CN101015030B - Reaction vessel for producing capacitor element, production method for capacitor element, capacitor element and capacitor - Google Patents
Reaction vessel for producing capacitor element, production method for capacitor element, capacitor element and capacitor Download PDFInfo
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- CN101015030B CN101015030B CN2005800303003A CN200580030300A CN101015030B CN 101015030 B CN101015030 B CN 101015030B CN 2005800303003 A CN2005800303003 A CN 2005800303003A CN 200580030300 A CN200580030300 A CN 200580030300A CN 101015030 B CN101015030 B CN 101015030B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G13/00—Apparatus specially adapted for manufacturing capacitors; Processes specially adapted for manufacturing capacitors not provided for in groups H01G4/00 - H01G11/00
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
- H01G9/0032—Processes of manufacture formation of the dielectric layer
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
- H01G9/042—Electrodes or formation of dielectric layers thereon characterised by the material
Abstract
There is provided a reaction vessel for manufacturing capacitor elements. The reaction vessel contains electrolytic liquid in which a plurality of conductors having a dielectric layer on the surface are simultaneously dipped and a semiconductor layer is formed by the electricity application method. The reaction vessel for manufacturing a capacitor element is characterized in that a plurality of cathodes are arranged in the reaction vessel to correspond to the respective conductors and a plurality of constant current sources are electrically connected to the respective cathodes. There are also provided a method for manufacturing the capacitor elements by using the reaction vessel and a capacitor using the capacitor elements. Thus, it is possible to simultaneously obtain a plenty of capacitors using a semiconductor layer as one of the electrodes and having a narrow appearing capacity distribution.
Description
Technical field
The manufacture method, this capacitor element manufacturing that the present invention relates to realize the capacitor element of stable electric capacity occurrence rate is with reaction vessel, the capacitor element and the capacitor that use above-mentioned manufacture method or reaction vessel to make.
Background technology
Capacitor in the circuit of the CPU (central processing unit) that computer etc. are used etc., in order to suppress voltage fluctuation, reduce high fluctuation (ripple) by the time heating, pursue is high capacitance and low ESR (equivalent serial resistance) always.
Usually, the capacitor as using in cpu circuit is just using a plurality of solid aluminium electrolytic capacitors, tantalum solid electrolytic capacitor.
Such solid electrolytic capacitor is made of as electrode, the dielectric layer that forms on the top layer of this electrode of side's electrode (electric conductor) and the opposing party's electrode (normally semiconductor layer) that is arranged on this dielectric layer the aluminium foil that superficial layer is had fine pore or inner sintered body with tantalum powder of small pore.
As with the formation method of semiconductor layer as the semiconductor layer of the capacitor of the opposing party's electrode, No. 1868722 specification of with good grounds for example Japan Patent, No. 1985056 specification of Japan Patent and the Japan Patent method that the electrifying method of record forms that is right for No. 2054506.Respectively to impregnated in semiconductor layer by the electric conductor that will be provided with on the top layer dielectric layer to form with in the solution, with the conduction side as anode and at applied voltage (current flowing) between it and the outer electrode (negative electrode) in semiconductor layer forms with solution, prepared, thereby the method for formation semiconductor layer.
In Unexamined Patent 3-22516 communique, record, exchanging the electric current be superimposed with dc bias current and be provided with circulation in the electric conductor of dielectric layer and form the method for semiconductor layer by making.In addition, in Unexamined Patent 3-163816 communique, record, make the chemical polymerization layer on the conductor contact dielectric layer, this conductor is formed the method for semiconductor layer as anode by electrolysis polymerization at the chemical polymerization layer.These methods are at the same time in the situation that a plurality of electric conductor forms semiconductor layer has problems.The method of namely in Unexamined Patent 3-22516 communique, putting down in writing, also form semiconductor layer at cathode side, have along with the process conduction time problem that the formation situation of semiconductor layer changes, in addition, not equably this guarantee of circulating current in a plurality of electric conductors.In addition, the method for putting down in writing in Unexamined Patent 3-163816 communique is switched on as anode because will be arranged on outside conductor, so do not form the guarantee of uniform semiconductor layer in the inside of each electric conductor.Especially little for the pore of inside and for for the electric conductor of large shape, also be very large problem.
Summary of the invention
In above-mentioned formation the electric conductor of dielectric layer adopt electrifying method to form the occasion of semiconductor layer, under industrial level, for example the electric conductor more than 100 forms in the situation of semiconductor layer, each electric conductor might not be homogeneous, sometimes semi-conductive formation speed is also different because of electric conductor in addition, so when especially on a plurality of electric conductors, forming semiconductor layer simultaneously, the current value that existence is circulated in each electric conductor is non-constant, the formation situation of the semiconductor layer of the capacitor of making is inconsistent, is difficult to the situation of the capacitor of the stable electric capacity of manufacturing.
Therefore, problem of the present invention is, provide a kind of and adopting electrifying method in the situation of the semiconductor layer of a plurality of electric conductors formation capacitors, the capacitor element that can access the formation capacitor stable, that capacitance profile is narrow of semiconductor layer is made means (reaction vessel and manufacture method).
What the present inventors studied with keen determination in order to solve above-mentioned problem found that, by supplying with constant current to electric conductor, forming semiconductor layer, can access the narrow capacitor group of capacitance profile, has finally finished the present invention.
That is, the invention provides following capacitor element manufacturing with the manufacture method of reaction vessel, capacitor element and capacitor element, capacitor.
1. capacitor element manufacturing reaction vessel, it is characterized in that, it be in the electrolyte that will be immersed in simultaneously at a plurality of electric conductors that the surface has formed dielectric layer reaction vessel, utilize electrifying method to form the reaction vessel of semiconductor layer, a plurality of negative electrodes corresponding to each electric conductor are set in reaction vessel, have a plurality of constant-current sources that are being connected with each cathodic electricity.
2. the capacitor element manufacturing reaction vessel put down in writing as in above-mentioned 1, a plurality of constant-current sources are made of a plurality of current regulator diodes, are electrically connected between its each negative electrode, and each anode is being connected with negative electrode.
3. the capacitor element manufacturing reaction vessel put down in writing as in above-mentioned 1 or 2, be configured in reaction vessel bottom inside each negative electrode and be configured in the anodic bonding of each current regulator diode in the outside of reaction vessel, be electrically connected between the negative electrode of each current regulator diode, thus on terminal current collection.
As above-mentioned 1 to 3 in each capacitor element manufacturing reaction vessel of putting down in writing, each current regulator diode that is arranged on each negative electrode on the face (surface) of insulating properties substrate and is configured on another face (back side) of insulating properties substrate is electrically connected by through hole, and the insulating properties substrate that through hole is sealed is as the bottom of reaction vessel.
5. the capacitor element manufacturing reaction vessel put down in writing as in above-mentioned 4, minus plate is membranaceous metal material.
6. the manufacture method of a capacitor element is characterized in that, uses in above-mentioned 1 to 5 each capacitor element manufacturing reaction vessel of putting down in writing.
7. the manufacture method of a capacitor element, it is characterized in that, the capacitor element manufacturing that in above-mentioned 1 to 5 each put down in writing is filled with electrolyte in reaction vessel, a plurality of electric conductors that will have dielectric layer are immersed in the above-mentioned electrolyte, take this conduction side as anode, take each negative electrode of in reaction vessel, arranging as negative electrode, utilize electrifying method to form semiconductor layer at dielectric layer.
8. capacitor element group of making according to the manufacture method of putting down in writing in above-mentioned 6 or 7.
9. a capacitor has used the capacitor element group of putting down in writing in above-mentioned 8, and it capacitance profile (appearing capacity distribution) occurs in the scope of average capacitance ± 20%.
As the example of the electric conductor that uses in the present invention, can enumerate metal, inorganic semiconductor, organic semiconductor, carbon, at least a mixture in them, be laminated with the laminated body of electric conductor on the top layer of described material.
Example as inorganic semiconductor, can enumerate the metal oxides such as brown lead oxide, molybdenum dioxide, tungsten dioxide, columbium monoxide, tin ash, a zirconia, as organic semiconductor, can enumerate polypyrrole, polythiophene, polyaniline and have the low molecule complexes such as complex, tcnq salt of the electroconductive polymers such as substituent, copolymer, four cyano quinone bismethane (TCNQ) of these macromolecular scaffolds and four sulphur aphthacenes.In addition, as the example that is laminated with the laminated body of electric conductor on the top layer, can be set forth in the upper stacked laminated body of above-mentioned electric conductor such as paper, insulating properties macromolecule, glass.
Use as electric conductor in the situation of metal, at least a processing that can be selected from the part of metal in carbonization, phosphatization, boronation, nitrogenize, the sulfuration re-uses afterwards.
The shape of electric conductor is not particularly limited, can with the paper tinsel shape, tabular, bar-shaped, electric conductor self made powdery and sintering and the shape that forms etc. are applicable after being shaped or being shaped.Thereby also the electric conductor surface can be waited to process by corrosion and make it to have fine pore.Electric conductor is being made powdery, and form the formed body shape or be shaped after in the situation of sintering and the shape that forms, the pressure when suitably selecting to be shaped, can be shaped or sintering after inside small pore is set.
Can on electric conductor, directly connect and draw lead-in wire, but electric conductor is made powdery and form the formed body shape or be shaped after in the situation of the shape that forms of sintering, the part of drawing lead-in wire (or lead-in wire paper tinsel) that also can will prepare separately when being shaped is with the electric conductor moulding, will draw the position of shaping outside of lead-in wire (or the paper tinsel that goes between) as the lead-in wire of drawing of side's electrode of capacitor.
In addition, do not form semiconductor layer described later on can the part of electric conductor yet and left behind as anode portion.On the border of anode portion and semiconductor layer forming portion, in order to prevent climbing of semiconductor layer, can be that holding shape ground adheres to insulative resin and make it sclerosis.
As the preferred example of electric conductor of the present invention, can enumerate the aluminium foil that exists most fine-pored sintered bodies and surface to be corroded and to process in inside that sintering formed after the powder such as tantalum powder, niobium powder, the alloyed powder take tantalum as principal component, the alloyed powder, niobium monoxide powder take niobium as principal component were shaped.
As the dielectric layer that forms on electric conductor of the present invention surface, can enumerate and to be selected from Ta
2O
5, Al
2O
3, TiO
2, Nb
2O
5Deng at least a dielectric layer as principal component in the metal oxide, in the field of ceramic capacitor, film capacitor known dielectric layer in the past.The former occasion that will be selected from least a dielectric layer as principal component in the metal oxide, when forming dielectric layer by the above-mentioned electric conductor that changes into the metallic element with metal oxide, resulting capacitor becomes the electrolytic capacitor that polarity is arranged.As known dielectric layer in the past in ceramic capacitor, the film capacitor, can enumerate the dielectric layer of putting down in writing in JP 63-29919 communique from the applicant, the JP 63-34917 communique.In addition, also can with take at least a dielectric layer as principal component that is selected from metal oxide, in ceramic capacitor, film capacitor stacked a plurality of use of known dielectric layer in the past.In addition, also can be with take at least a dielectric as principal component that is selected from metal oxide, known dielectric mixes the dielectric layer that forms in ceramic capacitor, film capacitor in the past.
About describing by changing into the object lesson that forms dielectric layer.
The long-bar metal plate multi-disc that a plurality of electric conductors are connected equally spacedly arranges side by side and is configured on the metal framework, a part and electric conductor with anode portion or lead-in wire (lead-in wire paper tinsel) in the electrolytic bath of preparing separately are immersed in the forming liquid, add the voltage of stipulated time take metal framework as anode, between the minus plate in it and the electrolytic bath, clean by promoting, dry, thereby at electric conductor top layer formation dielectric layer.
On the other hand, as another electrode of capacitor of the present invention, can enumerate at least a compound that is selected from organic semiconductor and the inorganic semiconductor, be important but form above-mentioned compound at this by electrifying method described later.
As the organic semi-conductor object lesson, can enumerate the organic semiconductor that formed by benzopyrrole quinoline tetraploid and chloranil, the organic semiconductor take four sulphur aphthacenes as principal component, the organic semiconductor take four cyano quinone bismethane as principal component, in the macromolecule that contains the repetitive shown in following formula (1) or (2), to be doped with the electroconductive polymer of alloy as the organic semiconductor of principal component.
In formula (1) and the formula (2), R
1～R
4Represent independently respectively the alkyl of hydrogen atom, carbon number 1-6 or the alkoxyl of carbon number 1-6, X represents oxygen, sulphur or nitrogen-atoms, and R5 only exists when X is nitrogen-atoms, the alkyl of expression hydrogen atom or carbon number 1-6, R
1And R
2, and R
3And R
4Can mutually combine and become ring-type.
In addition, in the present invention, as the macromolecule that contains the repetitive shown in the following formula (1), preferably list and contain the construction unit shown in the following formula (3) as the macromolecule of repetitive.
In the formula, R
6And R
7Represent independently that respectively saturated the or undersaturated alkyl of the straight chain shape of hydrogen atom, carbon number 1-6 or chain or this alkyl mutually in arbitrarily position combination, form the substituting group of the circulus of 5～7 yuan of ring filling hydrocarbon more than at least 1 that contain 2 oxygen atoms.The base of the phenylene structure that in addition, also comprise the base with ethenylidene key (vinylene bond) that can be replaced by above-mentioned circulus, can be replaced by above-mentioned circulus.
The electroconductive polymer that contains such chemical constitution, by charged, the doping alloy.Alloy without particular limitation of, can use known alloy.
As the preferred example of alloy, can enumerate and have sulfonic compound.As such compound, can enumerate various macromolecules (degree of polymerization 2-200) sulfonic acid of the sulfonic acid with alkyl, polyvinylsulfonic acid etc. of the sulfonic acid with aryl, butyl sulfonic acid, hexyl sulfonic acid and the cyclohexyl sulfonic acid etc. of benzene sulfonic acid, toluenesulfonic acid, naphthalene sulfonic acids, rylnthracene sulfonin, benzoquinones sulfonic acid, naphthoquinone sulfonic acid and anthraquinone sulfonic acid etc., the salt (ammonium salt, alkali metal salt, alkali earth metal salt etc.) of these sulfonic acid as typical example.These compounds both can have various substituting groups, can have a plurality of sulfonic groups again.In addition, alloy can use a plurality of simultaneously.
As the macromolecule that contains the repetitive shown in formula (1)～(3), such as enumerating polyaniline, polyoxy phenylene, polyphenylene sulfide, polythiophene, poly-furans, polypyrrole, poly-methyl pyrrole and their substitutive derivative and copolymer etc.Wherein, preferred polypyrrole, polythiophene and their substitutive derivative (for example poly-(3,4-ethylidene dioxy thiophene) etc.).
As the object lesson of inorganic semiconductor, can enumerate at least a compound that is selected from molybdenum dioxide, tungsten dioxide, brown lead oxide, the manganese dioxide etc.
As above-mentioned organic semiconductor and inorganic semiconductor, preferably use conductivity 10
-2～10
3During the semiconductor of S/cm scope, the ESR value of the capacitor that manufactures diminishes, and is therefore preferred.
Above-mentioned semiconductor layer, can form or make up these methods by pure chemical reaction (solution reaction, gas-phase reaction, solid-liquid reaction and their combination) formation, by electrifying method and form, but in the present invention, in semiconductor layer formation operation, adopt at least one times electrifying method.In addition, in the situation that the logical electrifying method that adopts forms semiconductor layer, by carrying out at least one times energising by constant-current supply (constant-current source) when the energising, thereby can reach purpose of the present invention.
As constant-current source, as long as can reach the constant-current circuit that the electric conductor energising of dielectric layer can be arranged to above-mentioned surface with constant current.For example, preferably, part count diminishbb current regulator diode simple by circuit consists of.Current regulator diode is not only as current regulator diode and commercially available diode also can be made of field-effect transistor.As the constant-current source beyond that, the constant-current source of the constant-current source that can enumerate and use transistorized constant-current source, uses IC, use three terminal pressurizers etc.
Below to using the example of current regulator diode to describe as constant-current source, but constant-current source is not limited thereto example.
The reaction vessel that is used for making simultaneously a plurality of capacitor elements involved in the present invention comprises following structure: the bottom in each chamber of reaction vessel inboard is provided with minus plate, the anodic bonding of each minus plate and each current regulator diode, and the negative electrode of each current regulator diode is electrically connected to each other current collection on terminal.About changing into, the metal framework that will carry out lining up to a plurality of electric conductors of above-mentioned formation dielectric layer is configured in and fills with reaction vessel is used in semiconductor layer formation with the capacitor element manufacturing of the present invention of electrolyte top, a plurality of electric conductors that will be connected with metal framework are arranged in each chamber in this reaction vessel, when the current-collecting terminals applied voltage in metal framework and described current regulator diode group, just flow through the constant electric current (in order to reach specific current range, can select current regulator diode) of the grade (current specification) corresponding to current regulator diode.Utilize this electric current to form semiconductor layer at the dielectric layer of electric conductor.Current regulator diode, when with forward (direction of current regulator diode) when the direction from anode to negative electrode adds the voltage of prescribed limit, just flow through the constant current of regulation, but because current value by selecting current regulator diode grade or, current regulator diode parallel connection that will a plurality of suitable grades or series and parallel connections and with use, can change on ladder ground, so the desired value according to the size of conductor and the semiconductor amount that forms is selected current regulator diode, the constant current of any range that can circulate.
Each current regulator diode, when being configured in the outside of each chamber of reaction vessel, can be staggered with the minus plate of the bottom inside that is configured in reaction vessel, thus can make the reaction vessel miniaturization, be preferred therefore.In this case, can be connected the hole connection distribution, reaction vessel with current regulator diode based on being positioned at minus plate inside and outside the reaction vessel with the obstructions such as resin (sealing).
Referring to accompanying drawing concrete scheme of the present invention is described.
Fig. 1 represents the capacitor element manufacturing with the ideograph of an example of reaction vessel (1), and Fig. 2 represents the plane graph (exterior view) of the preferred disposition example of the minus plate of reaction vessel of the present invention and current regulator diode, and Fig. 3 represents its back view.
Can enumerate the configuration example of following structure: the membranaceous metal material that will form by printing technology on the one side of insulating properties substrate is as minus plate (being circular in the illustrated example), by the through hole of insulating properties substrate overleaf the regulation position of printed wiring set current regulator diode (3) afterwards, stop up through-hole section with insulative resins such as epoxy resin.Hole configuration because at the through hole internal implementation printed wiring, therefore so can easily realize the electrical connection at the surperficial back side, be preferred.So, can use the insulating properties substrate that will set a plurality of minus plates (2) and each current regulator diode (3) as the bottom of reaction vessel, form the reaction vessel (1) that processes framework with insulative resin in the mode of surrounding the insulating properties substrate.In addition, also can make following structure: the framework (6) that specified altitude is set in the mode vertical with substrate at the regulation position of insulating properties substrate, in reaction vessel, make a plurality of chambers that each minus plate is housed, in each chamber, fill with the electrolyte that semiconductor layer forms usefulness.In order to supply with reliably desired electric current to each electric conductor, preferably the mode with above-mentioned each electric conductor that is formed with dielectric layer of dipping in each chamber of such reaction vessel designs.Can on part or all of the framework of specified altitude, make in advance the minus plate that only is electrically connected with the minus plate of the bottom surface that is positioned at each chamber.
The size of reaction vessel of the present invention can suitably determine according to the size of the volume of the electric conductor of once making and number, minus plate.The housing that can make the adjustment water circulation can be set in reaction vessel.
Each minus plate that arranges in the bottom surface of reaction vessel designs in the face of the mode of the lower surface of each electric conductor of one (5) with electrically insulated from one another, each minus plate.Therefore, preferably make the size of minus plate (2) greater than the lower surface of employed electric conductor.But if excessive, then the size of reaction vessel also becomes greatly, and the quantitative change of the electrolyte of employed semiconductor layer formation usefulness is many, therefore unfavorable on cost.Because such reason, the size of minus plate is decided to be the size that can circulate for the minimum of the electric current that forms sufficient semiconductor layer at electric conductor by preliminary experiment.For example, be in the rectangular situation at the lower surface of electric conductor, the size of minus plate is about 1.01～3 times of this rectangular area, preferably about 1.01～1.5 times.
As the material of minus plate, the electrolyte that can use semiconductor layer to form usefulness is noncorrosive conductor with respect to it.For example, can use ferroalloy, copper alloy, tantalum, platinum etc.Can on the minus plate surface, plating electrolyte be noncorrosive conductor with respect to it also, such as at least one deck of nickel and gold, silver, scolding tin etc.Being laminated with on the surface is the occasion of coating like this, also can use electrolyte to its mordant conductor, for example copper, aluminium.
Minus plate also can arrange multi-disc in a chamber.In this case, for example two minus plates need to make two all to be connected with a constant-current source that is positioned at its back side in a chamber, can not use two constant-current sources.The minus plate of the size that a slice can put into preferably is set in a chamber.
Capacitor element manufacturing reaction vessel of the present invention is the reaction vessel that each above-mentioned minus plate is electrically connected with the constant-current source of electric current induction type.In the situation that consist of constant-current source with current regulator diode, the situation of the formation that each cathodic electricity that for example can enumerate a plurality of current regulator diodes connects, above-mentioned minus plate and the anode of each current regulator diode in series are electrically connected.
, be described in more details with the reaction vessel example based on capacitor element manufacturing represented among Fig. 1.Have an independent existence in each chamber at a plurality of minus plates in the bottom of reaction vessel (1) (2), be connected in series the anode of the current regulator diode (3) of the bottom outside that is positioned at reaction vessel on each minus plate.In each chamber, fill with the electrolyte (not shown) that semiconductor layer forms usefulness in the mode of the height that is no more than the chamber with the basic height that equates.
Fig. 3 is the ideograph of the bottom of (back side) observing response container from the outside.Current regulator diode (3) is a plurality of side by side uniformly-spaced to configure, and the cathode side of each current regulator diode is electrically connected, and is being connected with upper left current-collecting terminals (4) among the figure.Fig. 2 is the ideograph from top (surface) observing response container.Minus plate (2) is a plurality of equally spaced to be configured.Each minus plate mutually insulated, and pass through at the through hole (not shown) of reaction container bottom and the setting of minus plate equal number ground and the anodic bonding of each current regulator diode among Fig. 3.Each through hole is by insulative resin, ceramic seal, and the electrolyte in the reaction vessel can not ooze out.Top at reaction vessel sets, with uniformly-spaced configure multi-disc, uniformly-spaced to have connected the electric conductor (5) that is formed with dielectric layer on the surface thus the integrated metal framework of metallic plate.The amount that each electric conductor is immersed in to stipulate one by one is contained in the electrolyte in each chamber that is arranged in the reaction vessel.
Then, to describing with reaction vessel, the method for utilizing electrifying method to form semiconductor layer with above-mentioned capacitor element manufacturing.
After the electrolyte that semiconductor layer is formed usefulness in the mode of the height that is no more than the chamber in each chamber of reaction vessel fills with the basic height that equates, the electric conductor that will form in the first-class arranged spaced of metal framework (7), on the surface dielectric layer steeps one by one into each chamber, take metal framework as anode, take the current-collecting terminals that is configured in the reaction container bottom outside as negative electrode, utilize electrifying method to form semiconductor layer.
By to being dissolved with, the semiconductor layer formation that becomes semi-conductive raw material through energising and according to circumstances be dissolved with above-mentioned alloy (known alloys such as aryl sulfonic acid or its salt, alkyl sulfonic acid or its salt, various macromolecule sulfonic acid or its salt) can form semiconductor layer at dielectric layer with the solution energising.Because form conduction time, semiconductor layer concentration, pH value, temperature, electrical current value with solution, the magnitude of voltage of switching on changes according to the formation thickness of the kind of employed electric conductor, size, quality, desired semiconductor layer etc., so determine by experiment in advance condition.Also can change power on condition repeatedly switches on.In addition, for the defective to the dielectric layer that forms on electric conductor surface is repaired, also can be halfway any the time (can be once also can be repeatedly) and/or carry out at last in the past knownly changing into again operation.
In addition, also can after the dielectric layer on the surface that is formed at conductor layer is made the tiny flaw section of electricity, form semiconductor layer by method of the present invention.
In the capacitor of the present invention, on the semiconductor layer of the formation such as employing said method, to draw electrically contacting well of lead-in wire (for example lead frame) in order making with the outside of capacitor, electrode layer can be set.
Electrode layer can be by forming such as adhering to of the curing of electroconductive paste, plating, metal evaporation, thermal endurance electroconductive resin film etc.As electroconductive paste, preferred silver paste, copper paste, aluminium paste, carbon paste, nickel paste etc.They can use a kind of, also can use two or more.In the situation that use is two or more, can mix, perhaps also can be used as different layers and carry out stacked.After using electroconductive paste, be placed in the air or heating makes its curing.Thickness after electroconductive paste solidifies, every layer of about 0.1～approximately 200 μ m normally.
Electroconductive paste take the conducting powder of resin and metal etc. as principal component, according to circumstances also can contain the solvent that is useful on dissolving resin, the curing agent of resin etc.Solvent disperses when sticking with paste curing.
As the resin in the electroconductive paste, can use the known various resins such as alkyd resins, acrylic resin, epoxy resin, phenolic resins, imide resin, fluororesin, ester resin, acid imide amide resin, amide resin, styrene resin, polyurethane resin.As conducting powder, can use silver, copper, aluminium, gold, carbon, nickel and with at least a as the mixture powder of the powder of the alloy of principal component, coating powder that these metals are positioned at the top layer and these powder of these metals.
Usually the conducting powder that contains 40～97 quality %.If less than 40 quality %, the conductivity of the electroconductive paste of then making is little, and if above 97 quality %, then the adhesiveness of electroconductive paste diminishes.Use after also can in electroconductive paste, mixing the powder of electroconductive polymer, metal oxide of above-mentioned formation semiconductor layer.
As plating, can enumerate nickel plating, copper facing, silver-plated, gold-plated, aluminize etc.As evaporation metal, can enumerate aluminium, nickel, copper, gold, silver etc. in addition.
Particularly, for example sequentially stacked carbon paste, silver are stuck with paste on the electric conductor that has formed semiconductor layer, and with the material seal of epoxy resin and so on, thereby the formation capacitor.This capacitor, can have be connected in advance with electric conductor or with the latter linked lead-in wire that is consisted of by metal wire, metal forming.
The capacitor of the present invention of formation as described above, can by such as the dipping of resin-molded, resin shell, metallic outer packing shell, resin, utilize the external packing of external packing that stack membrane carries out etc., make the capacitor goods of various uses.
Wherein, especially having carried out the capacitor of the sheet of resin-molded external packing, owing to can carry out miniaturization and cost degradation, is preferred therefore.
Situation to resin-molded external packing is specifically described, capacitor of the present invention is made by following step: the part of the conductor layer of above-mentioned capacitor element is positioned in the termination section of lead frame of the termination section with a pair of relative configuration of preparing separately, again with the part of anode tap (in order to make consistent size, use after can cutting off the termination of anode tap) be positioned in another termination section of above-mentioned lead frame, for example the former is by the curing of electroconductive paste, the latter carries out respectively after the electromechanical ground joint by welding, the part of the termination section of residual above-mentioned lead frame, carry out the resin sealing, and the regulation position beyond the resin sealing cuts off bending machining to conductive pane, and (lead frame is positioned at below the resin sealing, following or the following and side of residual lead frame and by the occasion of being sealed only, can only cut off processing), thus make.
Above-mentioned lead frame through cut-out as described above processing, finally become the outside terminal of capacitor, but shape is paper tinsel shape or tabular, and material can be used iron, copper, aluminium or with the alloy of these metals as principal component.Can implement the plating of scolding tin, tin, titanium, gold, nickel etc. to part or all of this lead frame.Between lead frame and coating, the prime coat of nickel or copper etc. can be arranged.
Also can be after above-mentioned cut-out bending machining or before lead frame is carried out these various plating.In addition, also can be in mounting, carry out plating before connecting capacitor element after, and then carry out again plating when any after the sealing.
There is the termination section of a pair of relative configuration in this lead frame, and is gapped between the section of termination, thus with anode portion and the negative pole part insulation of each capacitor element.
Kind as the resin that in resin-molded external packing, uses, the known resin that can adopt epoxy resin, phenolic resins, alkyd resins etc. in the sealing of solid electrolytic capacitor, to use, but when each resin all preferably uses the low stress resin, the generation for the Sealing Stress of capacitor element that can relax that when sealing cause, therefore preferred.In addition, as the maker that is used for carrying out the resin sealing, preferably use automatic assembly line.
The capacitor of making like this, dielectric layer heat and/or physics when forming in order to repair electrode layer, during external packing aging can carry out burin-in process.
Aging method is undertaken by the voltage (being generally in the twice of rated voltage) that capacitor is added regulation.Ageing time and temperature, the different optimum values of kind, electric capacity, rated voltage according to capacitor are also different, so decide by experiment in advance, but usually the time be several minutes～a couple of days, temperature consider applied voltage anchor clamps heat ageing and carrying out below 300 ℃.Aging atmosphere can be at decompression, normal pressure, add under any condition of depressing and carry out.In addition, in the gases such as aging atmosphere also can be in the air, argon, nitrogen, helium, but preferably in the steam.In the atmosphere that is containing steam that wears out, carry out, then in air, when carrying out in the gases such as argon, nitrogen, helium, sometimes advance the stabilisation of dielectric layer.Also can turn back to atmospheric pressure at room after supplying with steam, perhaps the high temperature at 150 ℃～250 ℃ is placed several minutes～a few hours after supplying with steam, thereby removes unnecessary moisture, then carries out above-mentioned aging.As an example of the supply method of steam, can enumerate the method that tank utilization heat from be placed on ageing oven is supplied with steam.
As the outer adding method of voltage, can with flow through direct current, have random waveform interchange, with direct current overlapping exchange and the mode of the arbitrarily electric current of pulse current etc. designs.Also can apply at the aging voltage that stops first temporarily midway, then carry out once again voltage and apply.
The capacitor of making according to the present invention is because the formation of semiconductor layer can carry out under stable identical conditions, so electric capacity is stable.Therefore, the capacitance profile (dispersing) of capacitor group (a plurality of capacitors of making simultaneously) is compared with goods in the past and is narrowed down.Therefore, when expecting the capacitor of specific capacitance range, do not need to select according to electric capacity, even if perhaps be necessary to select, qualification rate also improves.
In addition, capacitor group constructed in accordance can be applied in the electronic equipment of the digital devices such as personal computer, server, camera, game machine, DVD, AV equipment, mobile phone and various power supplys etc.
Description of drawings
Fig. 1 is expression capacitor element manufacturing of the present invention with the ideograph of the formation of a form of reaction vessel.
Fig. 2 is expression capacitor element manufacturing of the present invention with the ideograph of the formation of the container bottom inner face (surface) of a form of reaction vessel.
Fig. 3 is expression capacitor element manufacturing of the present invention with the ideograph of the formation at the container bottom back side of a form of reaction vessel.
Embodiment
Below, object lesson of the present invention is done more detailed explanation, but the present invention is not limited to following example.
Embodiment 1:
1. the capacitor element manufacturing making of reaction vessel
On the copper-surfaced glass epoxy board of long 322mm, wide 202mm, thick 2mm by printed wiring the interval has as one man been made longitudinally be 32, along laterally being that the copper material at diameter 7mm 20, that amount to 640 has been implemented gold-plated minus plate.And then carry out printed wiring at another face (back side), and so that be connected in series the anode-side of the such current regulator diode of Fig. 2 and each minus plate on surface by through hole.The negative pole part of each current regulator diode and the pad of printed wiring (land) surface is connected with scolding tin, and the distribution by final arrival current-collecting terminals connects.As current regulator diode, from the F-101 of stoneman electronics (strain) system, select 120～160 μ A's.Through-hole section epoxy resin landfill.Then, for each minus plate on surface is put into the chamber one by one, with the glass epoxy board of high 20mm, wide 2mm and Surface Vertical erect and fixed by binder resin, the cell of 640 same sizes of cardinal principle of making (plane 8 * 8mm), thus produce the cross section capacitor element manufacturing reaction vessel as shown in Figure 1 of each chamber.
2. the making of capacitor
The tantalum sintered object of CV10 ten thousand μ FV/g (size 4.5 * 3.0 * 1.0mm, quality 84mg, draw lead-in wire and be φ 0.40mm, expose 7mm on the surface) is used as electric conductor.The boiling of the solution on lead-in wire when preventing that semiconductor layer in the subsequent handling from forming and the packing ring of the tetrafluoroethene system of installation.With the top 2mm of the lead-in wire of 32 such electric conductors, the position from distance end 25mm on the plate of the stainless steel of length 360mm, width 20mm, thickness 2mm begins with the 10mm interval, is welded to connect with arranging.The same corrosion resistant plate that is connected with 32 electric conductors of preparing 20, with each corrosion resistant plate with the interval of 10mm, abreast its termination as one man is installed to can to set on the metal framework of 640 electric conductors in same direction.At the electrolytic bath that 0.1% phosphate aqueous solution is housed of preparing separately framework is set, be immersed in after mode in the aqueous solution configures by the part with electric conductor and lead-in wire, the tantalum plate that arranges take framework as anode, in the electrolytic bath is as negative electrode, add the voltage of 10V, make the aqueous solution be 80 ℃ and carry out 6 hours change into, after from groove, mentioning, wash, drying, a part inner at the pore of electric conductor and surface and lead-in wire has formed by Ta
2O
5The dielectric layer that consists of.Then, only the electric conductor of framework is steeped in 1% the naphthalene-2 sulfonic acid molten iron solution, mention, repeat after 7 times the washing and drying, be configured, so that 640 electric conductors of framework are immersed in respectively, in each chamber, is furnished with 30% glycol water that added 3% anthraquinone-2-sulfonic acid and ethylidene dioxy thiophene more than the saturated concentration with equal height, in 640 chambers of the reaction vessel of capacitor element manufacturing usefulness, take framework as anode, take the current-collecting terminals of the exterior bottom of reaction vessel as negative electrode, under 13.5V, room temperature energising one hour, thus semiconductor layer formed.Mention framework, wash, after the ethanol washing, drying, be configured, so that be the part of dipping electric conductor and lead-in wire in the above-mentioned electrolytic bath of 0.1% acetic acid at forming liquid, under 7V, 15 minutes, 80 ℃ condition, change into again.Framework is mentioned, wash, ethanol washing, drying.Such semiconductor layer is formed, changes into work again and repeatedly carry out 5 times, make final semiconductor layer.And then, by framework being set and carrying out drying to stick with paste the mode of sequentially flooding the electric conductor part in the groove at carbon paste groove and silver, thus on semiconductor layer stacked electrode layer.
Each electric conductor that has formed electrode layer is taken off from framework, the lead portion of electric conductor ground is cut off the anode-side of the two ends head that is positioned in the lead frame that the copper alloy by electroplating surfaces with tin prepared separately makes after removing, silver at cathode side mounting electric conductor is stuck with paste side, the former connects by spot welding, and the latter sticks with paste with silver and connects., by epoxy resin sealing after, carry out cut-out, the bending machining of lead frame, thereby produce the chip capacitor of size 7.3 * 4.3 * 1.8mm thereafter.Then, 115 ℃, be to carry out 5 hours aging under the condition of 3.5V to the applied voltage of capacitor.The appearance capacitance profile of resulting capacitor is in the scope of its average capacitance ± 10%.Specifically, resulting capacitor, specified 2.5V electric capacity is 680 μ F, have 594 be 720～645 μ F, 17 be 720～750 μ F, 29 be the capacitance profile of 645～610 μ F.
Comparative example 1:
For embodiment 1, do not use capacitor element manufacturing reaction vessel of the present invention, and in reaction vessel in the past, namely size identical but do not have each chamber, do not have each minus plate and the current source of electric current sucking-off type, below container inside be provided with floor space substantially the copper of identical size implemented in the reaction vessel of gold-plated minus plate, thereby form semiconductor layer take this minus plate as negative electrode, by switching on, in addition, produce similarly to Example 1 chip capacitor.The appearance capacitance profile of resulting capacitor exceeds its average capacitance ± 20%.Specifically, resulting capacitor, specified 2.5V electric capacity is 680 μ F, have 359 be 720～645 μ F, 15 be 720～750 μ F, 2 be 750～780 μ F, 150 be 645～610 μ F, 93 be 610～575 μ F, 17 be 575～540 μ F, 4 be the capacitance profile of 540～510 μ F.
Can know from embodiment 1 and comparative example 1, its capacitance profile of capacitor group that obtains in embodiment 1 is narrow than the capacitor group that obtains in comparative example 1 obviously.
Embodiment 2:
1. the capacitor element manufacturing making of reaction vessel
Compare with embodiment 1, the minus plate of each cell of reaction vessel is not made by printing technology, but be in the 14mm scope in the bottom of each cell and the height apart from the bottom of side, stuck with paste by the silver of silver powder 93 quality %, epoxy resin 7 quality % that to retouch out thickness be that the full coat section of 0.3mm is as minus plate, from the F-101L of stoneman electronics (strain) system, select using as current regulator diode of 60～100 μ A, in addition, produce similarly to Example 1 reaction vessel.
2. the making of capacitor
To utilize the hydrogen brittleness of niobium ingot and pulverize powder of niobium (average grain diameter 0.32 μ m) granulation of formation, thus obtain average grain diameter 110 μ m the niobium powder (so because be the micro mist surface by autoxidation, have the oxygen of 95000ppm).Then, by placing it in 450 ℃ the blanket of nitrogen and then be placed in 700 ℃ the argon, thereby make the niobium powder (CV298000 μ FV/g) of the part nitrogenize of nitrogenize amount 9600ppm.By with the niobium line of this niobium powder and Φ 0.37mm is common be shaped after, carry out sintering at 1280 ℃, producing a plurality of sizes is 4.0 * 3.5 * 1.7mm (quality 0.08g.The niobium line becomes lead-in wire, and sintered body inside exists 3.7mm, outside to have 8mm.) sintered body (electric conductor).Then, after similarly to Example 1 corrosion resistant plate connects the electric conductor of equal number, on metal framework, set with equal number.Change into by only voltage being decided to be 20V, thereby formed with Nb in the part of electric conductor surface and lead-in wire
2O
5Dielectric layer for principal component.
Then, after being placed on the capacitor element manufacturing in the low temperature chamber that is controlled in 12 ℃ with reaction vessel, the anthraquinone-2-sulfonic acid of embodiment 1 is replaced to the pyrroles, and will switch on voltage and again formation voltage be decided to be respectively 23V and 14V, and will be decided to be 90 minutes conduction time, reaction times be decided to be 11 times, in addition, carry out similarly to Example 1, form semiconductor layer, electrode layer, seal, thereby produce the chip solid electrolyte capacitor that size is 7.3 * 4.3 * 2.8mm.The appearance capacitance profile of resulting capacitor is in the scope of its average capacitance ± 15%.Specifically, resulting capacitor, specified 4V electric capacity is 1000 μ F, have 579 be 950～1050 μ F, 13 be 1050～1100 μ F, 44 be 950～900 μ F, 4 be the capacitance profile of 900～850 μ F.
Comparative example 2:
Compare with embodiment 2, do not use capacitor element manufacturing reaction vessel of the present invention, but use the reaction vessel in the past of in comparative example 1, using to make capacitor, in addition, carry out similarly to Example 2, produce chip solid electrolyte capacitor.The appearance capacitance profile of resulting capacitor exceeds its average capacitance ± 20%.Specifically, resulting capacitor, specified 4V electric capacity is 1000 μ F, have 365 be 950～1050 μ F, 7 be 1050～1100 μ F, 172 be 950～900 μ F, 68 be 900～850 μ F, 19 be 850～800 μ F, 6 be 800～750 μ F, 3 be the capacitance profile of 750～700 μ F.
Can know from embodiment 2 and comparative example 2, the capacitor group that obtains in embodiment 2, its capacitance profile be narrow than the capacitor group that obtains in comparative example 2 obviously.
Utilizability on the industry
The invention provides and a kind ofly switch on by constant-current source, the capacitor element manufacturing manufacture method of reaction vessel and capacitor element that forms thus semiconductor layer, according to the present invention, can access occur capacitance profile narrow, have a capacitor group that the capacitance profile of electric capacity in the scope of average capacitance ± 20% occur.
Claims (9)
1. capacitor element manufacturing reaction vessel, it is characterized in that, it be in the electrolyte that will be immersed in simultaneously at a plurality of electric conductors that the surface has formed dielectric layer reaction vessel, utilize electrifying method to form the reaction vessel of semiconductor layer, in reaction vessel, be provided with each chamber corresponding with each electric conductor, in each chamber, negative electrode is set, has a plurality of constant-current sources that are being connected with each cathodic electricity.
2. capacitor element manufacturing reaction vessel as claimed in claim 1, a plurality of constant-current sources are made of a plurality of current regulator diodes, are electrically connected between its each negative electrode, and each anode is being connected with negative electrode.
3. capacitor element manufacturing reaction vessel as claimed in claim 1 or 2, be configured in reaction vessel bottom inside each negative electrode and be configured in the anodic bonding of each current regulator diode in the outside of reaction vessel, be electrically connected between the negative electrode of each current regulator diode, thus on terminal current collection.
4. capacitor element manufacturing reaction vessel as claimed in claim 1 or 2, a face that is arranged on the insulating properties substrate is that lip-deep each negative electrode and another face of being configured in the insulating properties substrate are that each current regulator diode on the back side is electrically connected by through hole, and the insulating properties substrate that through hole is sealed is as the bottom of reaction vessel.
5. capacitor element manufacturing reaction vessel as claimed in claim 3, a face that is arranged on the insulating properties substrate is that lip-deep each negative electrode and another face of being configured in the insulating properties substrate are that each current regulator diode on the back side is electrically connected by through hole, and the insulating properties substrate that through hole is sealed is as the bottom of reaction vessel.
6. capacitor element manufacturing reaction vessel as claimed in claim 4, minus plate is membranaceous metal material.
7. capacitor element manufacturing reaction vessel as claimed in claim 5, minus plate is membranaceous metal material.
8. the manufacture method of a capacitor element is characterized in that, right to use requires each the described capacitor element manufacturing reaction vessel in 1～7.
9. the manufacture method of a capacitor element, it is characterized in that, the described capacitor element manufacturing of in claim 1～7 each is with filling with electrolyte in the reaction vessel, a plurality of electric conductors that will have dielectric layer are immersed in the above-mentioned electrolyte, take this conduction side as anode, take each negative electrode of in reaction vessel, arranging as negative electrode, utilize electrifying method to form semiconductor layer at dielectric layer.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP262246/2004 | 2004-09-09 | ||
| JP2004262246 | 2004-09-09 | ||
| PCT/JP2005/017005 WO2006028286A1 (en) | 2004-09-09 | 2005-09-08 | Reaction vessel for manufacturing capacitor element, method for manufacturing capacitor element, capacitor element, and capacitor |
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| CN101015030A CN101015030A (en) | 2007-08-08 |
| CN101015030B true CN101015030B (en) | 2013-01-02 |
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| CN2005800303003A Active CN101015030B (en) | 2004-09-09 | 2005-09-08 | Reaction vessel for producing capacitor element, production method for capacitor element, capacitor element and capacitor |
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| JP (1) | JP4717824B2 (en) |
| KR (1) | KR101142310B1 (en) |
| CN (1) | CN101015030B (en) |
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| JP5271023B2 (en) * | 2008-10-07 | 2013-08-21 | Ａｖｘタンタルアジア株式会社 | Solid electrolytic capacitor and manufacturing method thereof |
| JP4620184B2 (en) * | 2009-03-17 | 2011-01-26 | 昭和電工株式会社 | SOLID ELECTROLYTIC CAPACITOR ELEMENT, ITS MANUFACTURING METHOD, AND ITS MANUFACTURING JIG |
| US8792225B2 (en) | 2009-12-21 | 2014-07-29 | Showa Denko K.K. | Partitioned reaction container for manufacturing capacitor element including openable and closable passage |
| ES2898963T3 (en) | 2017-02-13 | 2022-03-09 | Grenzebach Envelon Gmbh | Panel for a PV module and PV module |
| CN110379627A (en) * | 2019-05-31 | 2019-10-25 | 益阳艾华富贤电子有限公司 | A kind of preparation process and solid-liquid mixed capacitor of solid-liquid mixed capacitor |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6139592A (en) * | 1997-06-19 | 2000-10-31 | Sanyo Electric Co., Ltd. | Process and apparatus for producing organic solid electrolyte capacitor |
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| US4192721A (en) * | 1979-04-24 | 1980-03-11 | Baranski Andrzej S | Method for producing a smooth coherent film of a metal chalconide |
| JPH0722075B2 (en) * | 1987-01-23 | 1995-03-08 | 日通工株式会社 | Method for forming semiconductor layer of solid electrolytic capacitor |
| JPS63249323A (en) * | 1987-04-06 | 1988-10-17 | 松下電器産業株式会社 | Solid electrolytic capacitor |
| JPH01121919A (en) * | 1987-11-06 | 1989-05-15 | Mitsubishi Electric Corp | Coordinate input device |
| JPH0536267Y2 (en) * | 1988-02-12 | 1993-09-14 | ||
| JP2836098B2 (en) * | 1989-05-12 | 1998-12-14 | 松下電器産業株式会社 | Method for manufacturing solid electrolytic capacitor |
| JP3408125B2 (en) * | 1997-11-14 | 2003-05-19 | 三洋電機株式会社 | Method and apparatus for manufacturing organic solid electrolytic capacitor |
| CN1220997C (en) * | 1998-05-22 | 2005-09-28 | 松下电器产业株式会社 | Electrolytic condenser and its manufacturing method |
| US6671168B2 (en) * | 2001-11-30 | 2003-12-30 | Matsushita Electric Industrial Co., Ltd. | Solid electrolytic capacitor and method for manufacturing the same |
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- 2005-09-08 WO PCT/JP2005/017005 patent/WO2006028286A1/en active Application Filing
- 2005-09-08 KR KR1020077006353A patent/KR101142310B1/en active IP Right Grant
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| US6139592A (en) * | 1997-06-19 | 2000-10-31 | Sanyo Electric Co., Ltd. | Process and apparatus for producing organic solid electrolyte capacitor |
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| Publication number | Publication date |
|---|---|
| WO2006028286A1 (en) | 2006-03-16 |
| TWI417917B (en) | 2013-12-01 |
| KR101142310B1 (en) | 2012-05-17 |
| JPWO2006028286A1 (en) | 2008-05-08 |
| TW200615991A (en) | 2006-05-16 |
| CN101015030A (en) | 2007-08-08 |
| KR20070053769A (en) | 2007-05-25 |
| JP4717824B2 (en) | 2011-07-06 |
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