CA1169117A - Process for the production of a layer of an electrode for a cell, particularly for a fuel cell and electrode containing such a layer - Google Patents
Process for the production of a layer of an electrode for a cell, particularly for a fuel cell and electrode containing such a layerInfo
- Publication number
- CA1169117A CA1169117A CA000381310A CA381310A CA1169117A CA 1169117 A CA1169117 A CA 1169117A CA 000381310 A CA000381310 A CA 000381310A CA 381310 A CA381310 A CA 381310A CA 1169117 A CA1169117 A CA 1169117A
- Authority
- CA
- Canada
- Prior art keywords
- layer
- electrode
- rolling
- process according
- thickness
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired
Links
Classifications
-
- 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
- H01M4/88—Processes of manufacture
- H01M4/8875—Methods for shaping the electrode into free-standing bodies, like sheets, films or grids, e.g. moulding, hot-pressing, casting without support, extrusion without support
-
- 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
- H01M4/88—Processes of manufacture
- H01M4/8878—Treatment steps after deposition of the catalytic active composition or after shaping of the electrode being free-standing body
- H01M4/8882—Heat treatment, e.g. drying, baking
-
- 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
- H01M4/88—Processes of manufacture
- H01M4/8878—Treatment steps after deposition of the catalytic active composition or after shaping of the electrode being free-standing body
- H01M4/8896—Pressing, rolling, calendering
-
- 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
Abstract
ABSTRACT
The invention relates to a process for the production of a layer of an electrode for a cell, particularly for a fuel cell, starting from an electrically conductive fine-grained powder and a powdery binder, according to which the powder and the binder are mixed in dry condition and the mixture is subjected to an agglomeration step, the agglo-merates obtained are broken and pressed together to form a whole and the pressed whole is rolled, in various steps, to form a layer.
The process also relates to the production of an electrode containing such a layer.
The invention relates to a process for the production of a layer of an electrode for a cell, particularly for a fuel cell, starting from an electrically conductive fine-grained powder and a powdery binder, according to which the powder and the binder are mixed in dry condition and the mixture is subjected to an agglomeration step, the agglo-merates obtained are broken and pressed together to form a whole and the pressed whole is rolled, in various steps, to form a layer.
The process also relates to the production of an electrode containing such a layer.
Description
~lt~
ELECTROCHEMISCHE ENERGIECONVERSIE N.V~-, AE 3203 Mol - Belgium PROCESS FOR THE PRODUCTION OF A LAYER 0~ AN ELECTRODE FOR A CELL, PARTICULARLY FOR A FUEL CELL AND ELECTRODE CONTAINING SUCH A LAYER
The invention relates to a process for the production of a layer of an electrode for a cell, particularly for a fuel cell, starting from an electrically conductive fine-grained powder and a powdery binder, according to which the powder and the binder are mixed in dry condition and the dry mixture is rolled to form a layer and to an electrode containing such a layer.
A process of this kind is known from the U.S. patent specifi-cation no. 4.175.055.
According to this known process, the dry mixture is fixed on a porous carrler using a vacuum technique to make the particles of the dry mixture penetrate the pores of the carrier. The dry mixture together with the carrier is compacted between rollers and thereafter the electrode obtained is sintered.
This known process is quite complicated and the conditions and/or the treatment necessary to conduct the sintering can have a bad influence on the quality of the electrode.
The process according to the invention corrects these disadvantages.
To this end the dry mixture is sub~ected to an agglomeration step, the agglomerates obtained are broken, pressed together to form one whole, and the presset whole is rolled in various steps, to form a layer.
In an advantageous embodiment of the invention a kneading operation is carried out as agglomeration step.
In a special embodiment of the invention the agglomeration step is carried out in a ball mill rotating at high speed.
In an efficient embodiment of the invention the ground agglo-merates are pressed to a thickness in the order of fifty to two hundred times the desired final thickness of the layer.
Other details and advantages of the invention will appear from the description following hereinafter of various embodiments of a pro-cess for the production of a layer of an electrode for a cell, specifi-Il'~v,~
1 ~tj'3117 cally for a fuel cell according to the invention; this description i9 given only as an example and does not limit the invention.
The powders which must occur in the electrode layer are mixed.
These powders differ according to the de~ired composition of the layer; in any case the mixture will contain an electrically conduc-tive fine-grained powder and a powdery binder.
The electrically conductive fine-grained powder may have to give the layer the required electric conductivity, in which case it con-sists of, for instance, carbon; it may also have to give the layer the required electric conductivity and, moreover, have to be catalytically active, in which case it consists, for instance, at least partly, of carbon partlcles with metal. This metal may wholly or psrtly consist of platinum. It may also wholly or partly be palladium, iridium, rhodium, ruthenium, nickel, silver and gold or a mixture of these metals.
The powdery binder is an organic binding agent, for instance polytetrafluoroethylene.
In general an apolar synthetic resin can be used a~ binder, for instance, instead of the said polytetrafluoroethylene, also polyethylene, polypropylene and polyv-inylchloride.
The weight ratio between the constituent parts of the layer depends on the desired properties, but the quantity of organic binder fluctuates, for instance, between 2 and 30 % by weight in respect of the total quantity of the layer and preferably between 3 and 30 % by weight, speciically between 5 and 25 % by weight, more specifically between 10 and 25 % by weight.
The quantities of electrically conductive fine-gralned powder and powdery binder de~tlned for the same layer are mixed intimately in dry condition in any powder mixer. The mixer consists in, for instance, a ball mill, with a contact-speed of the balls with respect to the mill of e.g. 0.1-1.0 m/s.
The mixture obtained by the mixing step is agglomerated. This is achieved by very intence kneading the mixture. Very intence kneading is understood here to mean any process in which the mixture is sub~ected to very violent successive combined acts of deformation and shearing.
The kneading requires much energy amounting to about at least 5 times, by preference 10 times, especially 20 time~ the amount of energy needed for the thorough mixing of the said powder and binder. Such a process ~ .
l.~lf;~ 7 can be carried out, for instance, with a ball mill rotating at high speed, with a contact-speed of the balls with respect to the mill of e.g. 4-6 m,!s.
The same ball mill can be used for the dry mixing and for the agglomeration, the mixing being effected at a low speed of rotation and with a larger number of smaller balls with a diameter of e.g. 10-15 mm and the agglomeration being carried out at a high speed of rotation and with a smaller number of larger balls with a diameter of e.g. 25-35 mm.
So during the mixing the pressure exercised on the powders is smaller; in the agglomeration process the pressure on the powders is greater. In consequence of the agglomeration, agglomerates will be formed, in the form of scales or skins with a surface area ranging from a new square centimetres to a few hundred square centimetres. These agglomerates are mechanically Rtrong enough to be treated.
The agglomerates are ground fine on laboratory scale in an electric coffee grinder or in a so-called mixer. On an industrial scale a so-called granulator is used for this purpose.
From the ground agglomerates a useful fraction is sifted out e.g the parts smaller than 0.6 mm.
This sifted powder is pressed into the form of a sheet with a thickneffs of a few mm. The sheet thus obtained is strong enough to be treated.
The sheet is now brought to its desired thickness by by pre-ference blaxial rolling; thl~ will also lncrease the surface area and strengthen the mechanical cohesion.
The rolling-process ls effected in various rolling-steps of which the smount lles by preference between 10 and 50, especially bet-ween 30 and 45. By preference every rolling-step is effected with a rolling-direction which is turned 90 with respect to the rolling-dlrection of the former step.
The step-process described above and especially the mixing and the rolling ar by preference effected at about room-te~perature e.8.
between 280 and 310 K.
By the rolling-~teps described above a raising of the binder percentage in the outer part of the layer is brought about. Thus a layer i8 obtained which layer at both sides is covered with a partial layer enriched with binder with a thichknesff of about 10-2 ~m. By these psr-4 .~.*~j~117 tial layers the binding together of various layers becomes more easy.The binder percentage in the said partial layers rises with the rising of the amount of rolling-steps. E.g. when is started with 85 % by weight of graphite and 15 % by weight of polytetrafluoroethylene (PTFE) as binder, which in a homogeneous mixture equals 88.60 atom ~ of C and 11.40 atom % of F, it is found that after one rolling-step the C con-centration in said partial layers is already dropped to about 70 atom ~, and with the further rolling-steps this concentration drops even further. So in the said partial layers the PTFE concentration clearly rises. The hydrophobicity also rises than.
The layer eventually obtained is cut off to the desired dimen-sions ant optionally ~oined with other layers ant with a collector to form an electrode, e.g. by one or more pres~-steps and/or one or more rolllng-steps.
It i8 remarked that from the FR patent 1.582.267 it is known ~o form an electrode layer by pressing ground flakes consisting of graphite, PTF~ and sodiumsulfate. Such an electrode layer do~s not have the special advantages of a layer accordlng to the invention, like a very good hydrofobic performance and mechanical strength.
It is of a great advantage in maklng an electrode to combine, by preference by a light rolling-step, a layer prepared according to the lnventlon wlth at least a second blnder containlng layer, which second layer is by preference also prepared according to the lnvention. In this way a multilayer electrode is formed of which at least one partial layer enriched with binder with risen hydrophobicity is closed in between two electrode layers, 80 that this very thin partial layer en~oys a great mechanical protection. A multilayer electrode composed in such way has a ~trongly improved quality because it has at least one enclosed, mechani-cally strong barrier (the enclosed partial layer enriched with binder) a8ainst over-saturation with electrolyte.
The application of at least two layers prepared according to the lnvention has as further advantage that the rolllng ln two dlrec-tlons ln the preparatlon can be omitted if in the composltlon of the multllayer the layers are flxed together crosswlse, thls means that the rolllng-orlentation of the succeeding layers hsd to be turned 90 each time.
The invention also covers an electrode, partlcularly a flat fuel cell electrode, which con~lsts at least of one or more layers pre-5 ~1~i'3117 pared according to the inventlon, by preference connected with a porouscollector consisting of a conductive material, e.g. a metal gauze, an expanded metal or a perforated metal plate. Suitable metals for this collector are e.g. copper, iron, tantalum, zirconium, noble metals such as gold, silver, platinum, palladium, osmiu~, ruthenium and by pre-ference nickel. These electrodes can very suitably be mounted in a frame, by preference at least partly consisting of a thermoplastic. Thus they form electrode elements which can be stacked and of which batteries containing a stack of ~uch elements can be made.
For the purpose of elucidatlng the invention the production is described, hereinafter, of a fuel cell electrode with a porous multilayer, two layers of which are made according to the invention.
The electrode consi~ts of a collector gauze fro~ pure nickel with three part layers linked to it in the following order.
The layers are to be composed as follows.
First layer thickness 40 ~m 85 % by weight of carbon powder 15 % by weight of polytetrafluoroe~hylene Second layer thickness 70 ~m 53.4 % by weight of carbon powder 26.6 % by weight of carbon whereon and wherein 5 % by weight of Pt 20 % by weight of polytetrafluoroethylene Third layer thickness 240 ~m 100 % by weight of polytetrafluoroethylene, except for the pore-forming agent, which i9 not retained in the layer.
As carbon powder, a carbon powder with a grain size smaller than 1 micron and a specific surface of about 800 m2/g i8 used.
As polytetrafluoroethylene the commercial product Teflon of Du Pont 18 used.
In order to make the third layer porous, ammoniumbicarbonate is used in it.
The productlon comprises four steps:
I. The preparation of the powders and of the nickel collector II. The making of the agglomerate6 III. The making of the films IV. The conditioning of the electrode.
*trade mark I. The preparation.
The pore-forming agent, that is the ammoniumbicarbonate, is broken and sifted to obtain the useful fraction with a grain size of 10 to 30 ~m for the third layer.
The binder, that is the Teflon, is sifted through a sieve with a mesh size of 600 ~m. The usable fraction, thi~ is the part with a grain size smaller than 600 ~m, i8 used as binder for the three layers.
The collector gauze i8 cut to size.
II. Making of the agglomerates.
The mixtures of powders according to the compositions given above for the three layers do not form rollable substances. Each of these mixtures must first be transformed into agglomerates, which are broken and sifted, after which disc~ are pressed. To this end the powder mixtures must be sub~ected to four operation~:
1. Mixing
ELECTROCHEMISCHE ENERGIECONVERSIE N.V~-, AE 3203 Mol - Belgium PROCESS FOR THE PRODUCTION OF A LAYER 0~ AN ELECTRODE FOR A CELL, PARTICULARLY FOR A FUEL CELL AND ELECTRODE CONTAINING SUCH A LAYER
The invention relates to a process for the production of a layer of an electrode for a cell, particularly for a fuel cell, starting from an electrically conductive fine-grained powder and a powdery binder, according to which the powder and the binder are mixed in dry condition and the dry mixture is rolled to form a layer and to an electrode containing such a layer.
A process of this kind is known from the U.S. patent specifi-cation no. 4.175.055.
According to this known process, the dry mixture is fixed on a porous carrler using a vacuum technique to make the particles of the dry mixture penetrate the pores of the carrier. The dry mixture together with the carrier is compacted between rollers and thereafter the electrode obtained is sintered.
This known process is quite complicated and the conditions and/or the treatment necessary to conduct the sintering can have a bad influence on the quality of the electrode.
The process according to the invention corrects these disadvantages.
To this end the dry mixture is sub~ected to an agglomeration step, the agglomerates obtained are broken, pressed together to form one whole, and the presset whole is rolled in various steps, to form a layer.
In an advantageous embodiment of the invention a kneading operation is carried out as agglomeration step.
In a special embodiment of the invention the agglomeration step is carried out in a ball mill rotating at high speed.
In an efficient embodiment of the invention the ground agglo-merates are pressed to a thickness in the order of fifty to two hundred times the desired final thickness of the layer.
Other details and advantages of the invention will appear from the description following hereinafter of various embodiments of a pro-cess for the production of a layer of an electrode for a cell, specifi-Il'~v,~
1 ~tj'3117 cally for a fuel cell according to the invention; this description i9 given only as an example and does not limit the invention.
The powders which must occur in the electrode layer are mixed.
These powders differ according to the de~ired composition of the layer; in any case the mixture will contain an electrically conduc-tive fine-grained powder and a powdery binder.
The electrically conductive fine-grained powder may have to give the layer the required electric conductivity, in which case it con-sists of, for instance, carbon; it may also have to give the layer the required electric conductivity and, moreover, have to be catalytically active, in which case it consists, for instance, at least partly, of carbon partlcles with metal. This metal may wholly or psrtly consist of platinum. It may also wholly or partly be palladium, iridium, rhodium, ruthenium, nickel, silver and gold or a mixture of these metals.
The powdery binder is an organic binding agent, for instance polytetrafluoroethylene.
In general an apolar synthetic resin can be used a~ binder, for instance, instead of the said polytetrafluoroethylene, also polyethylene, polypropylene and polyv-inylchloride.
The weight ratio between the constituent parts of the layer depends on the desired properties, but the quantity of organic binder fluctuates, for instance, between 2 and 30 % by weight in respect of the total quantity of the layer and preferably between 3 and 30 % by weight, speciically between 5 and 25 % by weight, more specifically between 10 and 25 % by weight.
The quantities of electrically conductive fine-gralned powder and powdery binder de~tlned for the same layer are mixed intimately in dry condition in any powder mixer. The mixer consists in, for instance, a ball mill, with a contact-speed of the balls with respect to the mill of e.g. 0.1-1.0 m/s.
The mixture obtained by the mixing step is agglomerated. This is achieved by very intence kneading the mixture. Very intence kneading is understood here to mean any process in which the mixture is sub~ected to very violent successive combined acts of deformation and shearing.
The kneading requires much energy amounting to about at least 5 times, by preference 10 times, especially 20 time~ the amount of energy needed for the thorough mixing of the said powder and binder. Such a process ~ .
l.~lf;~ 7 can be carried out, for instance, with a ball mill rotating at high speed, with a contact-speed of the balls with respect to the mill of e.g. 4-6 m,!s.
The same ball mill can be used for the dry mixing and for the agglomeration, the mixing being effected at a low speed of rotation and with a larger number of smaller balls with a diameter of e.g. 10-15 mm and the agglomeration being carried out at a high speed of rotation and with a smaller number of larger balls with a diameter of e.g. 25-35 mm.
So during the mixing the pressure exercised on the powders is smaller; in the agglomeration process the pressure on the powders is greater. In consequence of the agglomeration, agglomerates will be formed, in the form of scales or skins with a surface area ranging from a new square centimetres to a few hundred square centimetres. These agglomerates are mechanically Rtrong enough to be treated.
The agglomerates are ground fine on laboratory scale in an electric coffee grinder or in a so-called mixer. On an industrial scale a so-called granulator is used for this purpose.
From the ground agglomerates a useful fraction is sifted out e.g the parts smaller than 0.6 mm.
This sifted powder is pressed into the form of a sheet with a thickneffs of a few mm. The sheet thus obtained is strong enough to be treated.
The sheet is now brought to its desired thickness by by pre-ference blaxial rolling; thl~ will also lncrease the surface area and strengthen the mechanical cohesion.
The rolling-process ls effected in various rolling-steps of which the smount lles by preference between 10 and 50, especially bet-ween 30 and 45. By preference every rolling-step is effected with a rolling-direction which is turned 90 with respect to the rolling-dlrection of the former step.
The step-process described above and especially the mixing and the rolling ar by preference effected at about room-te~perature e.8.
between 280 and 310 K.
By the rolling-~teps described above a raising of the binder percentage in the outer part of the layer is brought about. Thus a layer i8 obtained which layer at both sides is covered with a partial layer enriched with binder with a thichknesff of about 10-2 ~m. By these psr-4 .~.*~j~117 tial layers the binding together of various layers becomes more easy.The binder percentage in the said partial layers rises with the rising of the amount of rolling-steps. E.g. when is started with 85 % by weight of graphite and 15 % by weight of polytetrafluoroethylene (PTFE) as binder, which in a homogeneous mixture equals 88.60 atom ~ of C and 11.40 atom % of F, it is found that after one rolling-step the C con-centration in said partial layers is already dropped to about 70 atom ~, and with the further rolling-steps this concentration drops even further. So in the said partial layers the PTFE concentration clearly rises. The hydrophobicity also rises than.
The layer eventually obtained is cut off to the desired dimen-sions ant optionally ~oined with other layers ant with a collector to form an electrode, e.g. by one or more pres~-steps and/or one or more rolllng-steps.
It i8 remarked that from the FR patent 1.582.267 it is known ~o form an electrode layer by pressing ground flakes consisting of graphite, PTF~ and sodiumsulfate. Such an electrode layer do~s not have the special advantages of a layer accordlng to the invention, like a very good hydrofobic performance and mechanical strength.
It is of a great advantage in maklng an electrode to combine, by preference by a light rolling-step, a layer prepared according to the lnventlon wlth at least a second blnder containlng layer, which second layer is by preference also prepared according to the lnvention. In this way a multilayer electrode is formed of which at least one partial layer enriched with binder with risen hydrophobicity is closed in between two electrode layers, 80 that this very thin partial layer en~oys a great mechanical protection. A multilayer electrode composed in such way has a ~trongly improved quality because it has at least one enclosed, mechani-cally strong barrier (the enclosed partial layer enriched with binder) a8ainst over-saturation with electrolyte.
The application of at least two layers prepared according to the lnvention has as further advantage that the rolllng ln two dlrec-tlons ln the preparatlon can be omitted if in the composltlon of the multllayer the layers are flxed together crosswlse, thls means that the rolllng-orlentation of the succeeding layers hsd to be turned 90 each time.
The invention also covers an electrode, partlcularly a flat fuel cell electrode, which con~lsts at least of one or more layers pre-5 ~1~i'3117 pared according to the inventlon, by preference connected with a porouscollector consisting of a conductive material, e.g. a metal gauze, an expanded metal or a perforated metal plate. Suitable metals for this collector are e.g. copper, iron, tantalum, zirconium, noble metals such as gold, silver, platinum, palladium, osmiu~, ruthenium and by pre-ference nickel. These electrodes can very suitably be mounted in a frame, by preference at least partly consisting of a thermoplastic. Thus they form electrode elements which can be stacked and of which batteries containing a stack of ~uch elements can be made.
For the purpose of elucidatlng the invention the production is described, hereinafter, of a fuel cell electrode with a porous multilayer, two layers of which are made according to the invention.
The electrode consi~ts of a collector gauze fro~ pure nickel with three part layers linked to it in the following order.
The layers are to be composed as follows.
First layer thickness 40 ~m 85 % by weight of carbon powder 15 % by weight of polytetrafluoroe~hylene Second layer thickness 70 ~m 53.4 % by weight of carbon powder 26.6 % by weight of carbon whereon and wherein 5 % by weight of Pt 20 % by weight of polytetrafluoroethylene Third layer thickness 240 ~m 100 % by weight of polytetrafluoroethylene, except for the pore-forming agent, which i9 not retained in the layer.
As carbon powder, a carbon powder with a grain size smaller than 1 micron and a specific surface of about 800 m2/g i8 used.
As polytetrafluoroethylene the commercial product Teflon of Du Pont 18 used.
In order to make the third layer porous, ammoniumbicarbonate is used in it.
The productlon comprises four steps:
I. The preparation of the powders and of the nickel collector II. The making of the agglomerate6 III. The making of the films IV. The conditioning of the electrode.
*trade mark I. The preparation.
The pore-forming agent, that is the ammoniumbicarbonate, is broken and sifted to obtain the useful fraction with a grain size of 10 to 30 ~m for the third layer.
The binder, that is the Teflon, is sifted through a sieve with a mesh size of 600 ~m. The usable fraction, thi~ is the part with a grain size smaller than 600 ~m, i8 used as binder for the three layers.
The collector gauze i8 cut to size.
II. Making of the agglomerates.
The mixtures of powders according to the compositions given above for the three layers do not form rollable substances. Each of these mixtures must first be transformed into agglomerates, which are broken and sifted, after which disc~ are pressed. To this end the powder mixtures must be sub~ected to four operation~:
1. Mixing
2. Agglomerating
3. Breaking and sifting
4. Pressing 1. Mixing.
First layer : 85 g carbon powder and 15 g Teflon with a particle size smaller than 600 ~m are intensely mixed in a ball mill.
14 wear-resistant balls of a diameter of 10 ~m are adted to increase the mixing effect.
The mlxing time is 30 minutes.
Second layer : 53.4 g carbon powder, 26.6 g carbon powder carrying
First layer : 85 g carbon powder and 15 g Teflon with a particle size smaller than 600 ~m are intensely mixed in a ball mill.
14 wear-resistant balls of a diameter of 10 ~m are adted to increase the mixing effect.
The mlxing time is 30 minutes.
Second layer : 53.4 g carbon powder, 26.6 g carbon powder carrying
5 % platinum and 20 g Teflon with a particle size smaller than 600 ~m are mixed in the same way as the first layer.
Third layer : 84 g ammoniumbicarbonste and 36 g Teflon with a par-ticle size smaller than 600 ~m are mixed like the first and the second layer.
2. Agglomerating The mixtures of the three layers are sub~ected separately to the for-mation of an agglomerate.
*trade mark 7 1 ~ 117 The agglomerate formation takes place in the same ball mill in which the mixing was carried out.
The 14 balls with a diameter of lO mm are replaced by 4 balls with a diameter of 30 mm and the speed of rotation of the mill drum ls se~
as high as possible.
The operation lasts 60 minutes.
3. Breaking and sifting.
As agglomerates are of irregular shapes, they are broken.
On a laboratory scale this can be done with a coffee grinder. They are sifted through a 30-mesh sieve in order to obtain material that can be metered out.
4. Pressing.
The broken and sifted agglomerate is used as starting material for making discs.
For the first and for the second layer 80 g agglomerate is poured into a mould each time and pressed under a pressure of 30 tons to a thickness of 4.5 mm.
For the third layer 120 g agglomerate is poured into the mould and pressed under a pressure of 5 tons to a thickness of practically 7 mm.
III. Maklng of films by rolling.
Starting from the dlscs obtained by pressing, the films and layers mentioned hereinafter are formed by rolling. For all rolling operations mentioned hereinafter the linear rolling speed is 5.6 m/mlnute.
a. Production of the film for the first layer.
Starting from the tisc formed, having a thickness of 4.5 mm, a film with a thicknes~ of 300 ~m is rolled in various rolling operations.
The thickness is reduced by 200 ~m in each rolling operation or pass until a film thickness of 1.3 mm has been reached, subsequently by 100 ~m until a thickness of 400 ~m has been reached and subsequently by 50 ~m until the final thickness of 300 ~m has been reached.
b. Production of the film for the second layer.
Starting from the disc formed, having a thickness of 4.5 mm, a film with a thickness of 600 ~m is rolled in various rolling operations.
8 1 ~ 117 The change in thickness per rolling operation or pass is 200 ~Im until a film thickness of 1.3 mm has been reached, subsequently 100 ~m until a thickness of 700 ~m has been reached and subsequently S0 ~m until the final thickness of 600 ~m has been reached.
c. Production of the double layer (first and second layers).
The double layer is formed by attaching the film for the first layer~
having a thickness of 300 ~m, onto the film for the second layer, having a thickness of 600 ~m, and by bringing the whole to a thickness of 450 ~m in various rolling steps.
The decrease in thickness per rolling step is 100 ~m until the sheet thickness is 500 ~m.
The finishing is further effected by a rolling step with a decrease in thickness of 50 ~m.
d. Production of film for the third layer.
Starting from the disc formed for the third layer, a film with a thickness of 900 ~m is rolled in various rolling operations.
The decrease in thickness per rolling operation or pa~s is 200 ~m until a film thicknes~ of 1.3 mm has been reached and subsequently 50 ~m until the final thickness of 900 ~m has been reached.
e. Production of the multilayer.
The multilayer 18 made by rolling the double layer formed, having a thlckness of 450 ~m, onto the third layer formed, having a thickness of 900 ~m, in various rolling steps until a final thickness of 350 +
10 ~m has been reached.
The decrease ln thickness per rolling step 18 50 ~m.
f. The final-rolling.
The final rolling consists in attaching the multilayer, having a thickness of 350 ~m, onto a collector gauze, havlng a thickness of again 350 ~m, by bringing the whole, in one rolling operation, to 400 + 10 ~m. So the roll opening is set at 400 ~m.
IV. Conditioning.
The electrode produced is conditioned by, among other things, removlng the pore-forming agent from the third layer, for instance by thermal treatment.
The maklng of an electrode as describet above comprises the making of two layers, of a double layer and of a multllayer according to the invention.
9 .~ 1lti'3~ 17 The invention, however, is by no means limited to the above embodiments, and within the scope of the patent application many altera-tions can be mada to the embodiments described, among other things as far as the component parts are concerned.
S The invention can be applled also in, among other things, the production of a cathode for a metal-air cell.
Third layer : 84 g ammoniumbicarbonste and 36 g Teflon with a par-ticle size smaller than 600 ~m are mixed like the first and the second layer.
2. Agglomerating The mixtures of the three layers are sub~ected separately to the for-mation of an agglomerate.
*trade mark 7 1 ~ 117 The agglomerate formation takes place in the same ball mill in which the mixing was carried out.
The 14 balls with a diameter of lO mm are replaced by 4 balls with a diameter of 30 mm and the speed of rotation of the mill drum ls se~
as high as possible.
The operation lasts 60 minutes.
3. Breaking and sifting.
As agglomerates are of irregular shapes, they are broken.
On a laboratory scale this can be done with a coffee grinder. They are sifted through a 30-mesh sieve in order to obtain material that can be metered out.
4. Pressing.
The broken and sifted agglomerate is used as starting material for making discs.
For the first and for the second layer 80 g agglomerate is poured into a mould each time and pressed under a pressure of 30 tons to a thickness of 4.5 mm.
For the third layer 120 g agglomerate is poured into the mould and pressed under a pressure of 5 tons to a thickness of practically 7 mm.
III. Maklng of films by rolling.
Starting from the dlscs obtained by pressing, the films and layers mentioned hereinafter are formed by rolling. For all rolling operations mentioned hereinafter the linear rolling speed is 5.6 m/mlnute.
a. Production of the film for the first layer.
Starting from the tisc formed, having a thickness of 4.5 mm, a film with a thicknes~ of 300 ~m is rolled in various rolling operations.
The thickness is reduced by 200 ~m in each rolling operation or pass until a film thickness of 1.3 mm has been reached, subsequently by 100 ~m until a thickness of 400 ~m has been reached and subsequently by 50 ~m until the final thickness of 300 ~m has been reached.
b. Production of the film for the second layer.
Starting from the disc formed, having a thickness of 4.5 mm, a film with a thickness of 600 ~m is rolled in various rolling operations.
8 1 ~ 117 The change in thickness per rolling operation or pass is 200 ~Im until a film thickness of 1.3 mm has been reached, subsequently 100 ~m until a thickness of 700 ~m has been reached and subsequently S0 ~m until the final thickness of 600 ~m has been reached.
c. Production of the double layer (first and second layers).
The double layer is formed by attaching the film for the first layer~
having a thickness of 300 ~m, onto the film for the second layer, having a thickness of 600 ~m, and by bringing the whole to a thickness of 450 ~m in various rolling steps.
The decrease in thickness per rolling step is 100 ~m until the sheet thickness is 500 ~m.
The finishing is further effected by a rolling step with a decrease in thickness of 50 ~m.
d. Production of film for the third layer.
Starting from the disc formed for the third layer, a film with a thickness of 900 ~m is rolled in various rolling operations.
The decrease in thickness per rolling operation or pa~s is 200 ~m until a film thicknes~ of 1.3 mm has been reached and subsequently 50 ~m until the final thickness of 900 ~m has been reached.
e. Production of the multilayer.
The multilayer 18 made by rolling the double layer formed, having a thlckness of 450 ~m, onto the third layer formed, having a thickness of 900 ~m, in various rolling steps until a final thickness of 350 +
10 ~m has been reached.
The decrease ln thickness per rolling step 18 50 ~m.
f. The final-rolling.
The final rolling consists in attaching the multilayer, having a thickness of 350 ~m, onto a collector gauze, havlng a thickness of again 350 ~m, by bringing the whole, in one rolling operation, to 400 + 10 ~m. So the roll opening is set at 400 ~m.
IV. Conditioning.
The electrode produced is conditioned by, among other things, removlng the pore-forming agent from the third layer, for instance by thermal treatment.
The maklng of an electrode as describet above comprises the making of two layers, of a double layer and of a multllayer according to the invention.
9 .~ 1lti'3~ 17 The invention, however, is by no means limited to the above embodiments, and within the scope of the patent application many altera-tions can be mada to the embodiments described, among other things as far as the component parts are concerned.
S The invention can be applled also in, among other things, the production of a cathode for a metal-air cell.
Claims (12)
PROPERTY OR PRIVILEGE IS CLAIMED ARE DEFINED AS FOLLOWS:
1. A process for the production of a layer for an electrode for a cell, comprising the steps of:
(a) mixing an electrically conductive fine-grained powder and a powdery binder in a dry condition;
(b) subjecting the conductive fine-grained powder and a powdery binder mixed according to step (a) to agglomeration in a dry condition;
(c) breaking the agglomerates formed according to step (b) to obtain particles;
(d) pressing the particles obtained according to step (c) to form a mass; and (e) rolling the mass obtained according to step (d) to form a layer.
(a) mixing an electrically conductive fine-grained powder and a powdery binder in a dry condition;
(b) subjecting the conductive fine-grained powder and a powdery binder mixed according to step (a) to agglomeration in a dry condition;
(c) breaking the agglomerates formed according to step (b) to obtain particles;
(d) pressing the particles obtained according to step (c) to form a mass; and (e) rolling the mass obtained according to step (d) to form a layer.
2. A process according to claim 1, wherein step (d) is practiced so as to form a mass having a thickness of between 50 and 200 times the thickness of the layer formed according to step (e).
3. A process according to claim 1, wherein step (b) is practiced so as to form scale-shaped agglomerates having a surface area between a few square centimeters to a few hundred square centimeters.
4. A process according to claim 1, 2 or 3, wherein step (d) is practiced utilizing particles having sizes less than 600 µm.
5. A process according to claim 1, 2 or 3, wherein at least two layers are produced and are rolled together to form one layer.
6. A process according to claim 1, 2 or 3, wherein step (e) for succeeding rolling-steps different rolling-directions are applied.
7. A process according to claim 1, 2 or 3, wherein step (e) between 10 and 50 rolling-steps are used.
8. A process according to claim 1, 2 or 3, wherein all the process-steps are effected at a temperature of between 280 and 310°K.
9. A process according to claim 1, 2 or 3, wherein between 2 to 30% by weight of the layer obtained in step (e) consists of the powdery binder.
10. A process according to claim 1, 2 or 3, wherein said cell is a fuel cell.
11. An electrode comprising at least one layer produced according to claim 1, 2 or 3.
12. An electrode comprising at least one layer produced according to claim 1, 2 or 3, wherein said at least one layer is attached to a porous collector.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| NL8003949A NL8003949A (en) | 1980-07-09 | 1980-07-09 | METHOD FOR MANUFACTURING A COAT OF AN ELECTRODE FOR A CELL, IN PARTICULAR FOR A FUEL CELL. |
| NL8003949 | 1980-07-09 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA1169117A true CA1169117A (en) | 1984-06-12 |
Family
ID=19835593
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA000381310A Expired CA1169117A (en) | 1980-07-09 | 1981-07-08 | Process for the production of a layer of an electrode for a cell, particularly for a fuel cell and electrode containing such a layer |
Country Status (8)
| Country | Link |
|---|---|
| US (1) | US4383010A (en) |
| EP (1) | EP0043632B1 (en) |
| JP (1) | JPS5746475A (en) |
| AT (1) | ATE12559T1 (en) |
| CA (1) | CA1169117A (en) |
| DE (1) | DE3169672D1 (en) |
| ES (1) | ES8204884A1 (en) |
| NL (1) | NL8003949A (en) |
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| US4529672A (en) * | 1983-03-29 | 1985-07-16 | Union Carbide Corporation | Process of making electrochemical electrodes and electrodes made thereby |
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| LU85822A1 (en) * | 1985-03-27 | 1986-10-06 | Cen Centre Energie Nucleaire | PROCESS FOR PRODUCING A POROUS STRUCTURE COMPRISING ORGANIC MATERIAL DISPERSED IN A BINDER |
| JPS63187574A (en) * | 1987-01-29 | 1988-08-03 | Japan Gore Tex Inc | Fuel cell electrode-matrix monobloc forming and its manufacture |
| JP2575840B2 (en) * | 1988-09-13 | 1997-01-29 | 株式会社東芝 | Dry manufacturing method of hydrogen storage alloy electrode |
| JPH05258755A (en) * | 1991-12-31 | 1993-10-08 | Stonehard Assoc Inc | Manufacture of solid polyelectrolyte fuel cell |
| DE19509749C2 (en) * | 1995-03-17 | 1997-01-23 | Deutsche Forsch Luft Raumfahrt | Process for producing a composite of electrode material, catalyst material and a solid electrolyte membrane |
| DE19548422A1 (en) * | 1995-12-22 | 1997-09-11 | Hoechst Ag | Composites and their continuous production |
| DE19548421B4 (en) * | 1995-12-22 | 2004-06-03 | Celanese Ventures Gmbh | Process for the continuous production of membrane electrode assemblies |
| DE19608680A1 (en) * | 1996-03-06 | 1997-09-11 | Mtu Friedrichshafen Gmbh | Manufacture of foil filled with electrode powder |
| US6967183B2 (en) | 1998-08-27 | 2005-11-22 | Cabot Corporation | Electrocatalyst powders, methods for producing powders and devices fabricated from same |
| JP3356728B2 (en) * | 1999-08-27 | 2002-12-16 | 日清紡績株式会社 | Apparatus for charging powdery raw material for fuel cell separator, method for manufacturing fuel cell separator, and fuel cell separator |
| KR20040077655A (en) | 2001-10-19 | 2004-09-06 | 슈페리어 마이크로파우더스 엘엘씨 | Tape compositions for the deposition of electronic features |
| US7508651B2 (en) * | 2003-07-09 | 2009-03-24 | Maxwell Technologies, Inc. | Dry particle based adhesive and dry film and methods of making same |
| US20100014215A1 (en) * | 2004-04-02 | 2010-01-21 | Maxwell Technologies, Inc. | Recyclable dry particle based electrode and methods of making same |
| US7342770B2 (en) * | 2003-07-09 | 2008-03-11 | Maxwell Technologies, Inc. | Recyclable dry particle based adhesive electrode and methods of making same |
| US7352558B2 (en) * | 2003-07-09 | 2008-04-01 | Maxwell Technologies, Inc. | Dry particle based capacitor and methods of making same |
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| US20050250011A1 (en) * | 2004-04-02 | 2005-11-10 | Maxwell Technologies, Inc. | Particle packaging systems and methods |
| US20070122698A1 (en) * | 2004-04-02 | 2007-05-31 | Maxwell Technologies, Inc. | Dry-particle based adhesive and dry film and methods of making same |
| US20110165318A9 (en) * | 2004-04-02 | 2011-07-07 | Maxwell Technologies, Inc. | Electrode formation by lamination of particles onto a current collector |
| US7791860B2 (en) | 2003-07-09 | 2010-09-07 | Maxwell Technologies, Inc. | Particle based electrodes and methods of making same |
| US20060147712A1 (en) * | 2003-07-09 | 2006-07-06 | Maxwell Technologies, Inc. | Dry particle based adhesive electrode and methods of making same |
| US20050266298A1 (en) * | 2003-07-09 | 2005-12-01 | Maxwell Technologies, Inc. | Dry particle based electro-chemical device and methods of making same |
| US7920371B2 (en) * | 2003-09-12 | 2011-04-05 | Maxwell Technologies, Inc. | Electrical energy storage devices with separator between electrodes and methods for fabricating the devices |
| JP2005116762A (en) | 2003-10-07 | 2005-04-28 | Fujitsu Ltd | Method for protecting semiconductor device, cover for semiconductor device, semiconductor device unit, and packaging structure of semiconductor device |
| US7495349B2 (en) * | 2003-10-20 | 2009-02-24 | Maxwell Technologies, Inc. | Self aligning electrode |
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| US7492571B2 (en) * | 2004-04-02 | 2009-02-17 | Linda Zhong | Particles based electrodes and methods of making same |
| US20060137158A1 (en) * | 2004-04-02 | 2006-06-29 | Maxwell Technologies, Inc. | Dry-particle packaging systems and methods of making same |
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| US7647210B2 (en) * | 2006-02-20 | 2010-01-12 | Ford Global Technologies, Llc | Parametric modeling method and system for conceptual vehicle design |
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| US8518573B2 (en) * | 2006-09-29 | 2013-08-27 | Maxwell Technologies, Inc. | Low-inductive impedance, thermally decoupled, radii-modulated electrode core |
| US20080204973A1 (en) * | 2007-02-28 | 2008-08-28 | Maxwell Technologies, Inc. | Ultracapacitor electrode with controlled iron content |
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| US8926869B2 (en) | 2007-10-28 | 2015-01-06 | Clover Technologies Group, Llc | Method and composition for recoating toner cartridge developing member |
| EP2230561A1 (en) * | 2009-03-20 | 2010-09-22 | Wazana Brothers International, Inc., d/b/a Micro Solutions Enterprises | Method and composition for recoating toner cartridge developing member |
| US8231827B2 (en) * | 2009-06-17 | 2012-07-31 | The Gates Corporation | Method of manufacturing powder metal plates |
| EP2770565A1 (en) | 2013-02-26 | 2014-08-27 | Vito NV | Method of manufacturing gas diffusion electrodes |
| DE102018209955A1 (en) | 2018-06-20 | 2019-12-24 | Robert Bosch Gmbh | Process for the production of a porous carbon composite material for electrochemical cells |
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| US3181973A (en) * | 1960-12-28 | 1965-05-04 | Electric Storage Battery Co | Fuel cell electrode and method of making the same |
| US3423246A (en) * | 1964-01-06 | 1969-01-21 | Exxon Research Engineering Co | Leakproof electrode |
| DE1671713B2 (en) * | 1967-09-16 | 1976-07-29 | Battelle-Institut E.V., 6000 Frankfurt | METHOD FOR THE PRODUCTION OF POROES, ELECTRODES FOR FUEL ELEMENTS, COMPOSING A HYDROPHILE AND A HYDROPHOBIC LAYER |
| CA940196A (en) * | 1968-01-31 | 1974-01-15 | Matsushita Electric Industrial Co., Ltd. | Electrode for batteries |
| DE2023868A1 (en) * | 1970-05-15 | 1971-11-25 | Siemens Ag | Method and device for producing catalyst layers for electrodes in electrochemical cells, in particular fuel elements |
| US3935029A (en) * | 1971-11-18 | 1976-01-27 | Energy Research Corporation | Method of fabricating a carbon - polytetrafluoroethylene electrode - support |
| CA1008623A (en) * | 1972-02-11 | 1977-04-19 | Gould Inc. | Process and apparatus for manufacture of an electrode |
| DE2556731C3 (en) * | 1975-12-17 | 1979-11-22 | Licentia Patent-Verwaltungs-Gmbh, 6000 Frankfurt | Gas diffusion electrode for electrochemical cells with acidic electrolytes and process for their manufacture |
| US4123606A (en) * | 1977-09-21 | 1978-10-31 | E. I. Du Pont De Nemours And Company | Deagglomeration process |
| US4177159A (en) * | 1978-06-28 | 1979-12-04 | United Technologies Corporation | Catalytic dry powder material for fuel cell electrodes comprising fluorocarbon polymer and precatalyzed carbon |
| US4175055A (en) * | 1978-06-28 | 1979-11-20 | United Technologies Corporation | Dry mix method for making an electrochemical cell electrode |
| DE2941774C2 (en) * | 1979-10-16 | 1985-03-21 | Varta Batterie Ag, 3000 Hannover | Method and device for producing a plastic-bonded activated carbon layer for thin gas diffusion electrodes |
| FR2468218A1 (en) * | 1979-10-18 | 1981-04-30 | Alsthom Cgee | METHOD OF MANUFACTURING BY CALENDERING POROUS THIN STRIPS AND PRODUCTS OBTAINED, ESPECIALLY ELECTRODES FOR FUEL CELLS |
-
1980
- 1980-07-09 NL NL8003949A patent/NL8003949A/en not_active Application Discontinuation
-
1981
- 1981-07-07 ES ES503721A patent/ES8204884A1/en not_active Expired
- 1981-07-08 AT AT81200786T patent/ATE12559T1/en not_active IP Right Cessation
- 1981-07-08 EP EP81200786A patent/EP0043632B1/en not_active Expired
- 1981-07-08 CA CA000381310A patent/CA1169117A/en not_active Expired
- 1981-07-08 DE DE8181200786T patent/DE3169672D1/en not_active Expired
- 1981-07-09 JP JP56106302A patent/JPS5746475A/en active Granted
- 1981-07-09 US US06/281,851 patent/US4383010A/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| DE3169672D1 (en) | 1985-05-09 |
| US4383010A (en) | 1983-05-10 |
| ES503721A0 (en) | 1982-05-16 |
| ATE12559T1 (en) | 1985-04-15 |
| ES8204884A1 (en) | 1982-05-16 |
| EP0043632A1 (en) | 1982-01-13 |
| JPH0254622B2 (en) | 1990-11-22 |
| NL8003949A (en) | 1982-02-01 |
| JPS5746475A (en) | 1982-03-16 |
| EP0043632B1 (en) | 1985-04-03 |
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