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WO2007049688A1 - Cuve de reaction pour fabrication d’element de condensateur, procede de fabrication d’element de condensateur, et procede de fabrication de condensateur - Google Patents

Cuve de reaction pour fabrication d’element de condensateur, procede de fabrication d’element de condensateur, et procede de fabrication de condensateur Download PDF

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Publication number
WO2007049688A1
WO2007049688A1 PCT/JP2006/321351 JP2006321351W WO2007049688A1 WO 2007049688 A1 WO2007049688 A1 WO 2007049688A1 JP 2006321351 W JP2006321351 W JP 2006321351W WO 2007049688 A1 WO2007049688 A1 WO 2007049688A1
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WO
WIPO (PCT)
Prior art keywords
capacitor element
reaction vessel
manufacturing
cathode
capacitor
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/JP2006/321351
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English (en)
Japanese (ja)
Inventor
Kazumi Naito
Masahiro Suzuki
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.)
Resonac Holdings Corp
Original Assignee
Showa Denko KK
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Showa Denko KK filed Critical Showa Denko KK
Priority to JP2007522742A priority Critical patent/JP4049804B2/ja
Publication of WO2007049688A1 publication Critical patent/WO2007049688A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • 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
    • H01G9/0029—Processes of manufacture
    • H01G9/0036—Formation of the solid electrolyte layer
    • 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
    • H01G9/022—Electrolytes; Absorbents
    • H01G9/025—Solid electrolytes
    • H01G9/028—Organic semiconducting electrolytes, e.g. TCNQ
    • 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
    • H01G9/15—Solid electrolytic capacitors
    • 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
    • H01G9/28—Structural combinations of electrolytic capacitors, rectifiers, detectors, switching devices with other electric components not covered by this subclass

Definitions

  • Reaction vessel for manufacturing capacitor element method for manufacturing capacitor element, and method for manufacturing capacitor
  • the present invention relates to a reaction container for manufacturing a capacitor element, a method for manufacturing a capacitor element, and a method for manufacturing a capacitor, in which a stable capacity appearance rate is achieved.
  • Capacitors used in CPU (Central Processing Unit) circuits, etc. used in personal computers, etc. have a high capacity and a low capacity to suppress voltage fluctuation and reduce heat generation when passing through high ripples.
  • Low ESR equivalent series resistance
  • a plurality of aluminum solid electrolytic capacitors and tantalum solid electrolytic capacitors are used as capacitors used in CPU circuits.
  • an aluminum foil having fine pores in the surface layer, and a sintered body of tantalum powder having fine pores inside are used as one electrode (conductor), and the surface layer of the electrode is It is composed of the formed dielectric layer and the other electrode (usually a semiconductor layer) provided on the dielectric layer.
  • Patent Document 1 Patent No. 1868722
  • Patent Document 2 Patent No. 1985056
  • Patent Document 3 There is a method of forming by an energization method described in the specification (Patent Document 3). In each case, a conductor provided with a dielectric layer on the surface is immersed in the semiconductor layer forming solution, and a voltage is applied between the external electrode (cathode) prepared in the semiconductor layer forming solution with the conductor side as the anode (current is applied). This is a method of forming a semiconductor layer by flowing.
  • Patent Document 4 In Japanese Patent Application Laid-Open No. 3-22516 (Patent Document 4; related application US501727), a semiconductor layer is formed by passing a current obtained by superimposing a DC bias current on an alternating current through a conductor provided with a dielectric layer. How to do is described.
  • JP-A-3-163816 Patent Document 5 discloses that a conductor is brought into contact with a chemical polymerization layer provided on a dielectric layer, and a semiconductor layer is formed on the chemical polymerization layer by electrolytic polymerization using the conductor as an anode. How to do is described. These In this method, there is a problem when the semiconductor layer is formed on a plurality of conductors at the same time.
  • the method described in Patent Document 4 has a problem in that a semiconductor layer is formed on the cathode side, and the formation state of the semiconductor layer changes as the energization time elapses. There was no guarantee that the current would flow evenly. Further, in the method described in Patent Document 5, since a conductor provided outside is used as an anode, there is no guarantee that a uniform semiconductor layer is formed inside each conductor. In particular, it was a big problem in a conductor having a small internal pore and a large shape.
  • Patent Document 1 Patent No. 1868722 Specification
  • Patent Document 2 Patent No. 1985056
  • Patent Document 3 Patent No. 2054506
  • Patent Document 4 Japanese Patent Laid-Open No. 3-22516
  • Patent Document 5 Japanese Patent Laid-Open No. 3-163816
  • each conductor is not necessarily homogeneous and the rate of semiconductor formation may vary depending on the conductor.
  • the current value flowing through each conductor is not constant, and the formation of the semiconductor layer of the manufactured capacitor is not uniform, making it difficult to manufacture a capacitor with a stable capacity. There was a case.
  • reaction container in a form in which small reaction containers corresponding to individual conductors are assembled (refer to WO2006 / 028286 pamphlet). Since the reaction solution is consumed in the reaction vessel and adhesion to the conductor, drying, and the like proceed, changes in the liquid level of each small reaction vessel over time are not necessarily uniform. For this reason, it was difficult to repeatedly use the solution in each small reaction vessel without adjusting the liquid level.
  • the object is to propose a reaction vessel for manufacturing a capacitor element.
  • the present inventors have made a plurality of electrodes and rooms corresponding to individual conductors in a reaction vessel (a cathode and other electrodes electrically connected to respective constant current sources, respectively).
  • the reaction vessel can reduce the flow of current to other rooms when energized for forming a semiconductor layer. Settled.
  • the present invention provides the following reaction container for producing a capacitor element, a method for producing the capacitor element, a capacitor element, and a capacitor.
  • a reaction vessel in which a plurality of conductors having a dielectric layer formed on the surface are simultaneously immersed in an electrolytic solution in a reaction vessel to form a semiconductor layer by an energization method. Multiple cathodes and chambers corresponding to conductors are provided, each cathode is electrically connected to an individual constant current source, and the electrolyte can move between the other rooms.
  • a reaction vessel for producing a capacitor element characterized in that at least one passage is provided.
  • reaction container for manufacturing a capacitor element according to 1 above wherein the passage is a hole formed in a wall surface of the room, and the size (diameter) is 0.1 to LOmm.
  • reaction container for producing a capacitor element according to 1 or 2 wherein the passage is opened in a slit shape on the wall surface of the room, and the slit gap is 0.1 mm to 10 mm.
  • reaction container for producing a capacitor element according to any one of 1 to 3, wherein a cathode is provided on the bottom surface of each room.
  • reaction container for producing a capacitor element according to any one of 1 to 4, wherein a cathode is provided on a wall surface of each room.
  • each cathode is placed inside the bottom of the reaction vessel, each constant current diode is placed outside the reaction vessel, and the force swords of each constant current diode are electrically connected to each other and collected at the terminals. 7.
  • the bottom of the reaction vessel for manufacturing capacitor elements is made of an insulating substrate, and each cathode is provided on the inner surface of the insulating substrate, and a constant current source corresponding to each cathode is provided on the outer surface.
  • reaction container for producing a capacitor element according to any one of 1 to 8 above, wherein the cathode is a film metal material.
  • a method for producing a capacitor element comprising using the reaction container for producing a capacitor element according to any one of 1 to 9 above.
  • a plurality of conductors having a dielectric layer are immersed in the electrolytic solution in a reaction vessel for manufacturing a capacitor element filled with the electrolytic solution, and each of the conductors provided in the reaction vessel with the conductor side as an anode
  • the step of forming a semiconductor layer on the dielectric layer by an energization method with the cathode as the cathode is performed a plurality of times, the above steps are repeated without adjusting the liquid level in each chamber of the reaction container for producing the capacitor element.
  • a method for producing a capacitor for sealing the capacitor element obtained by the method 10 or 11 above.
  • Examples of the conductor used in the present invention include metals, inorganic semiconductors, organic semiconductors, carbon, a mixture of at least one of these, and a laminate in which these conductors are laminated on the surface layer.
  • Examples of inorganic semiconductors include metal oxides such as lead dioxide, molybdenum dioxide, tungsten dioxide, niobium monoxide, tin dioxide, and zirconium monoxide
  • examples of the organic semiconductor include polypyrrole, polythiophene, poly- Examples thereof include conductive polymers such as phosphorus and substituted or copolymer having these polymer skeletons, complexes of tetracyanoquinodimethane (TCNQ) and tetrathiotetracene, and low molecular complexes such as TCNQ salts.
  • Examples of a laminate in which a conductor is laminated on the surface layer include a laminate in which the conductor is laminated on paper, an insulating polymer, glass, or the like.
  • a metal is used as the conductor, a part of the metal is carbonized, phosphide, boronated, nitrided, It may be used after being subjected to at least one treatment selected from sulfurization.
  • the shape of the conductor is not particularly limited, and may be used as a foil shape, a plate shape, a rod shape, a shape in which the conductor itself is powdered, formed, or sintered after forming.
  • the surface of the conductor may be processed by etching or the like so as to have fine pores.
  • fine pores are provided inside the molded or sintered interior by selecting an appropriate pressure during molding. be able to.
  • the lead can be directly connected to the conductor. However, if the conductor is powdered and formed into a molded body shape or a sintered shape after molding, the lead lead prepared separately at the time of molding is used. A part of the wire (or lead foil) is molded together with a conductor, and the part outside the molded part of the lead wire (or lead foil) is used as a lead for one electrode of the capacitor.
  • a semiconductor layer to be described later may be left without forming a part of the conductor to form an anode part.
  • an insulating resin may be adhered and cured in a headband shape.
  • Preferred examples of the conductor used in the present invention include an aluminum foil whose surface is subjected to etching treatment, tantalum powder, niobium powder, alloy powder containing tantalum as a main component, alloy powder containing niobium as a main component, An example is a sintered body in which a large number of fine pores are present inside a powder such as niobium monoxide powder which has been formed and sintered.
  • TaO.AlO.Ti As a dielectric layer formed on the surface of the conductor used in the present invention, TaO.AlO.Ti
  • a dielectric layer composed mainly of at least one selected from metal oxides such as O and NbO;
  • dielectric layers can be mentioned in the field of ceramic capacitors and film capacitors.
  • a capacitor obtained by forming the dielectric layer by forming the conductor having a metal element of a metal oxide is: It becomes an electrolytic capacitor with polarity.
  • Examples of conventionally known dielectric layers for ceramic capacitors and film capacitors include dielectric layers described in Japanese Patent Application Laid-Open Nos. 63-29919 and 63-34917 by the present applicant.
  • a plurality of conventionally known dielectric layers may be laminated with a dielectric layer mainly composed of at least one selected from metal oxides or a ceramic capacitor. Yes.
  • a dielectric layer composed of at least one selected from metal oxides as a main component or a dielectric layer in which a conventionally known dielectric is mixed with a ceramic capacitor or a film capacitor may be used.
  • a plurality of long metal plates with a plurality of conductors connected at equal intervals are arranged in parallel in the metal frame and placed on the metal frame, and one anode or lead wire (lead foil) is placed in a separately prepared tank.
  • a dielectric layer is formed on the surface of the conductor by immersing the part and the conductor in the chemical conversion solution, applying a voltage between the metal frame side to the anode and the cathode plate in the chemical conversion tank for a predetermined time, lifting, washing and drying. It is formed.
  • examples of the other electrode of the capacitor obtained in the present invention include at least one compound selected from an organic semiconductor and an organic semiconductor power.
  • the compound is formed by an energization method described later. It is important.
  • organic semiconductor examples include an organic semiconductor composed of a benzopyrroline tetramer and chloranil, an organic semiconductor composed mainly of tetrathiotetracene, an organic semiconductor composed mainly of tetracyanoquinodimethane, Examples thereof include organic semiconductors mainly composed of a conductive polymer in which a polymer including a repeating unit represented by the following general formula (1) or (2) is doped with a dopant.
  • I ⁇ to R 4 each independently represents a hydrogen atom, an alkyl group having 1 to 6 carbon atoms, or an alkoxy group having 1 to 6 carbon atoms
  • X is Represents an oxygen, nitrogen or nitrogen atom
  • R 5 represents a hydrogen atom or an alkyl group having 1 to 6 carbon atoms only when X is a nitrogen atom
  • R 1 and R 2 and R 3 and R 4 represent , They may be joined together to form a ring.
  • the polymer containing a repeating unit represented by the general formula (1) is preferably a polymer containing a structural unit represented by the following general formula (3) as a repeating unit.
  • R 6 and R 7 are each independently a hydrogen atom, a linear or branched saturated or unsaturated alkyl group having 1 to 6 carbon atoms, or the alkyl group at any position with respect to each other. And a substituent which forms a cyclic structure of at least one or more 5- to 7-membered saturated hydrocarbons containing two oxygen atoms.
  • the cyclic structure may be substituted or may have a V-vinylene bond, may be substituted !, or may have a fullerene structure.
  • a conductive polymer containing such a chemical structure is charged and doped with a dopant.
  • a dopant is not specifically limited, A well-known dopant can be used.
  • Preferable examples of the dopant include a compound having a sulfonic acid group.
  • Such compounds include benzene sulfonic acid, toluene sulfonic acid, naphthalene sulfonic acid, anthracene sulfonic acid, benzoquinone sulfonic acid, naphthoquinone sulfonic acid, and sulfonic acid having an aryl group such as anthraquinone sulfonic acid, butyl sulfonic acid, Various polymers (degree of polymerization 2 to 200) such as sulfonic acid having an alkyl group such as xylsulfonic acid and cyclohexyl sulfonic acid, polyvinyl sulfonic acid, etc., sulfonic acid, salts of these sulfonic acids (ammonium salts, alkali metal salts) Typical examples are alkaline earth metal salts and the like. These compounds may have various substituents, and a plurality of sulfonic acid groups may be
  • Examples of the polymer containing the repeating unit represented by the formulas (1) to (3) include polyarylene, polyoxyphenylene, polyphenylene sulfide, polythiophene, polyfuran, polypyrrole, and polymethylbilol. And substituted derivatives and copolymers thereof. It is done. Of these, polypyrrole, polythiophene and substituted derivatives thereof (for example, poly (3,4-ethylenedioxythiophene)) are preferred.
  • the inorganic semiconductor include at least one compound selected from molybdenum dioxide, tungsten dioxide, lead dioxide, manganese dioxide, manganese dioxide and the like.
  • the ESR value of the manufactured capacitor is preferably reduced.
  • the semiconductor layer described above is formed by a pure chemical reaction (solution reaction, gas phase reaction, solid-liquid reaction and a combination thereof), formed by a current application method, or a combination of these methods.
  • the energization method is adopted at least once in the semiconductor layer forming step.
  • the object of the present invention is achieved by performing energization at least once by a constant current power source (constant current source) during energization.
  • the constant current source it is only necessary to achieve a constant current circuit capable of supplying a constant current to a conductor having a dielectric layer on the surface described above.
  • a constant current diode may be composed of a field effect transistor that is not limited to a commercially available constant current diode.
  • Other examples include constant current sources that use transistors, ICs, and three-terminal regulators.
  • a force constant current source described below for an example using a constant current diode as a constant current source is not limited to this example.
  • a reaction vessel for simultaneously producing a plurality of capacitor elements according to the present invention is provided with a cathode plate inside each chamber of the reaction vessel, and each cathode plate and a current sink type constant current source. It is characterized by the fact that there is a path to which the solution can move in another room.
  • a metal frame in which a plurality of conductors on which a dielectric layer is formed as described above for chemical conversion is arranged is placed on the upper part of the reaction vessel for producing a capacitor element of the present invention filled with an electrolyte for forming a semiconductor layer.
  • a plurality of conductors connected to are installed in individual chambers in the reaction vessel, and a constant current is applied to the metal frame and the cathode. This current forms a semiconductor layer on the dielectric layer of the conductor.
  • the current value is What is necessary is just to adjust according to the desired value of the magnitude
  • each constant current diode is arranged outside the individual chambers of the reaction vessel so that there is no crossing with the cathode plate arranged inside the bottom of the reaction vessel.
  • the reaction vessel can be reduced in size, which is preferable.
  • the hole in the reaction vessel formed by the connection wiring between the cathode plate inside and outside the reaction vessel and the constant current diode can be closed (sealed) with a resin.
  • each room is described as a rectangular cylindrical body, but each room is made of metal.
  • Other shapes for example, a cylindrical body having a hexagonal bottom surface
  • a gap may be provided between each part.
  • Fig. 1 shows a schematic side cross-sectional view of a reaction vessel (1) for manufacturing capacitor elements
  • Fig. 2 shows a plan view (surface view) of a preferred arrangement example of the cathode plate and constant current diode of the reaction vessel
  • Fig. 3 Similarly, a back view is shown.
  • a film-like metal material formed on one side of the insulating substrate by printing technology is used as a cathode plate (circular in the example shown in the figure), and a constant current diode (3 ), And the through-hole portion is closed with an insulating resin such as epoxy resin.
  • the through-hole structure is preferable because printed wiring is provided inside the through-hole, so that electrical connection between the front and back sides is easy.
  • the insulating substrate on which the plurality of cathode plates (2) and the constant current diodes (3) are arranged in this way is used as the bottom of the reaction vessel, and a frame is formed with insulating grease so as to surround the insulating substrate.
  • the reaction vessel (1) that has been processed can be used.
  • a frame (6) having a predetermined height is provided at a predetermined position of the insulating substrate so as to be perpendicular to the substrate, and a plurality of chambers into which each cathode plate is placed in the reaction vessel are prepared.
  • the chamber is structured to be filled with the electrolyte for forming the semiconductor layer, and at least one hole is provided to communicate with each other. Therefore, it is preferable to provide at least four holes on the wall surface in a room surrounded on four sides by another room. However, the liquid can actually move between rooms. If so, it is not necessary to provide a hole between all adjacent rooms. The hole should be located below the top surface of the solution to be put in the reaction vessel.
  • the size of the hole is larger than the size that the solution can move to make the liquid level uniform within the practical time range, and the size that allows the amount of current that flows to other rooms when energized to be acceptable.
  • the specific hole size varies depending on the size of the reaction vessel, the dimensions of each room, and the range of variation in the desired capacitor characteristic value, so it is determined by preliminary experiments. Usually 0. lmn! A hole with a size of ⁇ ⁇ , preferably lmm to 5mm (i) is selected. Within this range, the liquid level in each room becomes uniform within a few seconds to a few minutes, and variations in capacitor characteristics do not increase.
  • each room should be an electrical conductor (electrically connected to the cathode provided at the bottom) so that the electric field of each room does not affect other rooms as much as possible.
  • the shape of the hole is not necessarily round as long as the solution can move.
  • the clearance is preferably 0.1 to 5 mm, more preferably 1 to 5 mm.
  • each conductor with the above dielectric layer soaked in a reaction solution with a uniform liquid level, so that the desired current can be supplied to each conductor reliably. become.
  • a cathode plate that is electrically connected only to the cathode plate on the bottom surface of each room on a part or all of the frame having a predetermined height may be prepared in advance.
  • the size of the reaction vessel of the present invention can be appropriately determined according to the volume and number of conductors produced at one time and the size of the cathode plate.
  • the individual cathode plates provided in the reaction vessel are electrically insulated from each other, and each cathode plate is designed so that one conductor faces each other. For this reason, it is desirable to make the size of the cathode plate larger than the corresponding surface of the conductor to be used. However, if it is too large, the size of the reaction vessel also becomes large. For this reason, it is preferable that the size of the cathode plate is determined to be a minimum size capable of supplying a current for forming a semiconductor layer sufficient for the conductor by a preliminary experiment. For example, when the lower surface of the conductor is rectangular, the size of the cathode plate is about 1.01 to 3 times, preferably about 1.01 to 1.5 times the rectangular area.
  • a non-corrosive conductor can be used for the electrolyte for forming the semiconductor layer.
  • a non-corrosive conductor for example, iron alloy, copper alloy, tantalum, platinum or the like is used.
  • Electrolyte on the cathode plate surface Non-corrosive conductors such as nickel, gold, silver, solder, etc. may be plated. When such a plating layer is laminated on the surface, corrosive conductors such as copper and aluminum can also be used.
  • a plurality of cathode plates may be provided in one room.
  • each force sword of a plurality of constant current diodes is electrically connected, and the cathode plate is connected to the anode of each constant current diode. Are electrically connected in series.
  • a plurality of cathode plates (2) exist independently in each room at the bottom of the reaction vessel (1), and the anode of the constant current diode (3) outside the bottom of the reaction vessel is connected in series to each cathode plate. !
  • Each room is provided with holes through which the solution can freely enter and exit the frame walls that make up the room, so that the electrolyte for forming the semiconductor layer (not shown) has an equal height so as not to exceed the height of the room. Satisfied with.
  • FIG. 3 is a schematic view of the bottom of the reaction vessel as seen from the outside force.
  • a plurality of constant current diodes (3) are arranged in parallel at equal intervals, and the power sword side of each constant current diode is electrically connected to the current collector terminal (4) at the upper left in the figure.
  • Figure 2 is a schematic view of the reaction vessel as seen from above.
  • a plurality of cathode plates (2) are arranged at equal intervals. The individual cathode plates are insulated from each other and connected to the anodes of the constant current diodes in FIG. 3 through through holes (not shown) provided in the same number as the cathode plates at the bottom of the reaction vessel.
  • Each through hole is sealed with insulating resin ceramic so that the electrolyte in the reaction vessel does not ooze out.
  • a plurality of metal plates with a conductor (5) having a dielectric layer formed on the surface are connected at equal intervals, and an integrated metal frame is arranged at equal intervals.
  • Each conductor is immersed one by one in an electrolyte solution in a predetermined amount in each room provided in the reaction vessel.
  • each chamber of the reaction vessel was filled with an electrolyte for forming a semiconductor layer at an almost equal height so as not to exceed the height of the chamber, and then a dielectric layer was formed on the surface by being arranged at equal intervals on a metal frame.
  • a single conductor is immersed in each room, a metal frame is connected to the anode, and a current collecting terminal arranged outside the bottom of the reaction vessel is connected to the cathode of the power source to form a semiconductor layer by an energization method.
  • the raw material that becomes a semiconductor when energized and in some cases, the above-described dopants (for example, known dopants such as aryl sulfonic acid or salt, alkyl sulfonic acid or salt, various polymer sulfonic acid or salt) are dissolved.
  • the above-described dopants for example, known dopants such as aryl sulfonic acid or salt, alkyl sulfonic acid or salt, various polymer sulfonic acid or salt
  • energizing the semiconductor layer forming solution a semiconductor layer is formed on the dielectric layer.
  • the energization time, concentration of the semiconductor layer forming solution, pH, temperature, energizing current value, energizing voltage value vary depending on the type, size, mass, desired semiconductor layer formation thickness, etc. Determine the conditions by experiment
  • any time in the middle (can be one or more times) and Z or finally a known re-formation operation May be performed.
  • a semiconductor layer may be formed by the method of the present invention after an electrical minute defect is formed in a dielectric layer formed on the surface of the conductor layer.
  • an electrode layer is provided on the semiconductor layer formed by the above-described method in order to improve electrical contact with the external lead of the capacitor (for example, a lead frame). Also good.
  • the electrode layer can be formed by, for example, solidification of a conductive paste, plating, metal vapor deposition, adhesion of a heat-resistant conductive resin film, or the like.
  • a conductive paste silver paste, copper paste, aluminum paste, carbon paste, nickel paste and the like are preferable. These may be used alone or in combination of two or more. When two or more kinds are used, they may be mixed or laminated as separate layers. After applying the conductive paste, solidify it by heating in air or by heating. The thickness of the conductive paste after solidification is usually about 0.1 to about 200 m per layer.
  • the conductive paste is mainly composed of resin powder and conductive powder such as metal, and in some cases, it may contain a solvent for dissolving the resin, a curing agent for the resin. Solvent scatters when solidifying paste To do.
  • the resin paste in the conductive paste includes alkyd resin, acrylic resin, epoxy resin, phenol resin, imide resin, fluorine resin, ester resin, imidoamide resin, amide resin, styrene resin.
  • Various known resins such as urethane resin are used.
  • Conductive powders include silver, copper, aluminum, gold, carbon, nickel, and alloys based on these metals.
  • the conductive powder is usually contained in an amount of 40 to 97% by mass. When the content is less than 40% by mass, the conductivity of the produced conductive paste is small, and when it exceeds 97% by mass, the adhesion of the conductive paste is lowered.
  • a conductive polymer or metal oxide powder forming the semiconductor layer described above may be mixed with the conductive paste.
  • Examples of the plating include nickel plating, copper plating, silver plating, gold plating, and aluminum plating.
  • Examples of the deposited metal include aluminum, nickel, copper, gold, and silver.
  • a capacitor is formed by sequentially laminating a carbon paste and a silver paste on a conductor on which a semiconductor layer is formed and sealing with a material such as epoxy resin.
  • This capacitor may have leads that can also be pre-connected to the conductor or later connected to a metal wire or metal foil.
  • the capacitor of the present invention having the above-described configuration is, for example, a capacitor product for various uses depending on the exterior such as a resin mold, a resin case, a metallic exterior case, a resin dubbing, and an exterior using a laminate film. can do.
  • the chip-shaped capacitor with a resin-molded exterior is particularly preferred because it can reduce the size and cost.
  • the capacitor of the present invention is a lead having a pair of opposingly arranged tip portions in which a part of the conductor layer of the capacitor element is separately prepared. Place it on one end of the frame, and then place a part of the anode lead (you can cut the tip of the anode lead to match the dimensions) and place it on the other tip of the lead frame.
  • the former is solidification of the conductive paste
  • the latter is After the electrical and mechanical joining, the lead frame is sealed with a part of the tip of the lead frame, and the lead frame is cut and bent at a predetermined part outside the grease seal (the lead frame is filled with grease). If it is sealed on the bottom surface of the seal, leaving only the bottom surface or bottom and side surfaces of the lead frame, it can be made by cutting only).
  • the lead frame is cut as described above and finally becomes an external terminal of the capacitor, but the shape is foil or flat plate, and the material is iron, copper, aluminum, or these metals.
  • An alloy having a main component is used.
  • a part or all of the lead frame may be provided with a solder, tin, titanium, gold, nickel or the like. There may be an undercoating such as nickel or copper between the lead frame and the mesh.
  • the lead frame has a pair of opposed tip portions, and there is a gap between the tip portions, whereby the anode portion and the cathode portion of each capacitor element are insulated.
  • Known types of resin used for sealing solid electrolytic capacitors such as epoxy resin, phenol resin, alkyd resin, etc. can be adopted as the type of resin used for the resin mold exterior. It is preferable to use a low-stressed resin for both the resin and the resin since it is possible to mitigate the generation of the sealing stress on the capacitor element during the sealing.
  • a transfer machine is preferably used as a production machine for sealing the resin.
  • the capacitor thus fabricated may be subjected to an aging treatment in order to repair thermal and Z or physical deterioration of the dielectric layer when the electrode layer is formed or when it is packaged.
  • the aging method is performed by applying a predetermined voltage (usually within twice the rated voltage) to the capacitor.
  • the optimal values of aging time and temperature vary depending on the capacitor type, capacity, and rated voltage. At 300 ° C or less. Aging may be performed under any conditions of reduced pressure, normal pressure, and increased pressure.
  • the aging atmosphere may be air, a gas such as argon, nitrogen, or helium, but is preferably water vapor. For example, aging is performed in an atmosphere containing water vapor and then in air When performed in a gas such as gon, nitrogen or helium, the stability of the dielectric layer may advance.
  • One example of a method for supplying water vapor is a method for supplying water vapor by water in a water reservoir placed in an aging furnace.
  • the voltage application method can be designed so that an arbitrary current such as a direct current, an alternating current having an arbitrary waveform, or an alternating current superimposed on the direct current flows. It is also possible to stop the voltage application during the aging and apply the voltage again.
  • an arbitrary current such as a direct current, an alternating current having an arbitrary waveform, or an alternating current superimposed on the direct current flows. It is also possible to stop the voltage application during the aging and apply the voltage again.
  • the capacitor manufactured according to the present invention has a stable capacitance because the semiconductor layer can be formed under the same stable conditions. For this reason, the capacitance distribution (variation) of the capacitor group (a large number of capacitors manufactured simultaneously) is narrower than that of the conventional product. This improves the yield when trying to obtain a capacitor with a specific capacitance range.
  • the capacitor group manufactured in the present invention can be used for digital devices such as personal computers, servers, cameras, game machines, DVDs, AV devices, mobile phones, and electronic devices such as various power sources.
  • a cathode plate with gold plating on a copper material with a diameter of 7mm as shown in Fig. 3 A total of 640 pieces were prepared, with 32 pieces arranged in a row and 20 pieces in the width direction.
  • the other surface (back surface) was printed and wired so that the anode side of the constant current diode as shown in FIG. 2 and each cathode plate on the surface were connected in series via a through hole.
  • the force sword part of each constant current diode was soldered to the land of the printed wiring, and finally connected by wiring reaching the current collector terminal.
  • the constant current diodes were selected from F-101 from Ishizuka Electronics Co., Ltd., 120-160 A.
  • the through hole was filled with epoxy resin.
  • a glass epoxy plate (6) with a height of 20 mm and a width of 2 mm is placed perpendicular to the surface so that each cathode plate (2) on the surface enters the room one by one and is fixed with adhesive resin.
  • 640 8 x 8 mm) were prepared, and 2 mm diameter holes (7) were made at 5 mm from the bottom center of the wall of each of the 640 chambers of the reaction vessel. However, no hole is provided on the outermost wall.
  • Fig. 4 (A) shows an overview of the entire reaction vessel (1)
  • Fig. 4 (B) schematically shows three arbitrarily connected rooms.
  • the solution for forming the conductor layer was placed 15 mm in height, and the liquid level in each room was kept constant.
  • CV 100,000 F'VZg tantalum sintered body (size 4.5 X 3.0 X 1.0mm, mass 84mg, lead wire 0.40mm ⁇ out on 10mm surface) was used as the conductor.
  • a tetrafluoroethylene washer was attached to the lead wire to prevent the solution from splashing when the semiconductor layer was formed in the subsequent process.
  • the upper 2 mm of the conductor lead wire thus made was connected to a stainless steel plate with a length of 360 mm, a width of 20 mm, and a thickness of 2 mm by welding 32 pieces with the direction aligned at a distance of 10 mm from a position 25 mm from the end. .
  • a dielectric layer was formed. Next, only the conductor of the frame was dipped in 1% iron benzenesulfonate aqueous solution, pulled up, washed with water and dried seven times.
  • a reaction vessel for producing a capacitor element was filled with a 30% aqueous solution of ethylene glycol containing 3% anthraquinone-2-sulfonic acid and ethylenedioxythiophene having a saturation concentration or higher. Place the 640 conductors of the frame in the 640 rooms of the reaction vessel so that each frame is immersed in the 640 room, and energize at 13.5 V for 1 hour at room temperature with the frame as the anode and the current collector terminal at the outer bottom of the reaction vessel as the cathode.
  • a semiconductor layer was formed.
  • the frame was pulled up, washed with water and washed with alcohol. After that, the conductor and lead wire are partly immersed in the above-mentioned chemical conversion bath with 0.1% acetic acid. Then, re-formation was performed at 7V, 15 minutes, and 80 ° C. The frame was pulled up, washed with water and washed with alcohol. Such semiconductor layer formation and re-formation were repeated five times to obtain a final semiconductor layer. Furthermore, the electrode layer was laminated on the semiconductor layer by placing the frame in the order of the carbon paste tank and the silver paste tank so that the conductor portion can be immersed and drying.
  • Each conductor on which the electrode layer is formed is removed from the frame, and a part of the lead wire of the conductor is cut off and removed from the anode side of both ends of the lead frame made of copper alloy with tin plating on a separately prepared surface.
  • the silver paste side of the conductor was placed on the cathode side, and the former was connected by spot welding and the latter was connected by silver paste.
  • the lead frame was cut and bent, and a chip capacitor with a size of 7.3 x 4.3 x 1.8 mm was produced. Next, aging was performed at 115 ° C. and a voltage applied to the capacitor of 3.5 V for 5 hours.
  • the obtained capacitor has a rated capacity of 2.5V 680 / z F, 720 to 645 / z F, 525, 72 0 to 750 ⁇ F, 61, 645 to 610 ⁇ F, 49, The number distribution was 5 for 610 to 580 ⁇ F and 0 for 580 to 550 ⁇ F.
  • the capacitor was manufactured for the second time in the same manner without replenishing the solution (adjusting the liquid level) to the reactor for manufacturing the capacitor element.
  • the capacitance distribution of the obtained capacitors was almost the same between the first and second times. The results are shown in Table 1.
  • a chip capacitor was manufactured in the same manner as in Example 1 except that the size of the hole in the wall was set to 0.7 mm ⁇ in Example 1.
  • the obtained capacitors have a rated capacity of 2.5 V, 680 / z F, 556 from 720 to 645 ⁇ F, 28 from 720 to 750 ⁇ F, 56 from 645 to 610 ⁇ F, 610
  • the number distribution of 0 to 580 ⁇ F was 0, and the number of 580 to 550 ⁇ F was 0.
  • the capacitor was manufactured for the second time in the same manner without replenishing the solution (adjusting the liquid level) to the reactor for manufacturing the capacitor element.
  • the capacitance distribution of the obtained capacitors was almost the same between the first and second times. The results are shown in Table 1.
  • Example 1 except that the size of the hole in the wall was 0.2 mm ⁇ , the same as in Example 1.
  • a chip capacitor was produced.
  • the obtained capacitors have a rated 2.5V capacity of 680 / z F, 577 from 720 to 645 ⁇ F, 21 from 720 to 750 ⁇ F, 42 from 645 to 610 ⁇ F, 42, 610
  • the number distribution of 0 to 580 ⁇ F was 0, and the number of 580 to 550 ⁇ F was 0.
  • the capacitor was manufactured for the second time in the same manner without replenishing the solution (adjusting the liquid level) to the reactor for manufacturing the capacitor element.
  • the capacitance distribution of the obtained capacitors was almost the same between the first and second times. The results are shown in Table 1.
  • a chip capacitor was fabricated in the same manner as in Example 1 except that the size of the hole in the wall was set to 20 mm ⁇ in Example 1.
  • the obtained capacitors have a rated capacity of 2.5 V, 680 / z F, 455 to 720 to 645 ⁇ F, 29 to 720 to 750 ⁇ F, 108 to 645 to 610 ⁇ F, 610 It had a capacity distribution of 30 pieces of ⁇ 580 and 18 pieces of 580 to 550 F.
  • the capacitor was manufactured for the second time in the same manner without replenishing the solution (adjusting the liquid level) to the reactor for manufacturing the capacitor element.
  • the capacitance distribution of the obtained capacitors was almost the same between the first and second times. The results are shown in Table 1.
  • reaction vessel for capacitor element manufacturing the cathode plate of each small chamber of the reaction vessel was not produced by printing technology, and the bottom and side bottom forces of each small chamber were up to 14 mm in height, with 93% silver powder and 7% epoxy resin by weight.
  • two slits with a length of 7 mm and a width of 1 mm were provided as holes at 5 mm and 9 mm from the bottom of each room at the same wall position as in Example 1.
  • the solution for forming the semiconductor layer was 15 mm in height, and the liquid level in each room was kept constant.
  • Niobium primary powder (average particle size 0.32 m) crushed using the hydrogen embrittlement of niobium ingots is granulated, and niobium powder with an average particle size of 110 ⁇ m (the surface is naturally oxidized because it is a fine powder! 95000 ppm present).
  • niobium powder with an average particle size of 110 ⁇ m (the surface is naturally oxidized because it is a fine powder! 95000 ppm present).
  • it was left in a nitrogen atmosphere at 450 ° C and further in argon at 700 ° C to obtain a partially nitrided niobium powder (CV298000 ⁇ F-V / g) with a nitriding amount of 9600 ppm.
  • a plurality of sintered bodies (conductors) of mm and 10 mm outside) were produced.
  • the same number of conductors were connected to the same stainless steel plate as in Example 1, and then the same number of conductors were disposed on the metal frame.
  • a dielectric layer composed mainly of NbO was formed on the surface of the conductor and part of the lead wires by forming only the voltage at 20V.
  • Example 1 Next, after placing the reactor for producing the capacitor element in a low-temperature chamber controlled at 12 ° C, the anthraquinone 2-sulfonic acid of Example 1 was replaced with pyrrole, and the energizing voltage and the re-forming voltage were respectively set. A semiconductor layer and an electrode layer were formed and sealed in the same manner as in Example 1 except that the voltage was 23 V and 14 V, the energization time was 90 minutes, and the number of reactions was 11. An X 2.8 mm chip-shaped solid electrolytic capacitor was produced.
  • the obtained capacitors have a rated 4V capacity of 1000 ⁇ F, the number of 95 ⁇ to 1050 ⁇ F is 526, the number of 1050 to 1100 ⁇ F is 16, the number of 950 to 900 is 81, the number of 900 to 850 F is 17 It had a capacity distribution of pieces.
  • the capacitor was manufactured for the second time in the same manner without replenishing the solution (adjusting the liquid level) to the reactor for manufacturing the capacitor element.
  • the capacitance distribution of the obtained capacitor is the first time The second time was almost the same. The results are shown in Table 2.
  • a cathode plate with gold plating on a copper material with a diameter of 7mm as shown in Fig. 3 A total of 640 pieces were prepared, with 32 pieces arranged in a row and 20 pieces in the width direction.
  • the other surface (back surface) was printed and wired so that the anode side of the constant current diode as shown in FIG. 2 and each cathode plate on the surface were connected in series via a through hole.
  • the force sword part of each constant current diode was soldered to the land of the printed wiring, and finally connected by wiring reaching the current collector terminal.
  • F-101 from 120-160 A manufactured by Ishizuka Electronics Co., Ltd. was selected.
  • the through hole was filled with epoxy resin.
  • a glass epoxy plate with a height of 20 mm and a width of 2 mm is placed vertically on the surface so that each cathode plate on the surface enters into the room, and is fastened with adhesive resin.
  • 640 pieces of 8 mm) were produced, and a reaction vessel for producing a capacitor element as shown in Fig. 1 was produced.
  • the obtained capacitors have a rated 2.5V capacity of 680 ⁇ F, the number of 720 to 645 ⁇ F is 594, the number of 720 to 750 is 17 and the number of 645 to 610 F is 29. I had.
  • the capacitor was manufactured for the second time in the same manner without replenishing the solution (adjusting the liquid level) to the reactor for manufacturing the capacitor element.
  • the capacitance distribution of the obtained capacitors expanded, and the appearance capacitance distribution appeared to exceed ⁇ 20% of the set capacitance (first average capacitance).
  • the number of capacitors obtained is 565 to 720 to 645 ⁇ F, 18 to 720 to 750 ⁇ F, 38 to 645 to 610 ⁇ F, 11 to 610 to 575 ⁇ F, and 575 to 540 ⁇ F.
  • the number distribution of 2 and the number of 540-510 / z F 5 had a capacity distribution. The results are shown in Table 3.
  • Example 1 the reaction vessel for manufacturing the capacitor element of the present invention was not used, but the conventional reaction vessel, that is, the same size, but also the individual room, the individual cathode plate, and the current sink type current source.
  • the semiconductor layer is formed by energizing the cathode plate as a cathode.
  • a chip capacitor was fabricated in the same manner as in Example 1 except that was formed. The appearance capacity distribution of the obtained capacitors exceeded ⁇ 20% of the average capacity.
  • the obtained capacitor has a rated capacity of 2.5V 680 / z F, 720-6 45 ⁇ F number 359, 720-750 ⁇ F number 15, 750-780 ⁇ F number 2, 64 Number of 5 to 610 ⁇ F 150, Number of 610 to 575 ⁇ F 93, Number of 575 to 540 ⁇ F 17, Number of 540 to 510 / ⁇ 4 4 Capacity distribution It was. The results are shown in Table 3.
  • the present invention provides a reaction container for manufacturing a capacitor element in which a semiconductor layer is formed by energization through a current sink type constant current source, and a method for manufacturing the capacitor element.
  • a reaction container for manufacturing a capacitor element in which a semiconductor layer is formed by energization through a current sink type constant current source, and a method for manufacturing the capacitor element.
  • FIG. 1 is a schematic cross-sectional view showing the configuration of one embodiment of a reaction vessel for producing a capacitor element of the present invention.
  • FIG. 2 is a schematic diagram showing the configuration of the inner surface (surface) of the bottom of one form of the reaction container for producing a capacitor element of the present invention.
  • FIG. 3 is a schematic diagram showing the configuration of the back of the bottom of one form of the reaction container for producing a capacitor element of the present invention.
  • FIG. 4 (A) Schematic view showing the overall appearance of the reaction container for capacitor element production in Example 1, and (B) An enlarged schematic view of three rooms in part a in FIG. 4 (A).

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  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Manufacturing & Machinery (AREA)
  • Fixed Capacitors And Capacitor Manufacturing Machines (AREA)

Abstract

Cette invention concerne une cuve de réaction destinée à former une couche à semi-conducteur grâce à un procédé d’excitation par immersion simultanée d’une pluralité de conducteurs ayant une couche diélectrique formée en surface dans un électrolyte de la cuve de réaction, qui se caractérise en ce qu’une pluralité de cathodes et de chambres correspondant à différents conducteurs sont disposées dans la cuve de réaction, chaque cathode étant reliée électriquement à une source de courant constant distincte, et chaque chambre comprenant au moins un passage pour permettre une circulation de l’électrolyte entre les chambres. On peut ainsi obtenir simultanément un grand nombre de condensateurs ayant une distribution de capacité de sortie minime.
PCT/JP2006/321351 2005-10-27 2006-10-26 Cuve de reaction pour fabrication d’element de condensateur, procede de fabrication d’element de condensateur, et procede de fabrication de condensateur Ceased WO2007049688A1 (fr)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2011077950A1 (fr) * 2009-12-21 2011-06-30 昭和電工株式会社 Conteneur de réaction pour fabriquer un élément condensateur, et procédé de fabrication de l'élément condensateur
CN110379627A (zh) * 2019-05-31 2019-10-25 益阳艾华富贤电子有限公司 一种固液混合电容器的制备工艺及固液混合电容器
TWI690958B (zh) * 2018-09-19 2020-04-11 鈺冠科技股份有限公司 電容器元件的前處理設備與電容器元件的快速製造方法

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0322516A (ja) * 1989-06-20 1991-01-30 Sanyo Electric Co Ltd 固体電解コンデンサの製造方法
JP2005244154A (ja) * 2003-07-10 2005-09-08 Showa Denko Kk コンデンサ製造用冶具、コンデンサの製造方法及びコンデンサ

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0322516A (ja) * 1989-06-20 1991-01-30 Sanyo Electric Co Ltd 固体電解コンデンサの製造方法
JP2005244154A (ja) * 2003-07-10 2005-09-08 Showa Denko Kk コンデンサ製造用冶具、コンデンサの製造方法及びコンデンサ

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2011077950A1 (fr) * 2009-12-21 2011-06-30 昭和電工株式会社 Conteneur de réaction pour fabriquer un élément condensateur, et procédé de fabrication de l'élément condensateur
JP4778126B2 (ja) * 2009-12-21 2011-09-21 昭和電工株式会社 コンデンサ素子製造用反応容器及びコンデンサ素子の製造方法
KR101387787B1 (ko) 2009-12-21 2014-04-21 쇼와 덴코 가부시키가이샤 콘덴서 소자 제조용 반응 용기 및 콘덴서 소자의 제조 방법
US8792225B2 (en) 2009-12-21 2014-07-29 Showa Denko K.K. Partitioned reaction container for manufacturing capacitor element including openable and closable passage
TWI690958B (zh) * 2018-09-19 2020-04-11 鈺冠科技股份有限公司 電容器元件的前處理設備與電容器元件的快速製造方法
CN110379627A (zh) * 2019-05-31 2019-10-25 益阳艾华富贤电子有限公司 一种固液混合电容器的制备工艺及固液混合电容器

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JP4049804B2 (ja) 2008-02-20

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