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US20030214776A1 - Capacitors having a high energy density - Google Patents

Capacitors having a high energy density Download PDF

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Publication number
US20030214776A1
US20030214776A1 US10/435,081 US43508103A US2003214776A1 US 20030214776 A1 US20030214776 A1 US 20030214776A1 US 43508103 A US43508103 A US 43508103A US 2003214776 A1 US2003214776 A1 US 2003214776A1
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Prior art keywords
capacitor
capacitors
electrically conductive
conductive layer
layer
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US10/435,081
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Hans-Josef Sterzel
Klaus Kuhling
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BASF SE
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Application filed by Individual filed Critical Individual
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Classifications

    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G4/00—Fixed capacitors; Processes of their manufacture
    • H01G4/002—Details
    • H01G4/018—Dielectrics
    • H01G4/06—Solid dielectrics
    • H01G4/08—Inorganic dielectrics
    • H01G4/12—Ceramic dielectrics
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G4/00—Fixed capacitors; Processes of their manufacture
    • H01G4/002—Details
    • H01G4/005—Electrodes
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G4/00—Fixed capacitors; Processes of their manufacture
    • H01G4/002—Details
    • H01G4/018—Dielectrics
    • H01G4/06—Solid dielectrics
    • H01G4/08—Inorganic dielectrics
    • H01G4/12—Ceramic dielectrics
    • H01G4/1209—Ceramic dielectrics characterised by the ceramic dielectric material
    • H01G4/1218—Ceramic dielectrics characterised by the ceramic dielectric material based on titanium oxides or titanates
    • H01G4/1227—Ceramic dielectrics characterised by the ceramic dielectric material based on titanium oxides or titanates based on alkaline earth titanates
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K1/00—Printed circuits
    • H05K1/16—Printed circuits incorporating printed electric components, e.g. printed resistor, capacitor, inductor
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K1/00—Printed circuits
    • H05K1/16—Printed circuits incorporating printed electric components, e.g. printed resistor, capacitor, inductor
    • H05K1/162—Printed circuits incorporating printed electric components, e.g. printed resistor, capacitor, inductor incorporating printed capacitors

Definitions

  • the present invention relates to capacitors comprising an inert porous shaped body onto which a first electrically conductive layer, a second layer of barium titanate and a further electrically conductive layer have been applied.
  • Capacitors perform many tasks in information technology and electric energy engineering. There has in recent times been a search for capacitors which have a high energy density and can perform the task of batteries or be used for covering short-term high load requirements.
  • Electrochemica Acta 45 (2000), 2483 to 2498 discloses electrochemical or double-layer capacitors. These devices, also known as supercapacitors or ultracapacitors, store electric energy in two capacitors which are connected in series and each have an electric double layer which is formed between the two electrodes and the ions in the electrolyte. The distance in which charge separation occurs is only a few Angstrom. As electrolytes, use is made of highly porous carbon having internal surface areas of up to 2 500 m 2 /g. As indicated by the capacitor formula
  • C is the capacitance
  • E 0 is the absolute dielectric constant
  • E is the dielectric constant of the dielectric
  • A is the area of the capacitor
  • d is the distance between the electrodes
  • Such double-layer capacitors at present achieve energy densities of from 3 to 7 Wh/kg or Wh/liter, which are far below the energy densities of conventional batteries (lithium ion batteries achieve from 150 to 200 Wh/kg). This is due to the maximum possible voltage loading being restricted to about 3.5 V by the electrochemical stability of the electrolyte.
  • Ceramic capacitors which comprise dielectrics based on barium titanate and operate at high working voltages because of the high dielectric breakdown resistance of the titanates of up to 200 V/0.1 ⁇ m are known from the prior art. However, ceramic capacitors have relatively low capacitances.
  • capacitors which comprise an inert porous shaped body onto which a first electrically conductive layer, a second layer of barium titanate and a further electrically conductive layer have been applied.
  • the capacitors of the present invention can be produced as follows:
  • An inert porous shaped body can, in a first step, be provided with a first electrically conductive layer and this can be provided with a contact.
  • a second layer of barium titanate can be applied on top of the first layer and, finally, another electrically conductive layer can be applied on top of this titanate layer and be provided with a contact.
  • the capacitors obtained in this way can be hermetically sealed, e.g. encapsulated, except for the electric contacts.
  • Suitable porous shaped bodies are in general catalyst support materials, for example those based on metal oxides such as aluminum oxide, silicon dioxide, titanium dioxide, zirconium dioxide, chromium oxide or mixtures thereof, preferably aluminum oxide, silicon dioxide, titanium dioxide, zirconium dioxide or mixtures thereof, particularly preferably aluminum oxide, zirconium dioxide or mixtures thereof, or carbides, preferably silicon carbide, having a BET surface area of from 0.1 to 20 m 2 /g, preferably from 0.5 to 10 m 2 /g, particularly preferably from 1 to 5 m 2 /g, a pore content of from 10 to 90% by volume, preferably from 30 to 85% by volume, particularly preferably from 50 to 80% by volume, and pore sizes of from 0.01 to 100 ⁇ m, preferably from 0.1 to 30 ⁇ m, particularly preferably from 1 to 10 ⁇ m.
  • metal oxides such as aluminum oxide, silicon dioxide, titanium dioxide, zirconium dioxide, chromium oxide or mixtures thereof, preferably aluminum oxide, silicon dioxide
  • the shaped bodies can have any shapes, for example rings, pellets, stars, wagon wheels, honeycombs, preferably cuboids, cylinders, rectangles or boxes of generally any size (diameter, longest edge length).
  • the size is generally in the range from 1 to 10 mm. Larger dimensions are necessary in energy engineering.
  • metals such as copper, nickel, chromium or mixtures thereof can be applied in any layer thickness, generally from 10 nm to 1 000 nm, preferably from 50 nm to 500 nm, particularly preferably from 100 nm to 200 nm.
  • the application of the electrically conductive layer to the shaped body can be carried out using all known methods such as vapor deposition, sputtering or electroless plating, preferably electroless plating.
  • electroless plating the shaped bodies are infiltrated or impregnated with suitable, commercially available plating liquids and heated to temperatures below 100° C. to deposit the metal. After metal deposition, the liquid, usually water, can be removed at elevated temperatures and, if desired, under reduced pressure.
  • the first conductive layer by heating the shaped bodies in iron carbonyl or nickel carbonyl vapors.
  • the shaped bodies can be heated to from about 150 to 200° C., and in the case of nickel to from 50 to 100° C.
  • the shaped bodies can be heated to elevated temperatures of from 50 to 100° C. in an inert atmosphere (e.g. nitrogen or argon) to produce a homogeneous metal layer. It may be advantageous to apply crystallization nuclei, e.g. nuclei based on platinum metals, likewise by impregnation with suitable liquids (see above).
  • an inert atmosphere e.g. nitrogen or argon
  • crystallization nuclei e.g. nuclei based on platinum metals, likewise by impregnation with suitable liquids (see above).
  • the first metal layer can be provided with a contact. This can be carried out, for example, by soldering a metal foil onto an area of the metal-coated shaped body (production of the first electrode).
  • a dielectric can then be applied on top of the initially produced electrode. This is advantageously carried out using dispersions of crystalline titanate particles having sizes of less than 10 nm in alcohols.
  • Such dispersions can be prepared by reaction of titanium alkoxides with barium hydroxides or strontium hydroxides in alcoholic solution as described in the German application No.: 102 21 499.9 (O.Z. 0050/53537).
  • the shaped body can be infiltrated or impregnated with such a dispersion which may contain from 5 to 60% by weight, preferably from 10 to 40% by weight, of titanate particles, followed by removal of the alcohol by increasing the temperature to 30-100° C., preferably 50-80° C., and, if desired, reducing the ambient pressure to deposit the titanium particles on the first electrode.
  • the shaped bodies can be heated to from 700 to 1 200° C., preferably from 900 to 1 100° C., in an inert gas atmosphere so that the titanate particles sinter together to form a dense film.
  • the impregnation with the titanate dispersion and the sintering can be repeated a number of times.
  • the layer thickness is generally from 10 to 1 000 nm, preferably from 20 to 500 nm, particularly preferably from 100 to 300 nm.
  • a second electrode layer can be applied in a manner analogous to that employed for the first.
  • this can be provided with a contact on the side opposite the first contact, thus producing the capacitor.
  • the latter can be hermetically encapsulated to protect it and for the purposes of insulation.
  • the capacitors of the present invention are suitable as smoothing capacitors or energy storing capacitors or phase shift capacitors in electric energy engineering and as coupling capacitors, filter capacitors or miniature energy storage capacitors in information technology.
  • capacitors of the present invention may be illustrated as follows:
  • a specific surface area (BET surface area) of the porous shaped body of 2 m 2 /g and a barium titanate layer thickness of 0.1 ⁇ m at a relative dielectric constant of 5 000 gives a capacitance calculated according to the formula on page 1, line 29, of about 1 farad/cm 3 .
  • Such a capacitor can be charged to a voltage of 200 V, and its energy density is then 20 000 Ws/cm 3 or approximately 5.5 kWh/liter.

Landscapes

  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Ceramic Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Electric Double-Layer Capacitors Or The Like (AREA)
  • Fixed Capacitors And Capacitor Manufacturing Machines (AREA)
  • Ceramic Capacitors (AREA)

Abstract

Capacitors comprising an inert porous shaped body onto which a first electrically conductive layer, a second layer of barium titanate and a further electrically conductive layer have been applied.

Description

  • The present invention relates to capacitors comprising an inert porous shaped body onto which a first electrically conductive layer, a second layer of barium titanate and a further electrically conductive layer have been applied. [0001]
  • Capacitors perform many tasks in information technology and electric energy engineering. There has in recent times been a search for capacitors which have a high energy density and can perform the task of batteries or be used for covering short-term high load requirements. [0002]
  • Electrochemica Acta 45 (2000), 2483 to 2498, discloses electrochemical or double-layer capacitors. These devices, also known as supercapacitors or ultracapacitors, store electric energy in two capacitors which are connected in series and each have an electric double layer which is formed between the two electrodes and the ions in the electrolyte. The distance in which charge separation occurs is only a few Angstrom. As electrolytes, use is made of highly porous carbon having internal surface areas of up to 2 500 m[0003] 2/g. As indicated by the capacitor formula
  • C=E 0 ·E·A/d
  • where C is the capacitance, E[0004] 0 is the absolute dielectric constant, E is the dielectric constant of the dielectric, A is the area of the capacitor and d is the distance between the electrodes, capacitances of up to 100 farad/cm3 are possible at large areas A and small spacings d.
  • Such double-layer capacitors (supercapacitors) at present achieve energy densities of from 3 to 7 Wh/kg or Wh/liter, which are far below the energy densities of conventional batteries (lithium ion batteries achieve from 150 to 200 Wh/kg). This is due to the maximum possible voltage loading being restricted to about 3.5 V by the electrochemical stability of the electrolyte. [0005]
  • On the other hand, there is a type of capacitor which operates at high voltages, namely ceramic capacitors comprising dielectrics based on barium titanate. [0006]
  • Ceramic capacitors which comprise dielectrics based on barium titanate and operate at high working voltages because of the high dielectric breakdown resistance of the titanates of up to 200 V/0.1 μm are known from the prior art. However, ceramic capacitors have relatively low capacitances.[0007]
  • It is an object of the present invention to remedy the abovementioned disadvantages. [0008]
  • We have found that this object is achieved by new and improved capacitors which comprise an inert porous shaped body onto which a first electrically conductive layer, a second layer of barium titanate and a further electrically conductive layer have been applied. [0009]
  • The capacitors of the present invention can be produced as follows: [0010]
  • An inert porous shaped body can, in a first step, be provided with a first electrically conductive layer and this can be provided with a contact. A second layer of barium titanate can be applied on top of the first layer and, finally, another electrically conductive layer can be applied on top of this titanate layer and be provided with a contact. The capacitors obtained in this way can be hermetically sealed, e.g. encapsulated, except for the electric contacts. [0011]
  • Suitable porous shaped bodies are in general catalyst support materials, for example those based on metal oxides such as aluminum oxide, silicon dioxide, titanium dioxide, zirconium dioxide, chromium oxide or mixtures thereof, preferably aluminum oxide, silicon dioxide, titanium dioxide, zirconium dioxide or mixtures thereof, particularly preferably aluminum oxide, zirconium dioxide or mixtures thereof, or carbides, preferably silicon carbide, having a BET surface area of from 0.1 to 20 m[0012] 2/g, preferably from 0.5 to 10 m2/g, particularly preferably from 1 to 5 m2/g, a pore content of from 10 to 90% by volume, preferably from 30 to 85% by volume, particularly preferably from 50 to 80% by volume, and pore sizes of from 0.01 to 100 μm, preferably from 0.1 to 30 μm, particularly preferably from 1 to 10 μm.
  • The shaped bodies can have any shapes, for example rings, pellets, stars, wagon wheels, honeycombs, preferably cuboids, cylinders, rectangles or boxes of generally any size (diameter, longest edge length). In the case of capacitors for information technology, for example, the size is generally in the range from 1 to 10 mm. Larger dimensions are necessary in energy engineering. [0013]
  • To produce the first conductive layer on the shaped body, metals such as copper, nickel, chromium or mixtures thereof can be applied in any layer thickness, generally from 10 nm to 1 000 nm, preferably from 50 nm to 500 nm, particularly preferably from 100 nm to 200 nm. [0014]
  • The application of the electrically conductive layer to the shaped body can be carried out using all known methods such as vapor deposition, sputtering or electroless plating, preferably electroless plating. In electroless plating, the shaped bodies are infiltrated or impregnated with suitable, commercially available plating liquids and heated to temperatures below 100° C. to deposit the metal. After metal deposition, the liquid, usually water, can be removed at elevated temperatures and, if desired, under reduced pressure. [0015]
  • It is also possible, for example in the case of iron or nickel, to produce the first conductive layer by heating the shaped bodies in iron carbonyl or nickel carbonyl vapors. In the case of iron, the shaped bodies can be heated to from about 150 to 200° C., and in the case of nickel to from 50 to 100° C. [0016]
  • In a preferred embodiment, the shaped bodies can be heated to elevated temperatures of from 50 to 100° C. in an inert atmosphere (e.g. nitrogen or argon) to produce a homogeneous metal layer. It may be advantageous to apply crystallization nuclei, e.g. nuclei based on platinum metals, likewise by impregnation with suitable liquids (see above). [0017]
  • Finally, the first metal layer can be provided with a contact. This can be carried out, for example, by soldering a metal foil onto an area of the metal-coated shaped body (production of the first electrode). [0018]
  • A dielectric can then be applied on top of the initially produced electrode. This is advantageously carried out using dispersions of crystalline titanate particles having sizes of less than 10 nm in alcohols. Such dispersions can be prepared by reaction of titanium alkoxides with barium hydroxides or strontium hydroxides in alcoholic solution as described in the German application No.: 102 21 499.9 (O.Z. 0050/53537). [0019]
  • The shaped body can be infiltrated or impregnated with such a dispersion which may contain from 5 to 60% by weight, preferably from 10 to 40% by weight, of titanate particles, followed by removal of the alcohol by increasing the temperature to 30-100° C., preferably 50-80° C., and, if desired, reducing the ambient pressure to deposit the titanium particles on the first electrode. [0020]
  • To produce a homogeneous, dense layer of the dielectric, the shaped bodies can be heated to from 700 to 1 200° C., preferably from 900 to 1 100° C., in an inert gas atmosphere so that the titanate particles sinter together to form a dense film. [0021]
  • To increase the layer thickness, the impregnation with the titanate dispersion and the sintering can be repeated a number of times. The layer thickness is generally from 10 to 1 000 nm, preferably from 20 to 500 nm, particularly preferably from 100 to 300 nm. [0022]
  • Finally, a second electrode layer can be applied in a manner analogous to that employed for the first. [0023]
  • After the second electrode layer has been applied, this can be provided with a contact on the side opposite the first contact, thus producing the capacitor. The latter can be hermetically encapsulated to protect it and for the purposes of insulation. [0024]
  • The capacitors of the present invention are suitable as smoothing capacitors or energy storing capacitors or phase shift capacitors in electric energy engineering and as coupling capacitors, filter capacitors or miniature energy storage capacitors in information technology. [0025]
  • The capacitors of the present invention may be illustrated as follows: [0026]
  • A specific surface area (BET surface area) of the porous shaped body of 2 m[0027] 2/g and a barium titanate layer thickness of 0.1 μm at a relative dielectric constant of 5 000 (“The Effect of Grain Size on the Dielectric Properties of Barium Titanate Ceramic”, A. J. Bell and A. J. Moulson, in Electrical Ceramics, British Ceramic Proceedings No. 36, October 1985, pages 57-65) gives a capacitance calculated according to the formula on page 1, line 29, of about 1 farad/cm3. Such a capacitor can be charged to a voltage of 200 V, and its energy density is then 20 000 Ws/cm3 or approximately 5.5 kWh/liter.

Claims (6)

We claim:
1. A capacitor comprising an inert porous shaped body onto which a first electrically conductive layer, a second layer of barium titanate and a further electrically conductive layer have been applied.
2. A capacitor as claimed in claim 1 consisting of an inert porous shaped body onto which a first electrically conductive layer, a second layer of barium titanate and a further electrically conductive layer have been applied.
3. A capacitor as claimed in claim 1 or 2, wherein the BET surface area of the inert porous shaped body is from 0.1 to 20 m2/g.
4. A capacitor as claimed in any of claims 1, 2 and 3, wherein the pore content of the inert, porous shaped body is from 10 to 90% by volume.
5. A process for producing capacitors as claimed in any of claims 1, 2, 3 and 4, which comprises applying an electrically conductive layer with contact onto an inert porous shaped body, applying a layer of barium titanate on top of this and applying an electrically conductive layer with contact on top of the latter.
6. The use of the capacitors in electric energy engineering as smoothing capacitor or energy storage capacitor or phase shift capacitor and in information technology as coupling capacitor, filter capacitor or miniature energy storage capacitor.
US10/435,081 2002-05-14 2003-05-12 Capacitors having a high energy density Abandoned US20030214776A1 (en)

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EP (1) EP1506555A2 (en)
JP (1) JP2005525700A (en)
KR (1) KR20040106399A (en)
CN (1) CN1653566A (en)
AU (1) AU2003242534A1 (en)
DE (1) DE10221498A1 (en)
TW (1) TW200401314A (en)
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20030215384A1 (en) * 2002-05-14 2003-11-20 Hans-Josef Sterzel Preparation of barium titanate or strontium titanate having a mean diameter of less than 10 nanometers
US20090135545A1 (en) * 2004-10-26 2009-05-28 Basf Aktiengesellschaft Capacitors having a high energy density
US20090168299A1 (en) * 2006-04-26 2009-07-02 Basf Se Method for the production of a coating of a porous, electrically conductive support material with a dielectric, and production of capacitors having high capacity density with the aid of said method
US20130301188A1 (en) * 2010-11-11 2013-11-14 Bert Walch Method for manufacturing a capacitive storage element, storage element and its use

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EP2392021A2 (en) * 2009-02-02 2011-12-07 Space Charge, LLC Capacitors using preformed dielectric
US20100200393A1 (en) * 2009-02-09 2010-08-12 Robert Chow Sputter deposition method and system for fabricating thin film capacitors with optically transparent smooth surface metal oxide standoff layer
WO2011050374A1 (en) 2009-10-30 2011-05-05 Franz Oberthaler Electrical capacitor having a high energy density
DK2630811T3 (en) 2010-10-19 2016-02-08 Sonova Ag A hearing instrument, comprising a rechargeable power source
US9396880B2 (en) 2011-11-16 2016-07-19 Martin A. Stuart High energy density storage device
JP6242337B2 (en) 2011-11-16 2017-12-06 スチュアート，マーティン，エー． High energy density power storage device
US9287701B2 (en) 2014-07-22 2016-03-15 Richard H. Sherratt and Susan B. Sherratt Revocable Trust Fund DC energy transfer apparatus, applications, components, and methods
CN105161304A (en) * 2015-06-22 2015-12-16 广东明路电力电子有限公司 Honeycomb electrode capacitor
KR101912286B1 (en) * 2017-03-27 2018-10-29 삼성전기 주식회사 Capacitor Component

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US6519136B1 (en) * 2002-03-29 2003-02-11 Intel Corporation Hybrid dielectric material and hybrid dielectric capacitor

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US4766522A (en) * 1987-07-15 1988-08-23 Hughes Aircraft Company Electrochemical capacitor
US5586001A (en) * 1994-08-16 1996-12-17 Nec Corporation Solid electrolyte capacitor using polyaniline doped with disulfonic acid
US5621608A (en) * 1994-11-25 1997-04-15 Nec Corporation Solid electrolytic capacitor having two solid electrolyte layers and method of manufacturing the same
US5825611A (en) * 1997-01-29 1998-10-20 Vishay Sprague, Inc. Doped sintered tantalum pellets with nitrogen in a capacitor
US6205015B1 (en) * 1998-01-20 2001-03-20 Murata Manufacturing Co., Ltd. Dielectric ceramic, method for producing the same, laminated ceramic electronic element, and method for producing the same
US6519136B1 (en) * 2002-03-29 2003-02-11 Intel Corporation Hybrid dielectric material and hybrid dielectric capacitor

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20030215384A1 (en) * 2002-05-14 2003-11-20 Hans-Josef Sterzel Preparation of barium titanate or strontium titanate having a mean diameter of less than 10 nanometers
US7223378B2 (en) 2002-05-14 2007-05-29 Basf Aktiengesellschaft Preparation of barium titanate or strontium titanate having a mean diameter of less than 10 nanometers
US20090135545A1 (en) * 2004-10-26 2009-05-28 Basf Aktiengesellschaft Capacitors having a high energy density
US20090168299A1 (en) * 2006-04-26 2009-07-02 Basf Se Method for the production of a coating of a porous, electrically conductive support material with a dielectric, and production of capacitors having high capacity density with the aid of said method
US20130301188A1 (en) * 2010-11-11 2013-11-14 Bert Walch Method for manufacturing a capacitive storage element, storage element and its use
US9583263B2 (en) * 2010-11-11 2017-02-28 Robert Bosch Gmbh Method for manufacturing a capacitive storage element, storage element and its use

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WO2003096362A2 (en) 2003-11-20
AU2003242534A1 (en) 2003-11-11
EP1506555A2 (en) 2005-02-16
KR20040106399A (en) 2004-12-17
JP2005525700A (en) 2005-08-25
TW200401314A (en) 2004-01-16
US7023687B2 (en) 2006-04-04
AU2003242534A8 (en) 2003-11-11
CN1653566A (en) 2005-08-10
WO2003096362A3 (en) 2004-08-26
DE10221498A1 (en) 2003-12-04
US20050152090A1 (en) 2005-07-14

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