FR2563512A1 - PROCESS FOR THE MANUFACTURE OF M-LIA102 FRITTABLE POWDER AND USE THEREOF - Google Patents
PROCESS FOR THE MANUFACTURE OF M-LIA102 FRITTABLE POWDER AND USE THEREOF Download PDFInfo
- Publication number
- FR2563512A1 FR2563512A1 FR8505317A FR8505317A FR2563512A1 FR 2563512 A1 FR2563512 A1 FR 2563512A1 FR 8505317 A FR8505317 A FR 8505317A FR 8505317 A FR8505317 A FR 8505317A FR 2563512 A1 FR2563512 A1 FR 2563512A1
- Authority
- FR
- France
- Prior art keywords
- powder
- lialo
- temperature
- lia102
- manufacture
- Prior art date
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Classifications
-
- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21B—FUSION REACTORS
- G21B1/00—Thermonuclear fusion reactors
- G21B1/11—Details
- G21B1/13—First wall; Blanket; Divertor
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B4/00—Hydrogen isotopes; Inorganic compounds thereof prepared by isotope exchange, e.g. NH3 + D2 → NH2D + HD
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/04—Preparation of alkali metal aluminates; Aluminium oxide or hydroxide therefrom
- C01F7/043—Lithium aluminates
-
- 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
- C04B35/44—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 aluminates
-
- 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
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/10—Nuclear fusion reactors
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Materials Engineering (AREA)
- Ceramic Engineering (AREA)
- Inorganic Chemistry (AREA)
- Geology (AREA)
- Plasma & Fusion (AREA)
- General Engineering & Computer Science (AREA)
- High Energy & Nuclear Physics (AREA)
- Manufacturing & Machinery (AREA)
- Life Sciences & Earth Sciences (AREA)
- Structural Engineering (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Compositions Of Oxide Ceramics (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
A.PROCEDE POUR LA FABRICATION DE -LIALO EN POUDRE FRITTABLE. B.LE PROCEDE, QUI SE DEROULE DANS UNE SOLUTION AQUEUSE D'HYDROXYDE DE LITHIUM, SE CARACTERISE EN CE QUE LA SUSPENSION QUI SE FORME PAR LA PRECIPITATION PRODUITE PENDANT LA REACTION EN SOLUTION, EST SECHEE PAR ATOMISATION, SANS TRAITEMENT INTERMEDIAIRE, DIRECTEMENT, AU MOYEN D'AIR, A UNE TEMPERATURE QUI SE SITUE ENTRE 200 ET 450C ET, AUSSITOT APRES, LA MATIERE SECHE EST CALCINEE A UNE TEMPERATURE ENTRE 850 ET 1100C, SE TRANSFORMANT AINSI EN -LIALO. C.LA POUDRE FRITTABLE DE LIALO PUR EST UTILISEE COMME MATIERE FERTILE DANS DES REACTEURS A FUSION, POUR LA PRODUCTION DE TRITIUM.A.PROCESS FOR THE MANUFACTURE OF -LIALO IN SINKABLE POWDER. B. THE PROCESS, WHICH TAKES PLACE IN AN AQUEOUS SOLUTION OF LITHIUM HYDROXIDE, IS CHARACTERIZED IN THAT THE SUSPENSION WHICH IS FORMED BY THE PRECIPITATION PRODUCED DURING THE REACTION IN SOLUTION, IS DRIED BY ATOMIZATION, WITHOUT INTERMEDIATE TREATMENT, DIRECTLY, AVERAGE AIR, AT A TEMPERATURE BETWEEN 200 AND 450C AND, SOON AFTER, THE DRY MATTER IS CALCINED AT A TEMPERATURE BETWEEN 850 AND 1100C, THUS TRANSFORMING INTO -LIALO. C. LIALO PUR SINKABLE POWDER IS USED AS FERTILE IN FUSION REACTORS, FOR THE PRODUCTION OF TRITIUM.
Description
"Procédé pour la fabrication rie poudre frittable de -LiAlO2 et sonProcess for making sinterable powder of LiAlO 2 and its
utilisation" L'invention concerne un procédé pour la fabrication de poudre frittable de 4-LiA102 avec une pureté de phase d'un ordre de grandeur de 99 %, dans lequel on dissout de l'aluminium métal dans une solution aqueuse The invention relates to a process for producing sinterable powder of 4-LiAlO 2 with a phase purity by an order of magnitude of 99%, in which aluminum metal is dissolved in an aqueous solution.
d'hydroxyde de lithium.of lithium hydroxide.
Les matières céramiques oxydées contenant du lithium, par exemple l'aluminate de lithium, ont déjà été proposées comme matières fertiles pour des réacteurs à fusion pour l'obtention du tritium. Pour fabriquer LiA10i, on a, la plupart du temps, finement broyé et mélangé des poudres solides de Li2CO3 et d'A1203, et les a soumises soit par voie sèche, par exemple sous la forme de boulettes comprimées, soit sous la forme d'une suspension avec de l'eau, à un traitement thermique qui comprenait un séchage et une calcination à une temperature élevée. Le broyage des substances de départ était poursuivi pendant plusieurs heures. Ensuite le produit broyé était comprimé et homogénéisé par diffusion pendant un à deux jours pour la calcination. I1 faJlait ensuite broyer encore une fois le produit afin de pouvoir obtenir la poudre frittable dés!.rée. La mouture et le broyage, non seulement des substances de départ, maïs aussi du produit de la réaction Oxidized ceramic materials containing lithium, for example lithium aluminate, have already been proposed as fertile materials for fusion reactors for obtaining tritium. To manufacture LiA10i, solid powders of Li 2 CO 3 and Al 2 O 3 were finely ground and mixed, and subjected either by dry process, for example in the form of compressed pellets, or in the form of a suspension with water, a heat treatment which included drying and calcining at a high temperature. Grinding of the starting materials was continued for several hours. Then the ground product was compressed and homogenized by diffusion for one to two days for calcination. He then crushed the product again in order to obtain the sinterable powder which had been removed. Grinding and grinding, not only of the starting substances, but also of the product of the reaction
calciné, peut être une source d'introduction d'impuretés. calcined, can be a source of introduction of impurities.
D'autre part, dans ces réactions entre matières solides, on ne peut compter obtenir en général que des proportions On the other hand, in these reactions between solids, one can not expect to obtain in general only proportions
de 90 à 95 % de la phase recherchée, dans le produit final. from 90 to 95% of the desired phase, in the final product.
Enfin la conductivité thermique du LiAl02 produit, néces- Finally, the thermal conductivity of LiAlO 2 produced, necessary
saire pour l'obtention du tritium, est défavorablement for obtaining tritium, is unfavorably
affectée par la présence d'autres phases. affected by the presence of other phases.
Il a été considéré, en conséquence, comme souhaitable de réaliser un procédé simple pour la fabrication It has therefore been considered desirable to carry out a simple process for manufacturing
de4"-LiA102, avec lequel on puisse éviter la présence d'impu- de4 "-LiA102, with which the presence of impurities can be avoided.
retés dans le produit final ainsi que diminuer le temps important (environ 3 à 4 jours) que demande le procédé appartenant à l'état actuel de la technique. Pour supprimer les étapes de broyage et de diffusion pour calcination, il a été proposé de faire se dérouler la plus grande partie possible des opérations en solution aqueuse. Il est connu que l'on peut dissoudre l'aluminium avec des solutions aqueuses de LIOH (Gmelin's Han'buch der Anorganischen Chemie, System Nr. 35, Aluminium, Partie A (1934, Réimpression 1953), page 408, Verlag Chemie GmbH, Weinheim). Il y est rapporté qu'après que l'on a porté à l'ébullition une telle solution, il doit se déposer un aluminate difficilement soluble répondant à la formule LiH(102)2. 5H20. On ne retained in the final product as well as reducing the important time (about 3 to 4 days) that the process belonging to the current state of the art requires. To eliminate the grinding and diffusion stages for calcination, it has been proposed to carry out as much of the operations as possible in aqueous solution. It is known that aluminum can be dissolved with aqueous solutions of LIOH (Gmelin's Hanbuch der Anorganischen Chemie, System No. 35, Aluminum, Part A (1934, Reprint 1953), page 408, Verlag Chemie GmbH, Weinheim). It is reported that after such a solution has been boiled, a poorly soluble aluminate having the formula LiH (102) 2 must be deposited. 5:20. We do not
parle pas dans ce document de la fabrication de y-LiAl02. not speak in this document of the manufacture of y-LiAl02.
L'invention a pour objet de réaliser un procédé simple et amélioré pour la fabrication de4-LiA102, dans lequel la plus grande partie possible des opérations se passe dans une solution aqueuse et dans lequel on obtient, en relativement peu de temps, une poudre, ayant une bonne aptitude au frittage, de l'aluminate de lithium voulu, en It is an object of the invention to provide a simple and improved method for the manufacture of 4-LiAlO 2, in which the largest possible part of the process is carried out in an aqueous solution and in which a powder is obtained in a relatively short time, having a good sinterability, of the desired lithium aluminate,
phase pratiquement pure.virtually pure phase.
A cet effet, l'invention propose un procédé o: a) la suspension qui se forme par la précipitation produite pendant la réaction en solution est séchée par atomisation, sans traitement intermédiaire, directement, au moyen d'air, une température qui se situe entre 200 et 450 C, et b) aussitôt après la matière sèche est calcinée à une température entre 850 et 1100 C se transformant ainsi en For this purpose, the invention proposes a process where: a) the suspension which is formed by the precipitation produced during the reaction in solution is spray-dried, without intermediate treatment, directly, by means of air, a temperature which is between 200 and 450 ° C, and b) immediately after the dry matter is calcined at a temperature between 850 and 1100 C thus becoming
L -LiA102.L-LiA102.
La dissolution de l'aluminium métal dans la solution de LiOH s'opère avantageusement sous agitation constante. I1 n'est pas absolument nécessaire de chauffer la solution, toutefois le précipité de l'hydroxoaluminate de lithium obtenu suivant l'équation 2LiOH + 2A1 t aq = Li [A12(OH)7]. nH20 + LiOH + aq The dissolution of the aluminum metal in the LiOH solution is advantageously carried out with constant stirring. It is not absolutely necessary to heat the solution, however the precipitate of the lithium hydroxoaluminate obtained according to the equation 2LiOH + 2A1 t aq = Li [A12 (OH) 7]. nH20 + LiOH + aq
ne se présentera pas en grains trop grossiers si la solu- will not be too coarse grains if the solution
tion a été chauffée préalablement à environ 40 à 50 C. Si l'étape d'atomisation est effectuée à une température de l'ordre de 350 à 400 C, et l'étape de calcination à la température préférée de 900 C, on obtiendra des particules de poudre dont le diamètre extérieur sera situé entre 5 et 15/u. L'utilisation duY-LiA102 fabriqué par le procédé suivant l'invention comme matière fertile dans les réacteurs à fusion, apporte avec elle des avantages inattendus pour l'obtension de tritium, car la poudre obtenue se fritte convenablement et peut être transformée en pièces moulées présentant des densités pouvant aller jusqu'à 95 % de la The atomization step is carried out at a temperature of about 350 to 400 ° C., and the calcination step at the preferred temperature of 900 ° C. will be obtained. powder particles whose outer diameter will be between 5 and 15 / u. The use of Y-LiA102 made by the process according to the invention as a fertile material in fusion reactors, brings with it unexpected advantages for the attainment of tritium, since the powder obtained sintered properly and can be converted into molded parts. with densities of up to 95% of the
densité théorique.theoretical density.
L'invention est expliquée plus en détail The invention is explained in more detail
ci-après d'après un exemple de réalisation. hereinafter according to an exemplary embodiment.
Exemple:Example:
Conformément à l'équation de réaction 2 Li0H + 2 A1 aq --*Li [Al2(0H),]. n H20 + LiOH + aq on a préparé les charges résumées dans le tableau en dissolvant de l'aluminium métal dans une solution aqueuse d'hydroxyde de lithium, sous agitation constante, à la température ambiante: Tableau: charges destinées à l'atomisation d'aluminate de lithium: No. LiOH AlMétal H20 Li [A12(OH)7] nombre (g) (g) (cm) (g/l) de charges According to reaction equation 2 Li0H + 2 Alq - * Li [Al2 (OH)]. The feeds summarized in the table were prepared by dissolving aluminum metal in an aqueous solution of lithium hydroxide, with constant stirring, at room temperature: Table 1: Charges for atomizing d lithium aluminate: No. LiOH AlMetal H20 Li [A12 (OH) 7] number (g) (g) (cm) (g / l) of fillers
1 23,95 26,98 1000 90 11 23.95 26.98 1000 90 1
2 47,90 53,96 1750 100 12 47.90 53.96 1750 100 1
Dans la charge N 2, on a utilisé de la feuille d'aluminium fabriquée industriellement, dans la In the load N 2, industrially manufactured aluminum foil was used in the
charge 1, une bande d'aluminium de grande pureté (Fa.Merck). load 1, a high purity aluminum strip (Fa.Merck).
Le LiOH peut être utilisé aussi bien sous la forme anhydre LiOH can be used both in the anhydrous form
que sous la forme d'hydroxyde contenant son eau de cris- only in the form of hydroxide containing its water of crys-
tallisation (LiOH. H20) pour la préparation de la solution aqueuse. L'atomisation de la suspension qui s'est formée constituée d'heptahydroxoaluminate de lithium très finement dispersé dans la solution d'hydroxyde de lithium s'est opérée dans un ordre de grandeur de la température de 250 à 400 C. Le rendement en poudre atomisée, qui est un mélange stoechiométrique d'hydroxoaluminate de lithium et d'hydroxyde de lithium se monte toujours à plus de 90 %. En raison des manipulations à l'air, des solutions d'hydroxyde de lithium et des suspensions, les poudres contiennent jusqu'à 5 % en poids de constituant carbonate qui sera éliminé pendant (LiOH, H 2 O) for the preparation of the aqueous solution. The atomization of the slurry formed of lithium heptahydroxoaluminate very finely dispersed in the lithium hydroxide solution was carried out in an order of magnitude of the temperature of 250 to 400 C. The powder yield atomized, which is a stoichiometric mixture of lithium hydroxoaluminate and lithium hydroxide always amounts to more than 90%. Due to air handling, lithium hydroxide solutions and suspensions, the powders contain up to 5% by weight of carbonate component which will be removed during
l'opération de calcination.the calcination operation.
Au cours de la calcination de la poudre (deux heures), il se forme, à partir du mélange de poudres stoechiométrique, finement dispersé, le monoaluminate de lithium recherché. Suivant la température de calcination, on observe ici la formation de mélanges de c- - et e-LiAlO2 (à 600OC),d et?-LiA102 (à 800eC) et de Y-LiAlO02 pur (au-dessus de 900 C). Les poudres calcinées à 9000C peuvent être compactéés par pressage et frittage, à environ 1250 C jusqu'à 80 à 85 %, et, à 1450 C, en six heures, jusqu'à à 95 X de la densité théorique. Les échantillons frittés During the calcination of the powder (two hours), the desired lithium monoaluminate is formed from the stoichiometric powder mixture, finely dispersed. Depending on the calcination temperature, the formation of mixtures of c- and e-LiAlO 2 (at 600 ° C), d 3 and Li 3 O 2 (at 800 ° C.) and pure Y-LiAlO 2 O (above 900 ° C.) is observed here. The powders calcined at 9000 ° C can be compacted by pressing and sintering, at about 1250 ° C. to 80-85%, and at 1450 ° C., in six hours, up to 95 × of the theoretical density. Sintered samples
étaient toujours constitués de 4-LiA102 monophasé. always consisted of 4-LiA102 single phase.
Claims (1)
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE3415324A DE3415324C2 (en) | 1984-04-25 | 1984-04-25 | Process for the preparation of sinterable powder from γ-LiAl0? 2? and its use |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| FR2563512A1 true FR2563512A1 (en) | 1985-10-31 |
Family
ID=6234300
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| FR8505317A Pending FR2563512A1 (en) | 1984-04-25 | 1985-04-09 | PROCESS FOR THE MANUFACTURE OF M-LIA102 FRITTABLE POWDER AND USE THEREOF |
Country Status (4)
| Country | Link |
|---|---|
| BE (1) | BE902191A (en) |
| DE (1) | DE3415324C2 (en) |
| FR (1) | FR2563512A1 (en) |
| GB (1) | GB2159805B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0235098A1 (en) * | 1986-02-26 | 1987-09-02 | ENEA-Comitato Nazionale per la Ricerca e per lo Sviluppo dell'Energia Nucleare e delle Energie Alternative | A process for preparing a lithium aluminate powder in gamma phase |
| EP0336322A1 (en) * | 1988-04-01 | 1989-10-11 | Hitachi, Ltd. | Process for producing lithium aluminate powder having large specific surface area |
| FR2687139A1 (en) * | 1992-02-07 | 1993-08-13 | Commissariat Energie Atomique | Process for the preparation of gamma lithium aluminate possessing controlled microstructure and stoichiometry |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3719825A1 (en) * | 1987-06-13 | 1988-12-29 | Kernforschungsz Karlsruhe | METHOD FOR PRODUCING CERAMIC POWDERS AND DEVICE FOR IMPLEMENTING THE SAME |
| CN116444261A (en) * | 2023-03-23 | 2023-07-18 | 宜春国轩电池有限公司 | Lithium metaaluminate material and preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2711420A1 (en) * | 1977-03-16 | 1978-09-21 | Degussa | PROCESS FOR THE PRODUCTION OF BETA LITHIUM ALUMINATE |
-
1984
- 1984-04-25 DE DE3415324A patent/DE3415324C2/en not_active Expired
-
1985
- 1985-04-09 FR FR8505317A patent/FR2563512A1/en active Pending
- 1985-04-12 GB GB08509431A patent/GB2159805B/en not_active Expired
- 1985-04-15 BE BE1/11235A patent/BE902191A/en not_active IP Right Cessation
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2711420A1 (en) * | 1977-03-16 | 1978-09-21 | Degussa | PROCESS FOR THE PRODUCTION OF BETA LITHIUM ALUMINATE |
Non-Patent Citations (1)
| Title |
|---|
| CHEMICAL ABSTRACTS, vol. 103, 1985, page 402, résumé no. 28662m, Columbus, Ohio, US; D. VOLLATH et al.: "Improved methods for fabrication of lithium metaaluminate (LiAlO2) and lithium metasilicate (Li2SiO3) pellets and spheres as breeder materials in fusion reactors", & COMM. EUR. COMMUNITIES ÄREPÜ EUR 1984, EUR 9183, Fusion Technol., vol. 2, 967-72 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0235098A1 (en) * | 1986-02-26 | 1987-09-02 | ENEA-Comitato Nazionale per la Ricerca e per lo Sviluppo dell'Energia Nucleare e delle Energie Alternative | A process for preparing a lithium aluminate powder in gamma phase |
| EP0336322A1 (en) * | 1988-04-01 | 1989-10-11 | Hitachi, Ltd. | Process for producing lithium aluminate powder having large specific surface area |
| FR2687139A1 (en) * | 1992-02-07 | 1993-08-13 | Commissariat Energie Atomique | Process for the preparation of gamma lithium aluminate possessing controlled microstructure and stoichiometry |
Also Published As
| Publication number | Publication date |
|---|---|
| BE902191A (en) | 1985-07-31 |
| DE3415324C2 (en) | 1986-11-06 |
| DE3415324A1 (en) | 1985-11-07 |
| GB2159805A (en) | 1985-12-11 |
| GB2159805B (en) | 1988-02-24 |
| GB8509431D0 (en) | 1985-06-19 |
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