GB1575231A - Components employing solid ionic conducting material - Google Patents

Components employing solid ionic conducting material Download PDF

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Publication number
GB1575231A
GB1575231A GB1002/77A GB100277A GB1575231A GB 1575231 A GB1575231 A GB 1575231A GB 1002/77 A GB1002/77 A GB 1002/77A GB 100277 A GB100277 A GB 100277A GB 1575231 A GB1575231 A GB 1575231A
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United Kingdom
Prior art keywords
component
alumina
beta
modified
barium
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Expired
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GB1002/77A
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Chloride Silent Power Ltd
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Chloride Silent Power Ltd
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Publication date
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Priority to GB1002/77A priority Critical patent/GB1575231A/en
Publication of GB1575231A publication Critical patent/GB1575231A/en
Expired legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
    • C04B35/111—Fine ceramics
    • C04B35/113—Fine ceramics based on beta-aluminium oxide
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
    • C04B41/5007—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with salts or salty compositions, e.g. for salt glazing
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
    • C04B41/81—Coating or impregnation
    • C04B41/85—Coating or impregnation with inorganic materials
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/36—Accumulators not provided for in groups H01M10/05-H01M10/34
    • H01M10/39—Accumulators not provided for in groups H01M10/05-H01M10/34 working at high temperature
    • H01M10/3909—Sodium-sulfur cells
    • H01M10/3918—Sodium-sulfur cells characterised by the electrolyte
    • H01M10/3927—Several layers of electrolyte or coatings containing electrolyte
    • 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
    • Y02E60/10—Energy storage using batteries

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Secondary Cells (AREA)
  • Compositions Of Oxide Ceramics (AREA)

Description

($4) IMPROVEMENTS IN OR RELATING TO COMPONENTS EMPLOYING SOLID IONIC CONDUCTING MATERIAL (71) We, CHLORIDE SILENT POWER LIMITED, a British Company, of 52 Grosvenor Gardens, London, SW1W OAU, do hereby declare the invention for which we pray that a patent may be granted to us, and the method by which it is to be performed, to be particularly described in and by the following statement:- This invention relates to components of solid ionic conducting material.
Solid ionic conductors find application in a number of devices, for example thermoelectric generators and electrical storage devices. A typical example is a battery cell in which the solid ionic conducting material separates a molten alkali metal forming the anode from a cathodic reactant comprising a liquid, for example molten sulphur and polysulphides, which is electro-chemically reactive with the alkali metal of the anode.
The solid electrolyte comprises a material permeable to the cations, that is to say the alkali metal but prevents the direct mixing of the anodic and cathodic materials. Another example of such a device employing a solid electrolyte is a sodium sulphur cell in which liquid sodium is separated from sodium/ sodium polysulphides by a solid electrolyte material typically beta-alumina.
One of the problems in such apparatus is that the solid electrolyte material has to be secured in position and typically has to be sealed to a closure member. For example the solid electrolyte material might be in the form of a tube separating the anodic reactant from the cathodic reactant, one being outside the tube and the other inside. The tube may be closed at one end but the other end has to be sealed so as to hold the reactant within the tube. There is a problem in sealing closures to solid ionic conducting material, referred to hereinafter as the electrolyte material, because of the electro-chemical reactions which may take place at the interface between the metal and the electro lyte due to the diffusion of ions through the electrolyte into the interface region. For example if beta-alumina is used as a conductor of sodium ions, reactions may take place at the interface between the electrolyte and the metal closure due to the- presence of the sodium ions. For this reason, in a sodiurn sulphur cell, although it would be convenient to make a direct metallic seal to the solid beta-alumina electrolyte material, it is not possible in practice to obtain a satisfactory seal. To overcome this difficulty, various techniques have been employed in which a component of alpha-alumina is interposed between the beta-alumina and the seal, the alpha-alumina being secured to the - the:-beta- alumina by a glass seal and the metal then being secured onto the alpha-aluminaj for example by diffusion bonding or brazing.
Seal arrangements of this kind for sodium sulphur cells are disclosed for example in Specification N9. 1502693 and in co-pending Patent Application No. 20959/76 (Serial No. 1574804).
It is an object of the present invention to provide an improved solid ionic conducting component for jointing to metal or other electronic conductors and a method of manufacture of such components.
According to one aspect of the present invention, there is provided a component of solid ionic conductive material in which, over part of the component, the bulk properties of the ionic conductor are modified by the substitution of ions which remain firmly bonded in the material for the ions for which the material is conductive, whereby, the bulk properties in the modified part of the component differ from the bulk properties in the unmodified part of the component. In the case of beta-alumina, in the required region, sodium ions may be replaced by ions of a divalent material for example barium or calcium.
Where the bulk properties of the material forming the component are modified in this way, the material will no longer act as an ionic conductor or will, at least, haye the ionic conductivity reduced, and hence a metal may be jointed onto the solid ionic conduct ing component in the region where the bulk properties are so modified without the corrosion problems arising due to ionic conductivity.-Metal may be sealed to such a solid ionic conductive component in these regions using the known techniques for securing metal onto alpha-alumina, such as for example the techniques described in the aforementioned specifications.
A further advantage of this technique arises in constructions where a beta-alumina electrolyte element is used in an assembly with glass in contact with the electrolyte element, e.g. a glass coating over part of the surface of the electrolyte or a glass seal between the electrolyte element and another part of the assembly. When glasses are used with beta-alumina in coatings or as part of an assembly, there is evidence to suggest that a diffusion of sodium from the beta-alumina into the glass may have a detrimental effect on the glass properties which could cause a Subsequent failure. If the beta-alumina in the appropriate area has previously been diffused with barium or calcium, this sodium diffusion would be reduced.
The invention furthermore includes within its scope a component of beta-alumina wherein, over a limited region of the com ponent, the sodium ions are replaced by barium or - calcium ions. The component typically is a tube which is open at one end, the material of the tube, at its open end, having the bulk properties modified as described above.
The modification of the bulk properties of a ceramic solid ionic conductor may be effected either before or after firing. For example the green shape before firing may be formed of powdered material comprising beta-alumina or a mixture which when heated will produce beta-alumina in which the composition of the powder is modified in the required region where the ionic conductivity is to be reduced. This may be effected either by suitable choice of materials in making up the green shape or by doping of the powder.
If the modification to the bulk properties is to be effected after firing, this may be done by immersing the appropriate region of the solid ionic conducting component in a suitable chemical to cause the diffusion, into the skin of the component, of ions which will give substantially reduced ionic conductivity.
In the case of beta-alumina, for example, the electrolyte,-after firing may be soaked in a molten salt, for example a barium or calcium salt.
Thus the invention includes within its scope a method of making a solid electrolyte com -ponent of beta-alumina ceramic wherein the ceramic material, after firing, is partly dipped into a molten barium or calcium salt so that barium or calcium ions diffuse into the surface of the electrolyte over -a limited region thereof. The manufacture of the component electrolyte material which is to be dipped into the molten salt may be effected in the known way, for example tubes may be formed using a zone sintering technique as described in Patent Specifications Nos. 1297373, 1375167 and 1458221.
In order further to reduce the conductivity of the component in the region where the bulk properties are modified, a coating of an insulating material such as alpha-alumina or glass may be put over this region. Such a coating may be a very thin coating forming only a skin on the surface, for example less than 1 mm thick. A thin coating of this nature does not introduce any weakness into the structure and is, in this respect, quite unlike the much thicker glass required for jointing an alpha-alumina component onto a beta-alumina component.
The following is a description of an example of the manufacture of an article of betaalumina with the bulk properties of part of the article modified by the introduction of barium or calcium.
A tube of beta-alumina ceramic material open at one end and closed at the other was formed using a zone sintering technique. In this technique a green shape is formed of finely powdered beta-alumina or finely powdered precursors thereof and is then fired by passing through a tubular furnace.
Reference may be made to Patent Specifications Nos. 1297373, 1375167 and 1458221 for further description of such a technique.
After the shape has been sintered, the open end of the tube was put for 2 hours in molten calcium chloride in a crucible, the molten salt being at a temperature of about 800"C.
In this particular example, the tube was about 30 cm long and a length of about 3 cm was immersed in the molten salt.
It was found that, by this process sodium in the end portion of the tube had been replaced by calcium and the external surface was no longer conductive.
Calcium chloride has a melting point of about 782"C. Other salts which may be used are calcium tetraborate (M.P. 986"C), calcium bromide (M.P. 730 C), calcium nitrate (M.P. 561"C) and calcium iodide (M.P.
784"C). A similar technique can be employed using barium salts, e.g. barium bromide (M.P. 850"C), barium chloride (M.P. 963"C), barium iodide (M.P. 740"C) or barium nitrate (M.P. 592"C).
Instead of using a calcium or barium salt, molten calcium or barium may be employed.
In this technique, where the sintered ceramic is immersed in molten calcium or barium or a salt thereof, the calcium or barium diffuses into the body of the electrolyte. The time required for diffusion of barium or calcium into an already sintered article will depend on a number of factors but typically is of the order of two hours at a temperature between 600"C and 1100 C.
The actual temperatures employed must be high enough to melt the material in the crucible.
Instead of modifying the properties of the beta-alumina after it has been sintered, the required modified properties for part of the electrolyte tube can be obtained by sintering a powdered material compressed in a mould in which, for example some beta-alumina powder is mixed with the required percentage of barium or calcium or of barium oxide or calcium oxide and introduced into one end of the mould. The remainder of the mould is filled with powdered beta-alumina.
If desired, a number of mixes with progressively less additive may be put in the mould after the first batch. The first batch may be used to form that part of the shape constituting the open end of the electrolyte tube. This would result in a graded electrolyte resistivity which would increase along the length of the tube as the seal area at the open end of the tube was approached and thus obviate any discontinuities in material properties. The powder material may be compressed in the mould and sintered using a zone sintering technique as described in the aforementioned Patent Specifications Nos. 1297373, 1375167 and 1458221 to which reference may be made for a fuller description of the sintering of beta-alumina tubes.
WHAT WE CLAIM IS 1. A component of solid ionic conductive material in which, over part of the component, the bulk properties of the ionic conductor are modified by the substitution of ions which remain firmly bonded in the material for the ions for which the material is conductive whereby the bulk properties in the modified part of the component differ from the bulk properties in the un-modified part of the component.
2. A component of beta-alumina in which the bulk properties of the material are modified by the substitution of ions of a divalent material for sodium ions over part of the component.
3. A component as claimed in claim 2 wherein the divalent material is barium or calcium.
4. A component as claimed in either claim 2 or claim 3 wherein the material, in the part of the component where the bulk properties are modified, is non-conductive for sodium ions.
5. The combination of a component as claimed in claim 4 with a metal element jointed onto the solid ionic conducting component in the region where the bulk properties are modified.
6. A component as claimed in any of claims 2 to 4 and having a glass coating over part of the surface of the component where the bulk properties have been modified.
7. A component of beta-alumina wherein, over a limited region of the component, the sodium ions are replaced by barium- or calcium ions.
8. A component as claimed in claim -7 and comprising a tube which is open at-one end, the material of the tube, at its open end, having the bulk properties modified.
9. A component as claimed in either claim 7 or claim 8 wherein said limited region is a surface region.
10. A method of making a component of beta-alumina ceramic solid ionic conductive material in which powdered material comprising beta-alumina or a mixture which when heated will produce beta-alumina is formed into a green shape and then fired characterised in that the composition of the powder is modified in a part of the component in order to reduce the ionic conductivity in that part either by the inclusion of barium or calcium or barium oxide or calcium oxide in making up the material for part of the green shape or by doping the green shape with a barium or calcium-containing material.
11. A method of making a component of ceramic solid ionic conductive material by firing of a green shape in which, after firing, the bulk properties of the sintered shape are modified in a predetermined region of the shape by immersing that region of the solid ionic conducting component in a liquid bath to cause the diffusion, into the skin of the component, of ions which will give substantially reduced ionic conductivity.
12. A method of making a solid electrolyte component of beta-alumina ceramic wherein the ceramic material, after firing, is partly dipped into a molten barium or calcium salt so that barium or calcium ions diffuse into the surface of the electrolyte over a limited region thereof.
13. A method as claimed in any of claims 10 to 12 wherein, in order further to reduce the conductivity of the component in the region where the bulk properties are modified, a coating of an insulating material is put over this region.
14. A method as claimed in claim 13 wherein the solid ionic conductive material is beta-alumina and wherein the insulating material is alpha-alumina or glass.
15. A beta-alumina ceramic tube having the bulk conductivity properties of the material modified near one end of the tube by the presence of barium and/or calcium ions in the ceramic substantially as hereinbefore described.
**WARNING** end of DESC field may overlap start of CLMS **.

Claims (15)

**WARNING** start of CLMS field may overlap end of DESC **. article will depend on a number of factors but typically is of the order of two hours at a temperature between 600"C and 1100 C. The actual temperatures employed must be high enough to melt the material in the crucible. Instead of modifying the properties of the beta-alumina after it has been sintered, the required modified properties for part of the electrolyte tube can be obtained by sintering a powdered material compressed in a mould in which, for example some beta-alumina powder is mixed with the required percentage of barium or calcium or of barium oxide or calcium oxide and introduced into one end of the mould. The remainder of the mould is filled with powdered beta-alumina. If desired, a number of mixes with progressively less additive may be put in the mould after the first batch. The first batch may be used to form that part of the shape constituting the open end of the electrolyte tube. This would result in a graded electrolyte resistivity which would increase along the length of the tube as the seal area at the open end of the tube was approached and thus obviate any discontinuities in material properties. The powder material may be compressed in the mould and sintered using a zone sintering technique as described in the aforementioned Patent Specifications Nos. 1297373, 1375167 and 1458221 to which reference may be made for a fuller description of the sintering of beta-alumina tubes. WHAT WE CLAIM IS
1. A component of solid ionic conductive material in which, over part of the component, the bulk properties of the ionic conductor are modified by the substitution of ions which remain firmly bonded in the material for the ions for which the material is conductive whereby the bulk properties in the modified part of the component differ from the bulk properties in the un-modified part of the component.
2. A component of beta-alumina in which the bulk properties of the material are modified by the substitution of ions of a divalent material for sodium ions over part of the component.
3. A component as claimed in claim 2 wherein the divalent material is barium or calcium.
4. A component as claimed in either claim 2 or claim 3 wherein the material, in the part of the component where the bulk properties are modified, is non-conductive for sodium ions.
5. The combination of a component as claimed in claim 4 with a metal element jointed onto the solid ionic conducting component in the region where the bulk properties are modified.
6. A component as claimed in any of claims 2 to 4 and having a glass coating over part of the surface of the component where the bulk properties have been modified.
7. A component of beta-alumina wherein, over a limited region of the component, the sodium ions are replaced by barium- or calcium ions.
8. A component as claimed in claim -7 and comprising a tube which is open at-one end, the material of the tube, at its open end, having the bulk properties modified.
9. A component as claimed in either claim 7 or claim 8 wherein said limited region is a surface region.
10. A method of making a component of beta-alumina ceramic solid ionic conductive material in which powdered material comprising beta-alumina or a mixture which when heated will produce beta-alumina is formed into a green shape and then fired characterised in that the composition of the powder is modified in a part of the component in order to reduce the ionic conductivity in that part either by the inclusion of barium or calcium or barium oxide or calcium oxide in making up the material for part of the green shape or by doping the green shape with a barium or calcium-containing material.
11. A method of making a component of ceramic solid ionic conductive material by firing of a green shape in which, after firing, the bulk properties of the sintered shape are modified in a predetermined region of the shape by immersing that region of the solid ionic conducting component in a liquid bath to cause the diffusion, into the skin of the component, of ions which will give substantially reduced ionic conductivity.
12. A method of making a solid electrolyte component of beta-alumina ceramic wherein the ceramic material, after firing, is partly dipped into a molten barium or calcium salt so that barium or calcium ions diffuse into the surface of the electrolyte over a limited region thereof.
13. A method as claimed in any of claims 10 to 12 wherein, in order further to reduce the conductivity of the component in the region where the bulk properties are modified, a coating of an insulating material is put over this region.
14. A method as claimed in claim 13 wherein the solid ionic conductive material is beta-alumina and wherein the insulating material is alpha-alumina or glass.
15. A beta-alumina ceramic tube having the bulk conductivity properties of the material modified near one end of the tube by the presence of barium and/or calcium ions in the ceramic substantially as hereinbefore described.
GB1002/77A 1978-04-11 1978-04-11 Components employing solid ionic conducting material Expired GB1575231A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1991003080A1 (en) * 1989-08-16 1991-03-07 Licentia Patent-Verwaltungs-Gmbh High-energy secondary battery
DE4035693A1 (en) * 1989-11-09 1991-05-16 Lilliwyte Sa METHOD FOR PRODUCING ANALOGS OF (BETA) "ALUMINUM OXIDE
US5458868A (en) * 1989-11-09 1995-10-17 Lilliwyte Societe Anonyme Method of making analogues of β-alumina

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1991003080A1 (en) * 1989-08-16 1991-03-07 Licentia Patent-Verwaltungs-Gmbh High-energy secondary battery
DE4035693A1 (en) * 1989-11-09 1991-05-16 Lilliwyte Sa METHOD FOR PRODUCING ANALOGS OF (BETA) "ALUMINUM OXIDE
US5458868A (en) * 1989-11-09 1995-10-17 Lilliwyte Societe Anonyme Method of making analogues of β-alumina

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PCNP Patent ceased through non-payment of renewal fee

Effective date: 19940411