AU2001266040B2 - Method for applying a solid electrolytic layer to a porous electrode - Google Patents

Method for applying a solid electrolytic layer to a porous electrode Download PDF

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Publication number
AU2001266040B2
AU2001266040B2 AU2001266040A AU2001266040A AU2001266040B2 AU 2001266040 B2 AU2001266040 B2 AU 2001266040B2 AU 2001266040 A AU2001266040 A AU 2001266040A AU 2001266040 A AU2001266040 A AU 2001266040A AU 2001266040 B2 AU2001266040 B2 AU 2001266040B2
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Australia
Prior art keywords
suspension
solid
hollow body
layer
constituents
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AU2001266040A
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AU2001266040A1 (en
Inventor
Gunter Blass
Hans Peter Buchkremer
Robert Fleck
Udo Flesch
Thomas Jansing
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Forschungszentrum Juelich GmbH
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Forschungszentrum Juelich GmbH
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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
    • H01M8/10—Fuel cells with solid electrolytes
    • H01M8/12—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte
    • H01M8/124—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte characterised by the process of manufacturing or by the material of the electrolyte
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/8605—Porous electrodes
    • H01M4/8626—Porous electrodes characterised by the form
    • 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
    • H01M8/1213—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte characterised by the electrode/electrolyte combination or the supporting material
    • 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
    • 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
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product

Description

WO 0195420 PCT/EP01/06251 Method for Applying a Solid Electrolytic Layer to a Porous Electrode The present invention relates to a method for applying a solid electrolytic layer to a porous electrode, in particular, to an electrode for a solid oxide fuel cell (SOFC), in which a layer of solid electrolytic material is applied to the electrode by the deposition of solid constituents from a suspension.
As a rule, a fuel cell comprises an anode and a cathode, between which an electrolytic layer is applied. A fuel is conducted across the surface of the anode, and oxygen is conducted across the surface of the cathode. Ion exchange takes place between the fuel and the oxygen across the electrolytic layer, so that a voltage is generated between the anode and the cathode.
A decisive factor for the efficiency of a fuel cell is, amongst other things, the electrolytic layer that, on the one hand, must be conductive for the ions and, on the other hand, must be largely impermeable to gas in order to prevent gaseous exchange between the fuel and oxygen. Thus, great demands are placed upon the electrolytic layer.
WO 01/95420 PCT/EPO 1/06251 In the case of so-called solid oxide fuel cells, the anode and cathode are both formed from a porous ceramic material between which there is a solid electrolytic layer. Solid oxide fuel cells with a planar geometry are known; in these, the anode and cathode are arranged so as to be essentially planeparallel. Also known is a cylindrical or tubular configuration in which the anode encloses the cylindrically configured cathode and encloses the solid electrolytic layer. Numerous methods are known for applying the solid electrolytic layer. For example 196 09 418 C2 describes the application of a suspension to a plane electrode, this suspension containing solid constituents of the solid electrolytic material. Excess solvent is removed by generating a partial vacuum on the side of the porous electrode that is opposite the suspension. The suspension contains coarse and fine solid constituents, the coarse constituents first filling the pores in the electrode and ensuring a good bond between the electrolytic layer and the electrode. The fine constituents are then deposited on the coarse constituents. The layer of solid material is dried and then sintered to form the solid electrolytic layer.
This coating method is not suitable for non-planar surfaces, since it is difficult to apply the suspension evenly to complex surface geometries.
WO 01/95420 PCT/EP01/06251 DE 196 09 418 C2 also describes how the electrolytic layer can be produced by means of electrophoresis or by means of foil casting.
The article titled "Status of Solid Oxide Fuel Cell Technology" by S.C. Singhal, which appeared in High a Temperature Electrode Chemistry: Ceramics and Metals, 17th Riso International Symposium and Material Science, Roskilde, Denmark (September 1996), describes an electro-chemical vapour deposition (EVD) method for applying the electrolytic layer. This method is also suitable for complex surface geometries, in particular for the curved surfaces that are found in cylindrical or tubular fuel cells. The EVD process is extremely costly and involved.
This document describes the construction principles for a tubular fuel cell.
This comprises a porous, ceramic inner cylinder as the cathode, on which the electrolytic layer and then the anode are applied as a casing. In order to connect two fuel cells electrically in series the anode of one fuel cell is connected directly to a so-called inter-connector of the second fuel cell, the electrolytic layer and the anode of the fuel cells being interrupted in the area of the interconnector. The article referred to also states that both the electrolytic layer as well as the interconnector and the anode are normally Q:\OPER\GCP2OO6\Fcb\2O01 266040.do-20/02/06 4 applied using the EVD method. The article addresses the problem of how to replace the costly EVD method with other coating systems. Although, as is proposed in the article, new coating methods for the interconnector and for the anode have been developed and are being used, the EVD process continues to be used for the electrolytic coating in order to ensure sufficiently high quality.
It is the objective of the present invention to describe a simple method for applying a solid electrolytic layer to a porous electrode, which is also suitable for complex geometries.
According to the present invention there is provided a method for applying a solid electrolytic layer to a porous electrode, in particular to an electrode for a solid oxide fuel cell, in which a layer of solid material that is of solid electrolytic material is applied to the electrode by the deposition of solid constituents from a suspension, characterized in that the electrode is configured as a hollow body that is immersed in the suspension in order to apply the layer of solid material.
In a simple and advantageous manner, the outer surface of the hollow body that is to be coated is wetted evenly by this immersion. Thus, even complex component geometries can be coated very simply by being so immersed.
WO 01/95420 PCT/EP01/06251 In order to achieve the most rapid possible build up of the layer of solid material, a pressure drop is created between the interior space of the hollow body and the suspension, so that a solvent that is contained in the suspension infiltrates into the interior chamber.
An important advantage of immersion in the suspension, in particular with the creation of a partial vacuum, is that, regardless of the special complex geometry of the hollow body, the solid constituents are deposited evenly on the outer surface so that ultimately a thin, homogenous solid electrolytic layer of constant thickness can be formed.
It is preferred that the pressure drop be maintained by way of a suction line that reaches into the interior space, in order to ensure the even deposition of the solid constituents. The pressure drop or the pressure difference between the suspension-side exterior of the hollow body and the inner side that faces the interior space is thus kept as constant as possible during the whole of the deposition process.
In one preferred embodiment, the solvent that infiltrates into the interior space is removed. In a comparatively simple manner, this makes it possible WOo 0 .1/95420 PCT/EP01/06251 to maintain a constant pressure drop and it helps ensure the most even possible deposition process for the solid constituents.
In a particularly effective manner, the solvent is removed by way of the suction line, so that there is no need for a separate system of lines for the solvent.
In order to achieve the most simple possible coating process, it is proposed that once the desired thickness of the layer of solid material has been achieved, the hollow body is removed from the suspension. Thus, there is an excess of solvent and it is not necessary to match the quantity of the suspension into which the hollow body is dipped to the desired thickness of the layer.
In order to prevent damage being done to the previously deposited layer of solid material when it is removed, it is preferred that the pressure drop be maintained during removal of the hollow body.
12-09-02 16:58 ID=613 232 8440 WO 01/95420 PCT/EP01/06251 It is particularly useful if the quantity of solvent that is removed be used to determine the thickness of the layer of solid material that has already been deposited. The amount of solid constituents that has been deposited can be calculated from the quantity of solid constituents that has been deposited.
This permits simple determination of the thickness of the layer. Additionally, or alternatively, the thickness of the layer can be determined from the quantity of the suspension that is drawn in. This is done in the simplest way by a measuring or regulating the level of the suspension in a tank into which the electrode is dipped.
In one particularly useful configuration, the suspension comprises both coarse and fine solid constituents so that a high quality solid electrolytic layer can form. The coarse solid constituents are deposited into the pores of the hollow body and thus ensure good bonding of the electrolytic layer. The fine solid constituents are then deposited, and ensure a dense configuration of the electrolytic layer.
In order to achieve a high-quality electrolytic layer, it is preferred that provision be made such that the maximal diameter of the coarse solid constituents corresponds more or less to the maximal pore diameter of the WO 01/95420 PCT/EP01/06251 hollow body. Typically, the value for maximal diameter of the solid constituents is between 5 and 20 pm. Such selection of the diameter prevents any solid constituents that may possibly be too coarse causing unevenness of the surface and thus to undesirable non-homogeneity. At the same time, it will also ensure a good configuration of the electrolytic layer on the electrode.
It is preferred that the proportion of coarse solid constituents account for between 1 and 15%-vol of the suspension. This proportion is sufficient to fill the coarse pores of the hollow body that are close to the surface.
In order to form the densest and most homogenous possible electrolytic layer, the diameter of the fine solid constituents amounts to approximately one-third of the minimal pore diameter of the hollow body. It is preferred that the diameter be somewhat smaller than 1 pm, since the pore diameter of the smaller pores lies between about 1 and 10 pm.
In order to ensure the strength of the applied layer once it has been tried, it is preferred that the binder and polyethyleneimine, PEI) be added to 12-09-02 16:58 ID=513 232 8440 P.06 WO 01/95420 PCT/EP01/06251 the suspension This brings about adhesion of the "green" particles of the layer.
In order to ensure the gas-tight adhesion of this solid electrolytic layer, it is preferred that the layer of solid material is first dried and then densified by sintering. The resulting layer is largely gas tight. Sintering is effected, for example, by the usual method, at temperatures ranging from 1300 to 1500 degrees Celsius, in a sintering oven that is heated by heating elements, and is continued for several hours.
One exemplary embodiment of the present invention is described in greater detail below on the basis of the drawings appended hereto. These drawings show the following: Figure 1: A setup for carrying out the method; Figure 2: Examples of hollow-body geometries; Figure 3: A diagram showing the distribution of particle-size distribution for the solid constituents in a suspension.
WO 01/ 95420 PCT/EP01/06251 Figure 1 shows a system for carrying out the method; this comprises a tank 2 that is filled with a suspension 4. The suspension 4 is made up of a solvent L, fine solid constituents F, and coarse solid constituents G, together with a binder B. The solid constituents F, G consist of a solid electrolytic material and are distributed homogeneously within the suspension 4. A cylindrical hollow body 6 is dipped into this suspension 4, and this body serves as an electrode, in particular a cathode, for a tubular fuel cell. The hollow body 6 is of a porous ceramic material. Each of its open ends is sealed off by a stopper 8A, 8B so that the suspension 4 cannot infiltrate into the interior space 10 of the hollow body 6. A suction line 12 passes through the upper stopper 8A into the interior space 10, and extends within this almost as far as the opposite stopper 8B. The suction line 12 is connected to a pumping system 14, and a flow meter is arranged in this suction line 12. This flow meter is connected to a control device 18 that controls the pumping system 4 The pumping system 14 is used to create a pressure drop across the wall 20 of the hollow body 6. This means that a pressure difference is created between of the outer side that faces the suspension 4 and the inner side of the hollow body 6 that is oriented towards the interior space WOo 01/95420 PCT/EP01/06251 The pumping system 14 is designed to separate gaseous constituents from liquid constituents. To this end, it incorporates a line 26 that opens out into a collector tank 26, and an exhaust line The solid constituents F, G, and B are deposited onto the outer side of the immersed hollow body 6 and thus form a layer of solid material 32 that is of solid electrolytic material. A continuous and durable layer buildup is ensured because a pressure differential has been generated by the pumping system 14. Because of the porous configuration of the hollow body 6, the solvent L infiltrates through the hollow body 6 into the interior space 10, from which the solvent is pumped continuously by way of the suction line 12. For this reason, the suction line 12 thus serves to simultaneously pump out gas from the interior space 10 and to pump out solvent L so as to create and maintain the pressure drop. The solvent L that is pumped out is collected in the collector tank 28. The quantity of solvent L that is pumped out is measured by the throughflow measuring device 16. The thickness of the layer of solid material 32 that is deposited is measured by the control system 18, using the measured quantity, taking into account the solid constituents in the suspension 4. Providing the solids content of the suspension is known, WO 01~95420 PCT/EP01/06251 then the layer thickness setting can be preset by regulating the level 34 of the suspension 4in the tank 2, for example, by reading a scale 36.
As soon as the layer has reached the desired thickness, the hollow body 6 is removed from the suspension 4 or the suspension is drained off whilst the pressure differential is maintained. The hollow body 6 now has an homogeneously applied the layer of solid material 32 that is of solid electrolytic material. In order to complete the solid electrolytic layer, in an additional step of the process the layer of solid material 32 is first air dried and then densified by being sintered. This sintering is effected, for example, using a conventional sintering process at temperatures that are between 13000C to 1500 0 C, and is continued for several hours.
The method that has been described is used to apply a solid electrolytic layer to the anode of a fuel cell that is, in particular, tubular or pipe-like, in a simple manner, an homogenous and even a coating of the hollow body 6 is made possible by immersion in the suspension 4. In particular, even bodies with complex geometries can be coated homogeneously in a simple way.
12-09-02 16:5B ID=613 232 8440 P.07 WO 01/95420 PCT/EP01/06251 Figures 2A to 2D show examples of different geometries for the hollow body 6. Figure 2A shows a cylindrical geometry of an open-ended hollow body 6A.
Figure 2 B shows a similar cylindrical hollow body 6 B that is closed off at one end. Even spherical hollow bodies 6C (Figure 2 C) or L-shaped hollow bodies 6D (Figure 2D) can be coated homogeneously using this method.
The particle-size distribution of the solid constituents F, G, in the suspension 4 is shown by way of an example in Figure 3. In this diagram, the particle size x in pm is plotted against the cumulative solid constituent as a percentage. From this it can be seen that the particle size x ranges from approximately 0.2 pm to 20 pm, the proportion a of the fine solid constituents F that are of a diameter of 1 pm is in excess of Accordingly, the proportion of coarse solid constituents G with a particle diameter greater than 5 pm lies in the range of only a few percentage points, relative to the total solid constituents C within the suspension 4. A proportion of 1-15 %-vol of the coarse solid constituents G relative to the suspension 4 is desired.
The distribution of the particle sizes is so selected that the largest particles of the coarse solid constituent are of a diameter that corresponds to the Q:\OPER\GCP2OO6\Feb\2001266040c.doc-20/02/06 14 maximum pore size of the hollow body 6. Thus, the pores of the hollow body 6 are filled with the coarse solid constituents G, so that the fine solid constituents F cannot infiltrate through the walls of the hollow body 20. Rather, they build up on the outside of the hollow body 6 and form a homogenous and even layer of solid material 32. In order to obtain the densest possible layer of solid material, and thus the densest possible solid electrolytic layer, the fine solid constituents F are selected so as to be very small and lie, in particular, in a range from approximately of the size of the small pores, the diameter of which typically lies between 1 and 10 pm.
The reference to any prior art in this specification is not, and should not be taken as, an acknowledgment or any form of suggestion that that prior art forms part of the common general knowledge in Australia.
The reference numerals in the following claims are not to be construed as imposing any limitations on the claims.

Claims (14)

1. Method for applying a solid electrolytic layer to a porous electrode in particular to an electrode for a solid oxide fuel cell, in which a layer of solid material (32) that is of solid electrolytic material is applied to the electrode by the deposition of solid constituents (F, G) from a suspension characterized in that the electrode is configured as a hollow body that is immersed in the suspension in order to apply the layer of solid material (32).
2. Method as defined in Claim 1, characterized in that a pressure drop is created between the interior space (10) of the hollow body and the suspension so that a solvent that is contained in the suspension infiltrates into the interior space (10) of the hollow body and the solid constituents G) are deposited on the exterior of the hollow body
3. Method as defined in Claim 2, characterized in that the pressure drop is maintained by way of a suction line (12) that extends into the interior space
4. Method as defined in Claim 2 or Claim 3, characterized in that solvent that has infiltrated through the hollow body is removed.
WO Oi/95420 PCT/EPO 1/06251 Method as defined in Claim 3 and Claim 4, characterized in that the solvent is removed through the suction line (12).
6. Method as defined in one of the Claims 2 to 5, characterized in that the hollow body is removed from the suspension once the desired thickness of the layer of solid material (32) has been reached.
7. Method as defined in Claim 6 and Claim 2, characterized in that the pressure drop is maintained when the hollow body is removed from the suspension
8. Method as defined in Claim 6 or Claim 7, characterized in that the thickness of the layer is determined by measuring the quantity of solvent that is removed and/or by measuring the quantity of suspension that is drawn in.
9. Method as defined in one of the preceding claims, characterized in that the suspension contains coarse solid constituents and fine solid constituents Method as defined in Claim 9, characterized in that the maximum diameter of the course solid constituents corresponds approximately to the maximal pore diameter of the hollow body and, in particular, lies between 5 and 20 im.
Q:\OPER\GCP\2006\Fb2001266040c doc.20/02/06 17
11. Method as defined in Claim 9 or Claim 10, characterized in that the portion of coarse solid constituents amounts to approximately 1 to 15%-vol of the suspension
12. Method as defined in one of the Claims 9 or 11, characterized in that the diameter of the fine solid constituents corresponds approximately to one-third of the minimal pore diameter of the hollow body and is, in particular, somewhat smaller than 1 pm.
13. Method as defined in one of the preceding claims, characterized in that the suspension contains a binding agent
14. Method as defined in one of the preceding claims, characterized in that the layer of solid material (32) that has been deposited is dried and then densified by sintering to form the solid electrolytic layer. A method for applying a solid electrolytic layer to a porous electrode substantially as hereinbefore described with reference to the accompanying drawings. DATED this 20th day of February 2006 FORSCHUNGSZENTRUM JULICH GMBH By its Patent Attorneys DAVIES COLLISON CAVE
AU2001266040A 2000-06-09 2001-06-01 Method for applying a solid electrolytic layer to a porous electrode Ceased AU2001266040B2 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
EP00112393 2000-06-09
EP00112393.4 2000-06-09
PCT/EP2001/006251 WO2001095420A1 (en) 2000-06-09 2001-06-01 Method for applying a solid electrolytic layer to a porous electrode

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AU2001266040B2 true AU2001266040B2 (en) 2006-03-16

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AU (2) AU2001266040B2 (en)
CA (1) CA2411711C (en)
CY (1) CY1117289T1 (en)
DK (1) DK1287576T3 (en)
ES (1) ES2557739T3 (en)
NO (1) NO328244B1 (en)
PT (1) PT1287576E (en)
WO (1) WO2001095420A1 (en)

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NL9002168A (en) * 1990-10-05 1992-05-06 Blandikus Catharikus Jaspers E HOLLOW ELECTRODE FOR AN ELECTROCHEMICAL CELL PROVIDED WITH AT LEAST A GAS SUPPLY AND EXHAUST OPENING, AND ELECTROCHEMICAL CELL INCLUDING SUCH ELECTRODE.
DE19609418C2 (en) * 1996-03-11 1998-08-13 Forschungszentrum Juelich Gmbh Coating of porous electrodes with thin layers of electrolyte
DE19628593A1 (en) * 1996-07-16 1998-01-22 Hans Hoffmann Electrode system with fuel-cell

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AU6604001A (en) 2001-12-17
CY1117289T1 (en) 2017-04-26
EP1287576B1 (en) 2015-12-23
CA2411711A1 (en) 2001-12-13
NO20025826L (en) 2003-02-06
NO328244B1 (en) 2010-01-18
NO20025826D0 (en) 2002-12-04
PT1287576E (en) 2016-03-03
DK1287576T3 (en) 2016-01-25
EP1287576A1 (en) 2003-03-05
WO2001095420A1 (en) 2001-12-13
CA2411711C (en) 2010-11-30
ES2557739T3 (en) 2016-01-28

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