WO2010003874A2 - Verfahren zur herstellung von elektrolytkondensatoren - Google Patents
Verfahren zur herstellung von elektrolytkondensatoren Download PDFInfo
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- WO2010003874A2 WO2010003874A2 PCT/EP2009/058308 EP2009058308W WO2010003874A2 WO 2010003874 A2 WO2010003874 A2 WO 2010003874A2 EP 2009058308 W EP2009058308 W EP 2009058308W WO 2010003874 A2 WO2010003874 A2 WO 2010003874A2
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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
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/48—Conductive polymers
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/54—Electrolytes
- H01G11/56—Solid electrolytes, e.g. gels; Additives therein
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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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Definitions
- the invention relates to a process for the preparation of electrolytic capacitors with low equivalent series resistance, electrolytic capacitors produced by this process and the use of such electrolytic capacitors.
- a commercially available solid electrolytic capacitor is usually composed of a porous metal electrode, an oxide layer on the metal surface, an electrically conductive solid introduced into the porous structure, an external electrode (contacting portion) such as a metal substrate. a silver layer or a metal foil with a separator, as well as further electrical contacts and a Verkapselu ⁇ g.
- solid electrolytic capacitors are tantalum, aluminum, niobium and niobium oxide capacitors with charge transfer complexes, brownstone or polymer solid electrolytes.
- porous bodies has the advantage that, due to the large surface area, a very high capacity density, i. high electrical capacity in a small space.
- ⁇ -conjugated polymers are particularly suitable as solid electrolytes.
- ⁇ -conjugated polymers are also referred to as conductive polymers or as synthetic metals. They are increasingly gaining economic importance because polymers have advantages over metals in terms of processability, weight, and targeted chemical properties modification.
- Examples of known ⁇ -conjugated polymers are polypyrroles, polythiophenes, polyanilines, polyacetylenes, polyphenylenes and poly (p-phenylene-vinylenes), where a particularly important and industrially used polythiophene is the poly-3 ) 4- (ethylene-l s 2 -dioxy) thiophene, often referred to as poly (3,4-ethylenedioxythiophene), because it has a very high conductivity in its oxidized form.
- ESR equivalent series resistances
- European Patent EP-B-340 512 describes the preparation of a solid electrolyte from 3,4-ethylene-1,2-dioxythiophene and the use of its cationic polymer prepared by oxidative polymerization as solid electrolyte in electrolytic capacitors.
- a disadvantage of this and similar methods is that the conductive polymer is generated by polymerization in situ in the electrolytic capacitor.
- the monomer e.g. 3,4-ethylene-l, 2-dioxythiophene, and oxidizing agent in the presence of solvents together or sequentially introduced into the porous Metuüisson and then polymerized.
- Such a chemical reaction is in the production of electronic
- oxidizing agents can damage the dielectric (oxide layer) on the metal electrode.
- transition metal salts e.g. Fe (III) salts used.
- the reduced metal salts e.g. Fe (II) salts in the electrode body.
- this is expensive and does not succeed completely, i. residues of the metal salts always remain in the electrode body.
- transition metals in particular can damage the dielectric, so that the resulting increased residual currents significantly reduce the life of the capacitors or even make it impossible to use the capacitors under harsh conditions, such as high temperatures and / or high air humidity.
- Polymerization of monomers can also be carried out electrochemically in the absence of oxidants.
- the electrochemical polymerization requires that first a conductive film is deposited on the insulating oxide layer of the metal electrode. This in turn requires an in-situ polymerization with all the disadvantages listed above. Finally, this layer then has to be electrically contacted for each individual metal electrode become. This Kontakltechnik is very expensive in mass production and can damage the oxide layer.
- the electrodeposition in the pores of the porous metal electrode is very difficult because the deposition due to the electric potential course occurs primarily on the outside of the electrode body.
- polymer solutions are adjusted to a pH of 5.4 to 8.1 so as not to corrode the dielectric of the electrolyte-controlling agent and thereby lower the ESR.
- the use of polymer solutions with a pH of 1.2 to 1.6 for the production of solid electrolytic capacitors leads to very high ESR values.
- the solid electrolyte of an electrolytic capacitor is prepared by means of a dispersion containing particles of poly (3,4-ethylenedioxythiophene) / polystyrene sulfonate having an average diameter of 1-100 nm.
- dispersions having a pH of 6 are used so as not to damage the dielectric.
- the object was therefore to provide such a method and the capacitors thus improved.
- a pH greater than or equal to 1.8 and less than or equal to 3.9 has, surprisingly, a very positive influence on the ESR of the solid electrolyte. This is particularly surprising since, according to previous findings, in particular in the case of corrosion-sensitive dielectrics such as aluminum oxide, the dielectric is attacked at such pH values and the ESR is increased.
- the subject matter of the present invention is therefore a process for producing an electrolyte capacitor, at least comprising
- a) on a porous body at least comprising a porous electrode body (2) of an electrode material and a dielectric (3) covering the surface of said electrode material,
- the pH of the dispersion A) measured at 25 ° C is greater than 1.8 and less than or equal to 3.9.
- the pH of the dispersion A) is preferably greater than or equal to 2 and less than or equal to 3.5, more preferably greater than or equal to 2 and less than or equal to 3, most preferably greater than or equal to 2 and less than or equal to 2.8, the pH being 25 ° C is measured.
- bases or acids can be added to the dispersions.
- bases inorganic bases, such as sodium hydroxide, potassium hydroxide, calcium hydroxide or ammonia, or organic bases, such as ethylamine, diethyamine, triethylamine, propyiamine, dipropylamine, tripropylamine, isopropylamine, diisopropylamine, butylamine, dibutylamine, tributylamine, isobutylamine, diisobutylamine, triisobutylamine, 1-methylpropylamine, methylethylamine, bis (1-methyl) propylamine, 1,1-dimethylethylamine, pentylamine, dipentylamine, tripentylamine, 2-pentylamine, 3-pentylamine, 2-methylbutylamine, 3-methylbutylamine, bis (3-methylbutyiamine), Tris (3-methylbutylamine), hexylamine),
- amine N, N-dimethylpropyl, N-Ethyld ⁇ sopropylamin, allylamine, diallylamine, ethanolamine, diethanolamine, Triethanolamine, methylethanolamine, methyldiethanolamine, dimethylethanolamine, diethylethanolamine, N-butyethanolamine, N-butyldiethanolamine, dibutylethanolamine, cyclohexylethanolamine, cyclohexyldiethanolamine, N-ethyl lethanolamine, N-propylethanolamine, tert-butylethanolamine tert-butyldiethanolamine, propanolamine, dipropanolamine, tripropartolamine or benzylamine.
- inorganic acids such as sulfuric acid, phosphoric acid or nitric acid
- organic acids such as carboxylic or sulfonic acids
- the particles B) of the dispersion A) have a specific electrical conductivity of greater than 100 S / cm in the dry state.
- the specific electrical conductivity of the particles B) in the dry state is the specific electrical conductivity of the fiim in the dry state, which forms on drying of the dispersion A) from the particles B).
- Dispersions A) are preferably used whose particles B) in the dried state have a specific electrical conductivity of greater than 150 S / cm, more preferably greater than 200 S / cm, very preferably greater than 250 S / cm, most preferably greater than 300 S / cm and in a particularly preferred embodiment have greater than 400 S / cm.
- the viscosity of the dispersion A) can mPa-s (measured with a Rheometcr at 20 0 C and a shear rate of 100 s depending on the type of application between 0.1 and 1000 be "1).
- the viscosity is preferably 0.1 to 500 MPA s, more preferably between 1 to 200 mPa s, most preferably 1 to 300 mPa s and most preferably 1 to 50 tnPas.
- the solids content of the dispersion A) is 0.1-90% by weight (% by weight), preferably 0.1-30% by weight, very particularly preferably 0.3-10% by weight and very preferably 0.5-5% by weight. -%.
- the solids content is determined by drying the dispersion A) at a temperature sufficiently high to remove the dispersant but not decomposing the solid.
- the particles B) of the conductive polymer in the dispersion A) in the process have an average diameter of 1 to 100 nra, preferably an average diameter of 1 to 80 ⁇ m, particularly preferably 1 to 50 nm and very particularly preferably 5 to 40 nm.
- the determination of the diameter of the particles B) takes place via an ultracentrifuge measurement.
- the general procedure is in Colloid Polym. Be. 267, 1113-1116 (1989).
- a diameter distribution of the particles B) refers to a mass distribution of the particles in the dispersion as a function of the particle diameter.
- the particles B) of the conductive polymer in the dispersion A) preferably have a dgo value of the diameter distribution of less than 150 nm, particularly preferably less than 100 nm, very particularly preferably less than 80 nm and more preferably less than 50 nm.
- the particles B) of the conductive polymer in the dispersion A) preferably have in the method a ⁇ 0 value of the diameter distribution of greater than 1 nm, more preferably greater than 3 nm, most preferably greater than 5 nm.
- the dio value of the diameter distribution means that 10% of the total mass of all particles B) of the conductive polymer in the dispersion A) can be assigned to particles B) having a diameter smaller than or equal to the d ) 0 value.
- the d 90 value of the diameter distribution states that 90% of the total mass of all particles B) of the conductive polymer in the dispersion A) can be assigned to those particles B) which have a diameter less than or equal to the ⁇ value.
- the dispersion A) preferably contains no or only small amounts of metals and transition metals.
- Metals are understood here to mean metals or metal ions of main or Mau district magnetctallen, the latter hereinafter also referred to as transition metals, the Periodic Table of the Elements.
- transition metals in particular can damage the dielectric, so that the resulting increased residual currents significantly reduce the life of the capacitors or even make it impossible to use the capacitors under harsh conditions, such as high temperatures and / or high air humidity.
- the dispersion A) in the process preferably has a content of metals less than 5000 mg / kg, more preferably less than 1000 mg / kg, most preferably less than 200 mg / kg.
- metals are, for example, Na, K, Mg, Ai, Ca, Fe, Cr, Mn, Co, Ni, Cu, Ru 3 Ce or Zn called.
- the dispersion A) in the process preferably has a content of transition metals of less than 1000 mg / kg, more preferably less than 100 mg / kg, most preferably less than 20 mg / kg.
- transition metals here are, for example, Fe, Cu, Cr, Mn, Ni 5 Ru, Ce, Zn or Co called.
- the dispersion A) in the process preferably has an iron content of less than 1000 mg / kg, particularly preferably less than 100 mg / kg, very particularly preferably less than 20 mg / kg.
- the low concentrations of metals in the dispersions have the great advantage that the dielectric is not damaged in the formation of the solid electrolyte and in later operation of the capacitor.
- the electrode material forms a porous body with a high surface area in the electroytic capacitor produced by the process according to the invention, and is in the form of a porous, for example Sintered body or a roughened film before.
- this porous body will also be referred to for short as the electrode body.
- the electrode body covered with a dielectric is also referred to below as the oxidized electrode body.
- the term "oxidized electrode body” also includes those electrode bodies that are covered with a dielectric that was not produced by oxidation of the electrode body.
- the electrode body covered with a dielectric as well as completely or partially with a solid electrolyte is also referred to below for short as the capacitor body.
- the outer surface of the capacitor body is understood to mean the outer surfaces of the capacitor body.
- polymers encompasses all compounds having more than one identical or different repeat unit.
- conductive polymers in particular the class of compounds of the ⁇ -conjugated polymers, which have an electrical conductivity after oxidation or reduction.
- Such ⁇ -conjugated polymers are preferably understood to be conductive polymers which, after the oxidation, have an electrical conductivity of the order of magnitude of at least 1 ⁇ S cm 4 .
- the particles B) of the electrically conductive polymer in the dispersion A) preferably contain at least one polythiophene, polypyrrole or polyaniline, which are optionally substituted.
- the particles B) of the electrically viable polymer in the dispersion A) comprise at least one polythiophene having repeating units of the general formula (I) or the general formula (H) or the general formula (X) or repeating units of the formulas (I) and (II) or recurring units of the formulas (I) and (X) or recurring units of the formulas (II) and (X) or recurring units of the formulas (I), (II) and (X)
- A represents an optionally substituted CVCs-alkylene radical
- R is independently H, a linear or branched, optionally
- substituted Ci-Cjg-alkyl radical an optionally substituted C 5 -Ci 2 - cycloalkyl radical, an optionally substituted C 6 -C 4 -aryl radical, an optionally substituted C 7 -Cj g-aralkyl radical, an optionally substituted Ci-CrHydroxya! kylrest or a Hydroxyl radical is,
- x stands for an integer from 0 to 8.
- radicals R are attached to A, they may be the same or different.
- polythiophenes having repeating units of the general formula (I) or (II) or recurring units of the general formula (I) and (I ⁇ ) in which A is an optionally substituted C 2 -C 3 -alkylene radical and x is 0 or 1 stands.
- A is an optionally substituted C 2 -C 3 -alkylene radical and x is 0 or 1 stands.
- the conductive polythiophene of the particles B) is poly (3,4-ethylenedioxythiophene), which is optionally substituted.
- the prefix Poiy- means that more than one identical or different repeating unit is contained in the polymer or polythiophene.
- the polythiophenes contain a total of n repeating units of the general formula (I) or the general formula (II) or the general formula (X) or the general formulas (I) and (II) or the general formulas (I) and (X ) or the general formulas (II) and (X) or the general formulas (I), (II) and (X), wherein n is an integer of 2 to 2,000, preferably 2 to 100.
- the recurring units of the general formula (I) or the general formula (O) or the general formula (X) or the repeating units of the general formulas (I) and (II) or the repeating units of the general formulas (I) and (X ) or the recurring units of the general formulas (II) and (X) or the repeating units of the general formulas (I), (II) and (X) may be the same or different within each polythiophene.
- polythiophenes having in each case the same recurring units of the general formula (I) or of the general formula (II) or of the general formula (X) or each having the same recurring units of the general formulas (I) and (II), or of the general formulas ( I) and (X), or the general formulas (II) and (X), or with in each case identical recurring units of the general formulas (I) 5 (II) and (X).
- Particularly preferred are polythiophenes having in each case the same recurring units of the general formula (I) or the general formula (II) or each having the same recurring units of the general formulas (I) and (II).
- the polythiophenes preferably carry H.
- C 1 -C 12 -alkylene radicals A are preferably methylene, ethylene, n-propylene, n-butylene or n-pentylene.
- d-Qg-Alalkyl R are preferably linear or branched Ci-C 1J - alkyl radicals such as methyl, ethyl, n- or iso-propyl, n-, iso-, sec- or tert-butyl, n-pentyl, 1-methylbutyl , 2-methylbutyl, 3-methylbutyl, 1-ethylpropyl, 1,1-dimethylpropyl, 1, 2-dimethylpropyl, 2,2-dimethylpropyl, n-hexyl, n-heptyl, n-octyl), 2-ethylhexyl, n-nonyl, n-decyl, n-undecyl, n-do
- the polythiophenes used as solid electrolyte in the preferred process may be neutral or cationic. In preferred embodiments, they are cationic, with "cationic" referring only to those located on the polythiophene backbone
- the polythiophenes can carry positive and negative charges in the structural unit, with the positive charges on the polythiophene backbone
- Polythiophene backbone and the negative charges are optionally present on the residues R substituted by sulfonate or carboxylate groups, whereby the positive charges of the polythiophene backbone may be partially or completely saturated by the optional anionic groups on the residues R.
- the polythiophenes can be considered in these cases However, they are all considered as cationic polythiophenes in the context of the invention, since the positive charges on the polythiophene backbone are relevant ..
- the positive charges are not shown in the formulas, since their gen The number and position are not perfectly ascertainable. However, the number of positive charges is at least 1 and at most n, where n is the total number of all repeating units (equal or different) within the polythiophene.
- the cationic polythiophenes require anions as counterions.
- Counterions may be monomeric or polymeric anions, the latter also referred to below as polyanions,
- Polymeric anions are preferred over monomeric anions because they contribute to film formation and because of their size lead to thermally more stable electrically conductive films.
- Polymeric anions can here be, for example, anions of polymeric carboxylic acids, such as polyacrylic acids, polymethacrylic or polymaleic acids, or polymeric sulfonic acids, such as polystyrenesulfonic acids and polyvinylsulfonic acids. These polycarboxylic and -sulfonic acids can also be copolymers of vinylcarboxylic and vinylsulfonic acids with other polymerizable monomers, such as acrylic acid esters and styrene ,
- an anion of a polymeric carboxylic acid or sulfonic acid is preferred as the polymeric anion.
- polystyrene sulfonic acid PSS
- the molecular weight of the polyanionic polyacids is preferably 1,000 to 2,000,000, more preferably 2,000 to 500,000.
- the polyacids or their alkali salts are commercially available, e.g. Polystyrenesulfonic acids and polyacrylic acids, or else can be prepared by known processes (see, for example, Houben Weyl, Methods of Organic Chemistry, Vol. E-20 Macromolecular Substances, Part 2, (3987), pp. 1141 and following).
- Polymer (s) anion (s) and electrically conductive polymers may in dispersion A) in particular in a weight ratio of 0.5: 1 to 50: 1, preferably from 1: 1 to 30: 1, more preferably 2: 1 to 20 : 1 be included.
- the weight of the electrically conductive polymers corresponds to the initial weight of the monomers used, assuming that complete conversion takes place during the polymerization.
- Examples of monomeric anions are those of C 1 -C 4 -alkanesulfonic acids, such as methane, etlian, propane, butane or higher sulfonic acids, such as dodecanesulfonic acid, of aliphatic perfluorosulfonic acids, such as trifluoromethanesulfonic acid, perfluorobutane stoichlonic acid or perfluorooctanesulfonic acid, of aliphatic C 1 -C -carboxylic acids such as 2-ethylhexylcarboxylic acid, aliphatic perfluorocarboxylic acids such as trifluoroacetic acid or perfluorooctanoic acid, and aromatic sulfonic acids optionally substituted by C 1 -C 4 -alkyl groups, such as benzene sulfonic acid, o-toluoic acid, p Toluenesulfonic acid or dodec
- Preferred as monomeric anions are the anions of p-toluenesulfonic acid, methanesulfonic acid or camphorsulfonic acid.
- Cationic polylhiophenes containing anions as counter ions for charge compensation are also often referred to in the art as polythiophene / (poly) anion complexes.
- the dispersions A) may contain one or more dispersion Mixtures D).
- dispersants D) which may be mentioned are the following solvents: aliphatic alcohols, such as methanol, ethanol, isopropanol and butanol; aliphatic ketones such as acetone and methyl ethyl ketone; aliphatic carboxylic esters such as EssigTalkreethy ⁇ ester and EssigTalkrebuty solid; aromatic hydrocarbons such as toluene and xylene; aliphatic hydrocarbons such as hexane, heptane and cyclohexane; Chlorinated hydrocarbons such as dichloromethane and dichloroethane; aliphatic nitriles such as acetonitrile, aliphatic sulfoxides and sulfones such as dimethylsulfoxide and sulfolane; aliphatic carboxylic acid amides such as methylacetamide, di
- Preferred dispersants D) are water or other protic solvents such as alcohols, e.g. Methanol, ethanol, i-propanol and butanol, and mixtures of water with these alcohols, particularly preferred solvent is water.
- alcohols e.g. Methanol, ethanol, i-propanol and butanol
- water particularly preferred solvent is water.
- the dispersion A) may further contain other components such as surfactants, e.g. ionic and / or nonionic surfactants; Adhesion promoters, e.g. organofunctional silanes or their hydrolysates, e.g. 3-glycidoxypropyltriaoxysilane, 3-aminopropyltriethoxysilane, 3-mercaptopropyltrimethoxysilane, 3-metacryloxypropyltrimethoxysilane, vinyltrimethoxysilane or octyltriethoxysilane; Converters such as melamine compounds, capped isocyanates, functional silanes - e.g.
- surfactants e.g. ionic and / or nonionic surfactants
- Adhesion promoters e.g. organofunctional silanes or their hydrolysates, e.g. 3-glycidoxypropyltriaoxysilane, 3-aminopropyltrie
- Tetraethoxysilane alkoxysilane hydrolysates, e.g. based on tetraethoxysilane, epoxysilanes such as 3-glycidoxypropyltrialkoxysilane ⁇ polyurethanes, polyacrylates or polyolefin dispersions, or other additives.
- the dispersions A) preferably contain further additives which increase the conductivity, for example compounds containing ether groups, for example tetrahydrofuran; lactone group-containing compounds such as ⁇ -butyrolactone, ⁇ -valerolactone; amide or lactam compounds such as Caprölactam, N-methyl caprolactam, N, N-dimethylacetamide, N-methylacetamide, N 5 ND imethyl- formamide (DMF), N-methyl formamide, N-methylformanilide, N-methylpyrrolidone (NMP), N- Octyl pyrrolidone, pyrrolidone; Sulfones and sulfoxides such as sulfolane (tetramethylene sulfene), dimethyl sulfoxide (DMSO); Sugar or sugar derivatives such as sucrose, glucose, fructose, lactose, sugar alcohols such as sorbitol, mannitol; Imides, such as succinimi
- Tetrahydrofiirane, N-methylformamide, N-methylpyrrolidone, ethylene glycol, dimethyl sulfoxide or sorbitol are particularly preferably used as conductivity-increasing additives.
- the further additives may either be present alone or in any combination thereof in dispersion A).
- the dispersions A) may also contain one or more binders.
- binders such as, for example, polyvinyl alcohols, polyvinylpyrrolidones, polyvinyl chlorides ; , Polyvinyl acetates, polyvinyl butyrates, polyacrylic acid esters, polyacrylic acid amides, polymethacrylic acid esters, polymethacrylic acid amides, polyacrylonitriles, styrene / acrylic ester, vinyl acetate / acrylic ester and ethylene / vinyl acetate copolymers, polybutadienes, polyisoprenes, polystyrenes, polyethers, polyesters, polycarbonates, polyurethanes, polyamides, polyimides, polysulfones, Melamine Formaldehyharze, epoxy resins, silicone resins or celluloses in question.
- polymeric organic binders which may be used are those which are prepared by addition of crosslinking agents, such as, for example, melamine compounds, blocked isocyanates or functional silanes, for example 3-glycidoxypropyltrialkoxysilane, tetraethoxysilane and tetraethoxysilane hydrolyzate, or crosslinkable polymers, for example polyurethanes, polyacrylates or polyolefins, and subsequent Networking are generated.
- crosslinking products suitable as polymeric tapes can also be formed, for example, by reaction of the added crosslinkers with polymeric anions optionally present in the dispersion A). Preference is given to those binders which have sufficient temperature stability to withstand the temperature stresses to which the finished capacitors are later exposed, eg brazing temperatures of 220 to 260 ° C.
- the solids content of the polymeric binder in the dispersion A) is 0.1-90% by weight, preferably 0.5-30% by weight and very particularly preferably 0.5-10% by weight.
- Fig. 1 describes a schematic representation of the structure of a solid electrolytic capacitor using the example of a tantalum capacitor with
- Fig. 2 describes the enlarged image section 10 of FIG. 2 of the schematic layer structure of the tantalum capacitor with
- Fig. 3 describes a schematic representation of the structure of a solid electrolytic capacitor using the example of an aluminum wound capacitor with
- such an electrolytic capacitor according to the invention can be produced as follows; First, e.g. a valve metal powder having a high surface area was pressed and sintered into a porous electrode body. This is usually an electrical
- Contact wire preferably from a valve metal, such. As tantalum, with pressed into the electrode body. Alternatively, metal foils may be etched to obtain a porous foil. In a wound capacitor, a porous anode foil forming the electrode body and a cathode foil are separated by a separator and wound up.
- a valve metal such as tantalum
- metal foils may be etched to obtain a porous foil.
- a porous anode foil forming the electrode body and a cathode foil are separated by a separator and wound up.
- the electrode body is then coated, for example by electrochemical oxidation, with a dielectric, ie an oxide layer.
- a dispersion A) comprising at least particles B) of an electrically conductive polymer, such as, for example, an optionally substituted polythiophene, and a Dispersionsniittel D) is applied and the D ispersionsrnittel D) is at least partially removed to form the solid electrolyte.
- further layers in FIG. 1 and FIG. 2 with a conductive outer layer (5) are applied to the outer surface of the capacitor body.
- oxidized electrode bodies are used in the form of a film which is wound up together with a separator and a cathode foil (as shown for example in Fig. 3) or stacked.
- the separator consists e.g. cellulose fibers or synthetic fibers, e.g. Polypropylene, polyester or polyamide fibers. Preference is given to containing separator papers
- valve metals are to be understood as metals whose oxide layers
- valve metals include Be, Mg, Al. Ge, Si, Sn, Sb, Bi, Ti, Zr, Hf, V, Nb, Ta and W and an alloy or compound of at least one of these metals with other elements.
- the best known representatives of the Ventümetalle are Al, Ta, and Nb.
- Compounds with a valve metal comparable electrical properties are those with metallic conductivity, which are oxidizable and their oxide layers have the properties described above.
- NbO has metallic conductivity, but is generally not considered a valve metal.
- layers of oxidized NbO have the typical properties of valve metal oxide layers such that NbO or an alloy or compound of NbO with other elements are typical examples of such compounds having comparable electrical properties to a valve metal.
- tantalum, aluminum and such electrode materials based on niobium or niobium oxide Preference is given to tantalum, aluminum and such electrode materials based on niobium or niobium oxide.
- Non-based electrode materials based on niobium or niobium oxide are understood as meaning those materials in which niobium or niobium oxide constitute the component with the greatest molar fraction.
- the niobium or niobium oxide based electrode material is preferably niobium, NbO, a niobium oxide NbO x , where x can have values of 0.8 to 1.2, niobium nitride, niobium oxynitride or mixtures of these materials or an alloy or joining at least one of these materials with other elements.
- Preferred alloys are alloys with at least one metal valve, such as Be, Mg, Al, Ge, Si, Sn, Sb, Bi, Ti, Zr, Hf, V, Nb, Ta or W.
- metal valve such as Be, Mg, Al, Ge, Si, Sn, Sb, Bi, Ti, Zr, Hf, V, Nb, Ta or W.
- oxidizable metal means not only metals, but also an alloy or compound of a metal with other elements as long as they have metallic conductivity and are oxidizable.
- the oxidizable metals are sintered into a porous electrode body in powder form, or a porous structure is impressed on a metallic body.
- the latter can e.g. by etching a foil.
- the porous electrode bodies are used, for example, in a suitable electrolyte, e.g. Phosphoric acid or an aqueous solution of Arnmoniumadipat, oxidized by applying a voltage.
- a suitable electrolyte e.g. Phosphoric acid or an aqueous solution of Arnmoniumadipat
- the height of this forming voltage depends on the oxide layer thickness to be achieved or the subsequent application voltage of the capacitor.
- Preferred forming voltages are 1 to SOO V, more preferably 1 to 300 V.
- the specific charge of the metal powder is calculated as follows:
- the capacity results from the capacity of the oxidized electrode body measured at
- the electrical conductivity of the electrolyte is sufficiently large, so that it is not yet at 120 Hz to a capacity drop due to the electrical resistance of the electrolyte comes.
- 18% aqueous sulfuric acid electrolytes are used for the measurement.
- the E ⁇ ektroden Strength used have a porosity of 10 to 90%, preferably from 30 to 80%, particularly preferably from 50 to 80%.
- the porous electrode bodies have an average pore diameter of 10 to 10,000 nm, preferably 50 to 5,000 nm, particularly preferably 100 to 3,000 nm.
- the subject of the present invention is accordingly a process for the production of electrolytic capacitors, characterized in that the valve metal or the compound has a comparable electrical properties to valve metal, such as tantalum, niobium, aluminum, titanium, zirconium, hafnium, vanadium, an alloy or Compound of at least one of these metals with other elements, NbO or an alloy or compound of NbO with other elements.
- valve metal such as tantalum, niobium, aluminum, titanium, zirconium, hafnium, vanadium, an alloy or Compound of at least one of these metals with other elements, NbO or an alloy or compound of NbO with other elements.
- the dielectric preferably consists of an oxide of the electrode material. It optionally contains further elements and / or compounds.
- the capacitance of the capacitor depends not only on the type of dielectric but also on the surface and the thickness of the dielectric.
- the specific charge is a measure of how much charge per unit weight the oxidized electrode body can accommodate. The specific charge is calculated as follows:
- the capacitance results from the capacitance of the finished capacitor measured at 120 Hz and the nominal voltage is the specified threshold voltage of the capacitor (rated voltage).
- the weight of the oxidized electrode body refers to the net weight of the dielectric-coated porous electrode material without polymer, contacts, and encapsulations.
- the electrolytic capacitors produced by the novel process preferably have a specific charge of 500 to 500,000 ⁇ C / g, more preferably a specific charge of 2,500 to 250,000 ⁇ C / g, most preferably a specific charge of 2,500 to 1,500,000 ⁇ C / g, most preferably one specific charge of 5000 to 100000 ⁇ C / g.
- precursors for the preparation of conductive polythiophenes of the particles B) in the dispersion A hereinafter also referred to as precursors, corresponding monomers or their Derivatives understood. It is also possible to use mixtures of different precursors.
- suitable monomeric precursors are optionally substituted thiophenes, preferably optionally substituted 3,4-alkylenedioxythiophenes, 3,4-alkylethylenethiathiophenes or thieno [3,4-b] thiophenes.
- 3,4-Alkylenoxythiathiophene or thieno [3,4-b] th ⁇ ophene are exemplified the compounds of general formula (III) or the general formula (IV) or the general formula (XI) or a A mixture of thiophenes of the general formulas (III) and (IV) or a mixture of thiophenes of the general formula (III) and (XI), or a mixture of thiophenes of the general formula (IV) and (XI) or a mixture of thiophenes of general formula (III), (IV) and (XI)
- a ' is an optionally substituted C r C 5 -alkylene radical, preferably an optionally substituted C 2 -C 3 -alkylene radical,
- R is a linear or branched, optionally substituted Ci-Cjs-alkyl radical, preferably linear or branched, optionally substituted C 5 -C 14 -alkyl radical, an optionally substituted Cs-C ⁇ -cycloalkyl radical, an optionally substituted C f i-C ⁇ -aryl radical , an optionally substituted C ⁇ -Cig-aralkyl radical, a given if substituted C 1 -C 4 -hydroxyalkyl radical, preferably optionally substituted C 1 -C 2 -hydroxyalkyl radical, or a hydroxyl radical,
- x is an integer from 0 to 8, preferably from 0 to 6, particularly preferably 0 or] and
- radicals R are attached to A, they may be the same or different.
- Particularly preferred monomeric precursors are optionally substituted 3,4-ethylenedioxythiophenes.
- R and x have the meaning given for the general formulas (IH) and (FV).
- derivatives of these monomeric precursors are, for example, dimers or trimers of these monomeric precursors. They are also high molecular weight derivatives, i. Tetramers, pentamers, etc. of the monomeric precursors as derivatives possible.
- n is an integer from 2 to 20, preferably 2 to 6, particularly preferably 2 or 3, and
- the derivatives can be constructed from the same or different monomer units and can be used in pure form and mixed with one another and / or with the monomer precursors.
- oxidized or reduced forms of these precursors are also encompassed by the term "precursors", provided that the same conductive polymers are formed during their polymerization as in the precursors listed above.
- radicals mentioned for the abovementioned precursors in particular for the thiophenes, preferably for the 3,4-alkylenedioxythiophenes, the radicals mentioned for the general formulas (III), (IV) or (XI) for R are suitable.
- radicals A and / or the radicals R are the organic groups mentioned in connection with the general formulas (I), (II) or (X)
- the 3,4-alkylene-oxythiathiophenes of the formula (III) required for the preparation of the polythiophenes to be used are known to the person skilled in the art or can be prepared by known processes (for example according to P. Blanchard, A. Cappon, E. Levillain, Y. Nicolas, P Frere and J. Roneali, Org. Lett., 4 (4), 2002, pp. 607-609).
- thieno [3,4-b] thiophenes of the formula (XI) required for the preparation of the polythiophenes to be used are known to the person skilled in the art or can be prepared by known processes (for example according to US2004 / 0074779A1).
- the dispersions are prepared from the precursors described above, for example analogously to the conditions mentioned in EP-A 440 957.
- An improved variant for the preparation of the dispersions is the use of ion exchangers for the removal of the inorganic salt content or a part thereof. Such a variant is described for example in DE-A 19627071.
- the ion exchanger can, for example, be stirred with the product or the product is conveyed through a column filled with ion exchange column.
- the use of the ion exchanger can achieve the low metal contents described above.
- the particle size of the particles B) in the dispersion A) can be reduced, for example, by means of a high-pressure homogenizer. This process can also be repeated to increase the effect. Especially pressures between 100 and 2000 bar have proved to be advantageous in order to greatly reduce the particle size.
- the particles B) of the conductive polymer preferably form a stable dispersion.
- even unstable dispersions may be used by, for example, stirring, rolling or shaking them prior to use to ensure even distribution of the particles B).
- the dispersions A) are prepared by known methods, e.g. by spin-coating, impregnation, pouring, dripping, spraying, spraying, tinting, brushing or printing, for example ink-jet, screen or pad printing, applied to the dielectric of the electrode body.
- the penetration of the dispersion into the porous electrode body can be facilitated for example by over or under pressure, vibration, ultrasound or heat.
- the application may be directly or using a coupling agent, for example a silane, e.g. organofunctional silanes or their hydrolysates, e.g. 3-glycidoxypropyltrialkoxysilane, 3-aminopropyltriethoxysilane, 3-mercaptopropyltrimethoxysilane, 3-methacryloxypropyltrimethoxysilane, vinyltrimethoxysilane or octyltriethoxysilane, and / or one or more other functional layers to the dielectric of the electrode body.
- a silane e.g. organofunctional silanes or their hydrolysates, e.g. 3-glycidoxypropyltrialkoxysilane, 3-aminopropyltriethoxysilane, 3-mercaptopropyltrimethoxysilane, 3-methacryloxypropyltrimethoxysilane, vinyltrimethoxysilane or octyltri
- the dispersant D) is preferably removed so that the solid electrolyte can be formed from the particles B) and optionally further additives in the dispersion. However, it is also possible for at least part of the dispersant D) to remain in the solid electrolyte.
- Removal of the dispersant D) after application of the dispersion may be accomplished by simple evaporation at room temperature. Beitungsgeschwyertechniken to achieve higher processed, it is advantageous to remove the dispersing agent D) at elevated temperatures, for example at temperatures of 20 to 30O 0 C, preferably from 40 up to 250 0 C to remove.
- a thermal aftertreatment can immediately with the removal of the Solvents are connected or else made at a time interval from the completion of the coating.
- the duration of the heat treatment is 5 seconds to several hours, depending on the type of dispersion used for the coating. Temperature profiles with different temperatures and residence times can also be used for the thermal treatment.
- the heat treatment may e.g. be carried out in such a way that one moves the coated oxidized electrode body at such a speed through a heat chamber at the desired temperature, that the desired residence time is reached at the selected temperature, or with a desired temperature at the desired heating plate for the desired residence time brings in contact.
- the heat treatment can be carried out, for example, in one or more heating furnaces, each with different temperatures.
- oxidized electrode body it may be advantageous to impregnate the oxidized electrode body a further number of times with the dispersions in order to achieve thicker polymer layers and / or greater coverage of the dielectric surface.
- the application of the dispersion A) and the at least partial removal of the dispersant D) takes place several times.
- the coverage of the dielectric with the solid electrolyte can be determined as follows: The capacitance of the capacitor is measured in the dry and wet state at 120 Hz. The degree of coverage is the ratio of the capacity in the dry state to the capacity in the wet state expressed as a percentage. Dry state means that the condenser was dried for several hours at elevated temperature (80-120 0 C) before being measured. Wet condition means that the condenser is exposed to saturated air humidity at elevated pressure over several hours, for example in a steam pressure vessel. The moisture penetrates into pores that are not covered by the solid electrolyte, where it acts as a liquid electrolyte.
- the coverage of the dielectric by the solid electrolyte is preferably greater than 50%, more preferably greater than 70%, most preferably greater than 80%.
- conductive layers such as a conductive outer layer
- a polymeric outer layer for example as in European Patent Application EP-A 1 524 678 described, applied.
- Other highly conductive layers such as graphite and / or silver layers serve as a current collector.
- a cathode foil which is separated from the capacitor body (anode foil) by a separator serves as a current collector.
- the capacitor is optionally contacted and finally encapsulated.
- the present invention further provides a dispersion containing at least particles comprising an electrically conductive polythiophene which is optionally substituted, and a dispersion medium, characterized in that the pH of the dispersion measured at 25 ° C is greater than 1.8 and less than or equal to 3.9 preferably greater than or equal to 2 and less than or equal to 3.5, particularly preferably greater than or equal to 2, more preferably greater than or equal to 2 and less than or equal to 2.8, and in that the particles containing a polythiophene in the dry state have a specific electrical conductivity greater than 100 S / cm own.
- the same preferred ranges as the preferred ranges mentioned above apply to the dispersion A) from the process according to the invention.
- the process according to the invention and the dispersion according to the invention thus make it possible to produce solid electrolyte capacitors with low equivalent series resistance (ESR) 5 in which no in situ polymerization is required.
- ESR equivalent series resistance
- the electrolytic capacitors produced by the method according to the invention constitute a further subject of the present invention.
- the electrolytic capacitors produced according to the invention are outstandingly suitable for use as components in electronic circuits, for example as a filter capacitor or decoupling capacitor.
- electronic circuits such as those found in computers (desktop, laptop, server), computer peripherals (e.g., PC cards), portable electronic devices such as personal computers.
- computers desktop, laptop, server
- computer peripherals e.g., PC cards
- portable electronic devices such as personal computers.
- Mobile phones digital cameras or consumer electronics, in consumer electronic devices, e.g. in CD / DVD players and computer game consoles, in navigation systems, in
- Telecommunications equipment in household appliances, in power supplies or in the automotive electronics.
- Poly (3,4-ethylenedioxythiophene) / polystyrenesulfonate dispersion was homogenized ten times at a pressure of 700 bar with a high-pressure homogenizer. Subsequently, the
- the pH of the dispersion A) -I was 1.6 at 25 ° C.
- the dispersion A) -I was adjusted to a pH of 2 by means of ammonia water.
- the viscosity of the dispersion A) -2 thus prepared was 34 mPa * s at a shear rate of 100 Hz and 20 ° C.
- Dispersion A) -2 had the following particle size distribution:
- the diameter of the particles B) of the conductive polymer refers to a mass distribution of the particles B) in the dispersion depending on the particle diameter. The determination was made by an ultracentrifuge measurement. The particle size was determined in the swollen state of the particles. An ICP analysis of the metal contents of dispersion A) -2 gave the following values:
- a porous 92 mm aluminum foil sized 170 mm 5 mm (anode foil) and a porous aluminum foil 200 mm 5 mm thick (cathode foil) were each provided with a contact wire and then together with two cellulose separator papers as shown in FIG wound up and fixed with an adhesive tape. 10 of these oxidized electrode bodies were produced. The separator of the oxidised electrode bodies were then carbonized in an oven at 300 0 C. 3.2 Preparation of the solid electrolyte
- the pH of the dispersion A) -I was adjusted by the addition of ammonia water to a value of 1.8 at 25 ° C.
- the oxidized electrode bodies were soaked in this dispersion for 15 minutes. This was followed by drying at 150 0 C for 40 min. Impregnation and drying were carried out two more times.
- the mean electrical values of the 10 capacitors fabricated in the foregoing manner are given in Table 1.
- the capacitance (in microfarads) was at 120 Hz and the equivalent series resistance (ESR) (in MiUiohms) at 100 kHz using an LCR meter (Agilent 4284A). certainly.
- capacitors according to the invention from Examples 3 to 7 have significantly lower ESR values and higher capacitance values than the capacitors from the
Abstract
Description
Claims
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JP2011517103A JP5475770B2 (ja) | 2008-07-11 | 2009-07-02 | 電解コンデンサを製造するためのプロセス |
US13/003,043 US8456803B2 (en) | 2008-07-11 | 2009-07-02 | Method for production of electrolyte capacitors |
EP09780085.8A EP2297753B1 (de) | 2008-07-11 | 2009-07-02 | Verfahren zur herstellung von festelektrolytkondensatoren |
CN2009801353366A CN102150226A (zh) | 2008-07-11 | 2009-07-02 | 生产固体电解电容器的方法 |
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Also Published As
Publication number | Publication date |
---|---|
US20110164348A1 (en) | 2011-07-07 |
DE102008032578A1 (de) | 2010-01-14 |
TW201021063A (en) | 2010-06-01 |
EP2297753B1 (de) | 2017-08-30 |
CN102150226A (zh) | 2011-08-10 |
US8456803B2 (en) | 2013-06-04 |
TWI506659B (zh) | 2015-11-01 |
EP2297753A2 (de) | 2011-03-23 |
WO2010003874A3 (de) | 2010-03-18 |
JP5475770B2 (ja) | 2014-04-16 |
JP2011527513A (ja) | 2011-10-27 |
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