solution at 50 ° C. for 60 seconds, then immersed in ultrapure water at 25 ° C. for 60 seconds, and then dried with dry air to obtain a treated aluminum foil A Manufactured.
  • Example 6 ⁇ Electrolytic etching method> (Example 6) To the treated aluminum foil A, an electrolytic etching power source (trade name “HA-151B”, manufactured by Hokuto Denshi Kogyo Co., Ltd.) and Example Composition No. Using the electrolytic etching bath No. 1, electrochemical etching was carried out under the conditions of 0.2 A / cm 2 , 75 ° C., and 300 seconds. Thus, the aluminum foil (Example aluminum foil No. 1) by which the electrolytic etching was performed and the pit was formed was manufactured.
  • an electrolytic etching power source trade name “HA-151B”, manufactured by Hokuto Denshi Kogyo Co., Ltd.
  • Example 7 to 10 Example Composition No. used in Example 6 was used. In place of Example No. 1, Example Composition No. Except that 2 to 5 were used, aluminum foil (Example aluminum foil Nos. 2 to 5) in which pits were formed by electrolytic etching was manufactured in the same manner as in Example 6.
  • Comparative Examples 5 to 8 In Comparative Examples 5 to 8, the Example Composition No. used in Example 6 was used. In the same manner as in Example 6 except that Comparative Compositions 1 to 4 were used instead of Comparative Example 1 to produce aluminum foils (Comparative Aluminum Foil 1 to 4) that were electrolytically etched to form pits, respectively. did.
  • Example Aluminum foil No. 1 using an aqueous solution in which 5% by mass of nitric acid and 0.5% by mass of boric acid were dissolved, and an electrolytic etching power source (trade name “HA-151B”, manufactured by Hokuto Denshi Kogyo Co., Ltd.), 0.1 A / cm 2 After-treatment was performed at 60 ° C. for 600 seconds.
  • Example 12 to 15 In Examples 12 to 15, the Example aluminum foil No. used in Example 11 was used. In place of Example 1, aluminum foil No. Except that 2 to 5 were used, electrode materials for aluminum electrolytic capacitors (aluminum foils Nos. 2 to 5 for evaluation of examples) were produced in the same manner as in Example 11.
  • Comparative Examples 9-12 In Comparative Examples 9 to 12, the Example aluminum foil No. 1 used in Example 11 was used. An electrode material for an aluminum electrolytic capacitor (comparative evaluation aluminum foils 1 to 4) was produced in the same manner as in Example 11 except that comparative aluminum foils 1 to 4 were used instead of 1, respectively.
  • the aluminum foil No. for Example evaluation obtained in Examples 11 to 15 was used. It was confirmed that the electrostatic capacities of 1 to 5 were 1.2 times or more of the electrostatic capacity of the comparative evaluation aluminum foil 1 obtained in Comparative Example 9. Especially, aluminum foil No. for Example evaluation obtained in Examples 13 and 14 was used. The capacitances of Nos. 3 and 4 were greatly increased, and among them, the aluminum foil No. 1 for Example evaluation obtained in Example 14 was used. It was confirmed that the capacitance of 4 increased particularly.

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  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • ing And Chemical Polishing (AREA)
  • Electric Double-Layer Capacitors Or The Like (AREA)

Abstract

L'invention concerne une composition d'agent de gravure électrolytique qui est en mesure de produire un substrat contenant de l'aluminium, ledit substrat présentant une capacité électrostatique élevée et étant approprié comme matériau d'électrode pour des condensateurs électrolytiques en aluminium. La présente invention concerne une composition d'agent de gravure électrolytique qui est utilisée dans le but de former un creux dans un substrat qui contient de l'aluminium par réalisation d'une gravure électrochimique. Cette composition d'agent de gravure électrolytique contient 10-70 % en masse, au total, d'au moins un acide choisi dans le groupe constitué par l'acide acétique et l'acide lactique, 0,1-10 % en masse de chlorure d'aluminium et de l'eau.
PCT/JP2017/044281 2017-01-26 2017-12-11 Composition d'agent de gravure électrolytique, procédé de gravure électrolytique, substrat gravé par électrolyse, matériau d'électrode pour condensateurs électrolytiques en aluminium et condensateur Ceased WO2018139072A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2017011865A JP2018119184A (ja) 2017-01-26 2017-01-26 電解エッチング液組成物、電解エッチング方法、電解エッチングされた基材、アルミニウム電解コンデンサ用電極材、及びコンデンサ
JP2017-011865 2017-06-01

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WO2018139072A1 true WO2018139072A1 (fr) 2018-08-02

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JP (1) JP2018119184A (fr)
TW (1) TW201840916A (fr)
WO (1) WO2018139072A1 (fr)

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS541243A (en) * 1977-04-16 1979-01-08 Vickers Ltd Process for electrolytically making granular surface of aluminum and aluminum alloy
JPS61159600A (ja) * 1984-08-29 1986-07-19 ノ−ス・アメリカン・フイリツプス・コ−ポレ−シヨン 高圧アルミニウム陽極箔用２段階電気化学エツチング方法
JPH0324289A (ja) * 1989-06-05 1991-02-01 Diaprint Srl アルミニウム面又はアルミニウム合金面の電気化学的砂目立て方法
US6858126B1 (en) * 2002-11-06 2005-02-22 Pacesetter, Inc. High capacitance anode and system and method for making same

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS541243A (en) * 1977-04-16 1979-01-08 Vickers Ltd Process for electrolytically making granular surface of aluminum and aluminum alloy
JPS61159600A (ja) * 1984-08-29 1986-07-19 ノ−ス・アメリカン・フイリツプス・コ−ポレ−シヨン 高圧アルミニウム陽極箔用２段階電気化学エツチング方法
JPH0324289A (ja) * 1989-06-05 1991-02-01 Diaprint Srl アルミニウム面又はアルミニウム合金面の電気化学的砂目立て方法
US6858126B1 (en) * 2002-11-06 2005-02-22 Pacesetter, Inc. High capacitance anode and system and method for making same

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TW201840916A (zh) 2018-11-16
JP2018119184A (ja) 2018-08-02

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