AU708078B2 - High-temperature fuel cell having at least one electrically insulating covering, and method for producing a high- temperature fuel cell - Google Patents

High-temperature fuel cell having at least one electrically insulating covering, and method for producing a high- temperature fuel cell Download PDF

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Publication number
AU708078B2
AU708078B2 AU14160/97A AU1416097A AU708078B2 AU 708078 B2 AU708078 B2 AU 708078B2 AU 14160/97 A AU14160/97 A AU 14160/97A AU 1416097 A AU1416097 A AU 1416097A AU 708078 B2 AU708078 B2 AU 708078B2
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Australia
Prior art keywords
electrically insulating
fuel cell
layer
temperature fuel
insulating covering
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AU14160/97A
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AU1416097A (en
Inventor
Jens Decker
Thomas Jansing
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Siemens AG
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Siemens AG
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M8/00—Fuel cells; Manufacture thereof
    • H01M8/02—Details
    • H01M8/0271—Sealing or supporting means around electrodes, matrices or membranes
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
    • C23C4/02—Pretreatment of the material to be coated, e.g. for coating on selected surface areas
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M8/00—Fuel cells; Manufacture thereof
    • H01M8/10—Fuel cells with solid electrolytes
    • H01M8/12—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte
    • H01M2008/1293—Fuel cells with solid oxide electrolytes
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M2300/00—Electrolytes
    • H01M2300/0017—Non-aqueous electrolytes
    • H01M2300/0065—Solid electrolytes
    • H01M2300/0068—Solid electrolytes inorganic
    • H01M2300/0071—Oxides
    • H01M2300/0074—Ion conductive at high temperature
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M8/00—Fuel cells; Manufacture thereof
    • H01M8/02—Details
    • H01M8/0202—Collectors; Separators, e.g. bipolar separators; Interconnectors
    • H01M8/0204—Non-porous and characterised by the material
    • H01M8/0206—Metals or alloys
    • H01M8/0208—Alloys
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M8/00—Fuel cells; Manufacture thereof
    • H01M8/02—Details
    • H01M8/0202—Collectors; Separators, e.g. bipolar separators; Interconnectors
    • H01M8/0204—Non-porous and characterised by the material
    • H01M8/0206—Metals or alloys
    • H01M8/0208—Alloys
    • H01M8/021—Alloys based on iron
    • 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
    • Y02E60/30—Hydrogen technology
    • Y02E60/50—Fuel cells

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Plasma & Fusion (AREA)
  • Sustainable Development (AREA)
  • Manufacturing & Machinery (AREA)
  • Electrochemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Sustainable Energy (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Fuel Cell (AREA)
  • Laminated Bodies (AREA)

Abstract

In the proposed high-temperature fuel cell with at least one electrically insulating layer (2), the latter comprises at least two layers (4, 6) one of which lies over the other and each of which consists of an electrically insulating ceramic material, the composition of the ceramic material of one layer (4) being different from that of the other layer (6). This measure optimises the insulation and adhesion of the electrically insulating layer (2).

Description

~1111 GR 95 P 8581 P 2 occur between these bipolar plates, as a result of electrolysis, if a glass-like substance is used, that is to say ion migration takes place from one electrode side to the other. In the process, the intrinsic strength of the glass-like substance is adversely affected even after a short time, as a result of which the probability of a malfunction occurring is in turn considerably increased.
In order to avoid this disadvantage, the bipolar plate is provided with an additional single-layer covering of stabilized ZrO 2 which, depending on the requirement or the design has a thickness of between, for example, 30 pm and 150 pm.
Optionally, for better adhesion of the covering on the bipolar plate, a so-called adhesion promoter composed of metal or ceramic is applied to the bipolar plate to improve the adhesion of the covering on the bipolar plate. The ZrO 2 material used is in general partially or fully stabilized using known technical stabilization components such as Y 2 0 3 CaO, MgO, A1 2 0 3 or CeO 2 This single-layer covering has inadequate electrical insulation which is required especially if a glass-like substance is used to join the metallic components together, since the glass-like substance is a poor electrical insulator.
US Patent Specification 5,338,577 discloses a method for coating a metallic substrate with ceramic by means of flame spraying, an intermediate covering of steel being sprayed on first of all, followed by a covering of yttrium-stabilized ZrO 2 and, finally, an A1 2 0 3 covering.
Furthermore, Japanese Laid-Open Specification 06-144 971 discloses a covering body which comprises a ceramic substrate, adhesion promoter coverings of steel, a ceramic covering and, possibly, an outer covering to close the pores, the adhesion promoter coverings and the ceramic covering being produced by GR 95 P 8581 P 2ameans of flame spraying, and the outer covering being produced by means of a sal-gel technique.
GR 95 P 8581 P 3 In addition, US Laid-Open Specification H 12 discloses a method for producing covering bodies for high-temperature fuel cells by means of a plasma spray process. However, in the case of this process, only a single electrically insulating covering, composed of yttrium-stabilized ZrO 2 is sprayed on.
The invention is now based on the object of specifying a high-temperature fuel cell, one of the coverings having the characteristics of providing electrical insulation which is as complete as possible, adhering well and being mechanically robust. In addition, the invention is based on the object of specifying a method for producing of a high-temperature fuel cell.
The first-mentioned object is achieved according to the invention by a high-temperature fuel cell having at least one electrically insulating covering, containing at least two layers which are arranged one on top of the other and are each composed of an electrically insulating ceramic material, the composition of the ceramic material of one layer being different to the composition of the ceramic material of the other layer.
The second-mentioned object is achieved according to the invention by a method for producing a high-temperature fuel cell having at least one electrically insulating covering, containing at least two layers which are arranged one on top of the other and are each composed of an electrically insulating ceramic material, the composition of the ceramic material of one layer being different to the composition of the ceramic material of the other layer, the individual ceramic layers each being produced successively by spraying of a ceramic and by being applied to a component.
-3a- According to a first aspect of the present invention, there is provided a hightemperature fuel cell having at least one electrically insulating covering, which is arranged between two bipolar plates, the electrically insulating covering-containing at least two layers which are arranged one on top of the other and are each composed of an electrically insulating ceramic material, the composition of the ceramic material of one layer being different to the composition of the ceramic material of the other layer.
According to a second aspect of the present invention, there is provided a method for producing a high-temperature fuel cell having at least one electrically insulating covering, which is arranged between two bipolar plates, the electrically insulating covering containing at least two layers which are arranged one on top of the other and are each composed of an electrically insulating ceramic material, the composition of the ceramic material of one layer being different to the composition of the ceramic material of the other layer, the individual ceramic layers each being produced successively by spraying of a ceramic and being applied to a component.
Si
S
S S [R:\LIBL]00140.doc:BFD GR 95 P 8581 P 4 The use of a plurality of electrically insulating ceramic layers in an electrically insulating covering has the advantage that the various requirements for electrical insulation and adhesion of different ceramic layers are satisfied separately, since these differing requirements cannot be satisfied in a single ceramic layer. Electrical insulation and good adhesion characteristics are thus satisfied by a plurality of ceramic layers of different composition within a covering. The electrically insulating covering thus comprises at least a first layer having good adhesion characteristics, that is to say, the linear coefficient of expansion of the first layer differs only slightly from the linear coefficient of expansion of that component to which the first layer is applied, and a second layer which is arranged on the first layer and is characterized by good electrical insulation.
In particular, at least two layers are composed of the same electrically insulating ceramic material, and are separated from one another by at least one layer composed of a different electrically insulating ceramic material. As is known from the prior art, a single ceramic layer is not sufficient for adequately good electrical insulation. Since the covering thickness of a ceramic layer cannot be increased indefinitely owing to the intrinsic mechanical stresses that occur, an electrically insulating covering, having a plurality of ceramic layers is used. In this case, covering thicknesses of, for example, 500 pm are achieved without the intrinsic stress in the covering being increased, since the covering is composed of a plurality of ceramic layers. This leads to considerable mechanical stabilization of the overall high-temperature fuel cell.
An adhesion promoter is preferably used for GR 95 P 8581 P 4a application of the electrically insulating covering to a component of the high-temperature fuel cell. The adhesion promoter additionally ensures good adhesion of the electrically insulating covering GR 95 P 8581 P 5 on the component of the high-temperature fuel cell on which the electrically insulating covering is applied.
In a further refinement, a layer for closing and healing the pores and cracks in the last ceramic layer is applied to the electrically insulating covering.
The electrically insulating covering is produced, in particular, by atmospheric plasma spraying, flame spraying, high-speed flame spraying, vacuum flame spraying or low-pressure flame spraying.
The use of different spraying processes allows the respectively desired ceramic covering to be produced in different external conditions.
A layer is preferably applied to the electrically insulating covering by means of a sol gel for closing and healing the pores and cracks in the last ceramic layer. If a glass-like substance, for example glass solder, is applied to the last ceramic layer in a further process, then, for electrical insulation, it is of major importance that the last ceramic layer of the electrically insulating coating be sealed well. If the porosity within the last ceramic layer is too high, the glass-like substance penetrates into this layer, and reduces the electrical insulation.
In a further refinement, the sol gel is vacuum-infiltrated after application. The vacuum infiltration, which may also be carried out actually during the application process, ensures that the cracks and pores are closed and healed.
In order to explain the invention further, reference is made to the exemplary embodiments in the drawing, in which: l GR 95 P 8581 P 6 Figure 1 and Figure 2 show a schematic illustration of details of a high-temperature fuel cell.
According to Figure 1, the detail of a high-temperature fuel cell comprises a component for example a bipolar plate, and an electrically insulating covering 2. In this case the electrically insulating covering 2 is arranged on the component said electrically insulating covering 2 containing a plurality of layers 4, 6 which are arranged one on top of the other and are each composed of an electrically insulating ceramic material, the composition of the ceramic material in the layers 4 being different to the composition of the ceramic material in the other layers 6.
In this arrangement, in each case two layers 4 composed of the same electrically insulating ceramic material are separated from one another by a layer of 6 composed of a different electrically insulating ceramic material.
In a first step, an adhesion promoter 8 is applied to the component 10. In this case, the component 10 is composed of a metal, a metal alloy or a ceramic. CrFe 5
Y
2 0 3 1 is used, for example, as the metal in the high-temperature fuel cell. Other special alloys, such as Haynes Alloy 230, Inconel 600 or conventional industrial stainless steels are likewise often used.
The ceramic layer 4 composed, for example, of ZrO 2 is sprayed onto the adhesion promoter 8, and the linear coefficient of thermal expansion of said ceramic layer 4 is matched to that of the component 10. The ceramic layer 4 is applied directly to the adhesion promoter 8 by the spraying process. The ceramic layer 4 thus adheres well to the component 10, but is not suitable for ensuring good electrical insulation at the same time.
GR 95 P 8581 P 6a In a further step, the ceramic layer 4 has applied to it the ceramic layer 6, which has better electrical insulation GR 95 P 8581 P 7 characteristic than that of the ceramic layer 4. If ZrO 2 is used in the ceramic layer 4, then high-purity A1 2 0 3 is suitable, for example, for the ceramic layer 6.
The MgAl20 4 may be produced, for example, from fused corundum spinels, for example MgAl20 4 mullites or from some other electrically insulating ceramic. As a rule, these ceramics do not have linear coefficients of thermal expansion similar to that of the component so that they adhere to the component 10 only poorly without using the ceramic layer 4. A succession of different ceramic layers 4, 6 thus has the advantage that different requirements, such as electrical insulation and linear coefficient of thermal expansion, are satisfied separately by different layers 4, 6. The ceramic layer 4 ensures good adhesion, while the ceramic layer 6 provides good electrical insulation.
For adequate electrical insulation, the ceramic layer 6 now has to have a thickness which cannot be achieved in a single layer since, if the thicknesses are too great, considerable mechanical intrinsic stresses occur which lead to destabilization of the overall high-temperature fuel cell. In consequence, a plurality of layers 4, 6 are applied one on top of the other for adequate electrical insulation, until the total thickness of the electrically insulating covering 2 is sufficient for electrical insulation.
The spraying of the individual ceramic layers 4, 6 may be carried out, for example, by atmospheric plasma spraying, flame spraying, high-speed flame spraying, vacuum flame spraying or low-pressure flame spraying. The use of different spraying methods makes it possible to produce any desired ceramic layer 4,6 with the desired characteristics.
As shown in the detail of a high-temperature fuel cell in Figure 2, the electrically insulating covering 2 GR 95 P 8581 P 8is arranged between two bipolar plates 20 and 22. The high-temperature fuel cell normally operates at an operating temperature of more than 800'C. In this case, the two bipolar plates 20, 22 can be connected with an integral material joint only by using a glass-like substance. A covering 24 of a glass-like substance is therefore arranged between the bipolar plate 22 and the electrically insulating covering 2. Such a glass-like substance may be, for example, a glass solder.
Since the covering 24 of a glass-like substance is in contact with the ceramic layer 4 applied last in the electrically insulating covering 2, the sealing of this ceramic layer 4 is of major importance for the electrical insulation. Use of spraying for production results in cracks 28 and pores 30 being formed in the surface 26 of the ceramic layer 4, and these may have a negative effect on the electrical insulation characteristic since, for example, glass solder from the covering 24 may penetrate into the cracks 28 and pores 30. This problem is solved by applying a layer 34 onto the last ceramic layer 4 in order to close and heal the cracks 28 and pores 30, and this layer 34 is arranged between the last ceramic layer 4 and the covering 24 composed of a glass-like substance.
Application of an aqueous sol gel as the layer 34, composed of Al(OH) 3 for example, which later dehydrates to form A1 2 0 3 or a sol gel composed of 4 components, allows the cracks 28 and pores 30 in the surface 26 of the ceramic layer 4 to be closed and healed. In the case of this method, the aqueous sol gel is first of all applied onto the surface 26 of the last ceramic layer 4 by spraying by means of compressed air or electrical atomization, by screen printing, by brushing, by sponging or by dipping. In a further step of the method, the sol gel in the layer 34 is GR 95 P 8581 P 8aintroduced into the cracks 28 and the pores 30 by vacuum filtration. Once the method has been completed, a closed GR 95 P 8581 P 9 smooth surface 26 is thus obtained, into which the glass solder in the covering 24 not longer penetrates.
Typical sealers, which are added to the sol gel, are used, based on epoxy resins and silicone resins. In the case of the high-temperature fuel cell, an aluminum oxide hydroxide sol with 86 to 96% aluminum oxide hydroxide hydrate and 4 to 14% aluminum acetate hydrate are infiltrated into a sprayed covering of ceroxide-stabilized zircon oxide and/or a covering of aluminum oxide. The infiltration can in this case also be carried out at room temperature and, optionally, at reduced pressure.
Owing to its electrical insulation and chemical robustness, the electrically insulating covering 2 is thus excellently suited to use in a high-temperature fuel cell. Gas-carrying ducts and cavities which are integrated in the electrically insulating covering 2 can in this case be sealed off from one another well.
The claims defining the invention are as follows: 1. A high-temperature fuel cell having at least one electrically insulating covering, which is arranged between two bipolar plates, the electricilly insulating covering containing at least two layers which are arranged one on top of the other and are each composed of an electrically insulating ceramic material, the composition of the ceramic material of one layer being different to the composition of the ceramic material of the other layer.
2. The high-temperature fuel cell as claimed in claim 1, which contains at least two layers composed of the same electrically insulating ceramic material, which are separated from one another by at least one layer composed of a different electrically insulating ceramic material.
3. The high-temperature fuel cell as claimed in claim 1 or 2, in which the electrically insulating covering is applied to a component using an adhesion promoter.
4. The high-temperature fuel cell as claimed in one of the preceding claims, in which a layer for closing and healing the pores and cracks in the last ceramic layer is applied onto the electrically insulating covering.
oo o 5. A method for producing a high-temperature fuel cell having at least one electrically insulating covering, which is arranged between two bipolar plates, the electrically insulating covering containing at least two layers which are arranged one on o• 25 top of the other and are each composed of an electrically insulating ceramic material, the "•composition of the ceramic material of one layer being different to the composition of the .o.ceramic material of the other layer, the individual ceramic layers each being produced successively by spraying of a ceramic and being applied to a component.
30 6. The method as claimed in claim 5, in which the electrically insulating covering is produced by atmospheric plasma spraying.
7. The method as claimed in claim 5, in which the electrically insulating Rcovering is produced by flame spraying.
[R:\LIBLJOO140.doc:I3FD

Claims (6)

  1. 8. The method as claimed in claim 7, in which the electrically insulating covering is produced by high-speed of flame spraying.
  2. 9. The method as claimed in claim 7, in which the electrically insulating covering is produced by vacuum flame spraying. The method as claimed in claim 7, in which the electrically insulating covering is produced by low-pressure flame spraying.
  3. 11. The method as claimed in one of claims 5 to 10, in which a layer is applied by means of a sol gel onto the electrically insulating covering in order to close and heal the pores and cracks in the last ceramic layer.
  4. 12. The method as claimed in claim 11, in which the sol gel is vacuum- infiltrated after application.
  5. 13. A high-temperature fuel cell substantially as herein described with reference to Figs. 1 and 2.
  6. 14. A method for producing a high-temperature fuel cell substantially as herein described with reference to Figs. 1 and 2. DATED this twenty-sixth Day of May, 1999 S 25 Siemens Aktiengesellschaft Patent Attorneys for the Applicant *SPRUSON FERGUSON 0 i* [R:\LIBL]00140.doc:BFD 7 GR 95 P 8581 P Abstract High-temperature fuel cell having at least one electrically insulating covering, and method for producing a high-temperature fuel cell. In the case of the present high-temperature fuel cell having at least one electrically insulating covering the electrically insulating covering (2) contains at least two layers 6) which are arranged one on top of the other and are each composed of an electrically insulating ceramic material, the composition of the ceramic material of one layer (4) being different to the composition of the ceramic material of the other layer This measure results in optimization of the insulation characteristic and the adhesion of the electrically insulating covering (2) FIG 1
AU14160/97A 1995-10-12 1996-10-09 High-temperature fuel cell having at least one electrically insulating covering, and method for producing a high- temperature fuel cell Ceased AU708078B2 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE19538034A DE19538034C1 (en) 1995-10-12 1995-10-12 High-temperature fuel cell with at least one electrically insulating layer and method for producing a high-temperature fuel cell
DE19538034 1995-10-12
PCT/DE1996/001931 WO1997013731A2 (en) 1995-10-12 1996-10-09 High-temperature fuel cell with at least one electrically insulating layer and a method of producing a high-temperature fuel cell

Publications (2)

Publication Number Publication Date
AU1416097A AU1416097A (en) 1997-04-30
AU708078B2 true AU708078B2 (en) 1999-07-29

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AU14160/97A Ceased AU708078B2 (en) 1995-10-12 1996-10-09 High-temperature fuel cell having at least one electrically insulating covering, and method for producing a high- temperature fuel cell

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EP (1) EP0867046B1 (en)
JP (1) JPH11515136A (en)
AT (1) ATE190755T1 (en)
AU (1) AU708078B2 (en)
CA (1) CA2234692A1 (en)
DE (2) DE19538034C1 (en)
DK (1) DK0867046T3 (en)
ES (1) ES2144805T3 (en)
WO (1) WO1997013731A2 (en)

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DE19608727C1 (en) * 1996-03-06 1997-06-19 Siemens Ag Insulating layer for joining high temperature fuel cell components
GB9807977D0 (en) 1998-04-16 1998-06-17 Gec Alsthom Ltd Improvements in or relating to coating
DE19942857C2 (en) * 1999-09-08 2001-07-05 Sulzer Metco Ag Wohlen Thick aluminum oxide-based layers produced by plasma spraying
DE10201935A1 (en) * 2002-01-19 2003-07-31 Daimler Chrysler Ag Process for coating a support component by thermal spraying of metal and/or ceramic comprises applying several layers to form a molded part or molded part regions having a simple and/or complex spatial structure
DE102005045053A1 (en) * 2005-09-21 2007-03-29 Elringklinger Ag A method of manufacturing a gasket assembly for a fuel cell stack and gasket assembly for a fuel cell stack
US8440367B2 (en) * 2006-12-05 2013-05-14 Corning Incorporated Solutions for solid oxide fuel cell seal failures
DE102007018610A1 (en) 2007-04-18 2008-10-23 Ceramtec Ag Innovative Ceramic Engineering Ceramic material having a composition that is tuned to a given by a metallic material thermal expansion coefficient
DE102013213015A1 (en) * 2013-07-03 2015-01-08 Deutsches Zentrum für Luft- und Raumfahrt e.V. Method for producing a bipolar plate and bipolar plate for an electrochemical cell
JP6210050B2 (en) 2014-11-12 2017-10-11 トヨタ自動車株式会社 Fuel cell

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WO1996017394A1 (en) * 1994-12-01 1996-06-06 Siemens Aktiengesellschaft Fuel cell with bipolar flanges coated with ceramic material and its production

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DK0867046T3 (en) 2000-08-21
DE59604703D1 (en) 2000-04-20
CA2234692A1 (en) 1997-04-17
JPH11515136A (en) 1999-12-21
WO1997013731A3 (en) 1997-07-03
DE19538034C1 (en) 1997-01-09
WO1997013731A2 (en) 1997-04-17
AU1416097A (en) 1997-04-30
EP0867046B1 (en) 2000-03-15
ATE190755T1 (en) 2000-04-15
ES2144805T3 (en) 2000-06-16
EP0867046A2 (en) 1998-09-30

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