FR2498587A1 - Magnetic iron oxide powder mfr. - by wet grinding non magnetic iron oxide with steel balls in steel mill - Google Patents
Magnetic iron oxide powder mfr. - by wet grinding non magnetic iron oxide with steel balls in steel mill Download PDFInfo
- Publication number
- FR2498587A1 FR2498587A1 FR8026991A FR8026991A FR2498587A1 FR 2498587 A1 FR2498587 A1 FR 2498587A1 FR 8026991 A FR8026991 A FR 8026991A FR 8026991 A FR8026991 A FR 8026991A FR 2498587 A1 FR2498587 A1 FR 2498587A1
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- Prior art keywords
- sep
- oxide
- steel
- iron oxide
- fe2o3
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/08—Ferroso-ferric oxide (Fe3O4)
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/06—Ferric oxide (Fe2O3)
-
- G—PHYSICS
- G11—INFORMATION STORAGE
- G11B—INFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
- G11B5/00—Recording by magnetisation or demagnetisation of a record carrier; Reproducing by magnetic means; Record carriers therefor
- G11B5/62—Record carriers characterised by the selection of the material
- G11B5/68—Record carriers characterised by the selection of the material comprising one or more layers of magnetisable material homogeneously mixed with a bonding agent
- G11B5/70—Record carriers characterised by the selection of the material comprising one or more layers of magnetisable material homogeneously mixed with a bonding agent on a base layer
- G11B5/706—Record carriers characterised by the selection of the material comprising one or more layers of magnetisable material homogeneously mixed with a bonding agent on a base layer characterised by the composition of the magnetic material
- G11B5/70626—Record carriers characterised by the selection of the material comprising one or more layers of magnetisable material homogeneously mixed with a bonding agent on a base layer characterised by the composition of the magnetic material containing non-metallic substances
- G11B5/70642—Record carriers characterised by the selection of the material comprising one or more layers of magnetisable material homogeneously mixed with a bonding agent on a base layer characterised by the composition of the magnetic material containing non-metallic substances iron oxides
- G11B5/70652—Record carriers characterised by the selection of the material comprising one or more layers of magnetisable material homogeneously mixed with a bonding agent on a base layer characterised by the composition of the magnetic material containing non-metallic substances iron oxides gamma - Fe2 O3
- G11B5/70663—Preparation processes specially adapted therefor, e.g. using stabilising agents
-
- G—PHYSICS
- G11—INFORMATION STORAGE
- G11B—INFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
- G11B5/00—Recording by magnetisation or demagnetisation of a record carrier; Reproducing by magnetic means; Record carriers therefor
- G11B5/62—Record carriers characterised by the selection of the material
- G11B5/68—Record carriers characterised by the selection of the material comprising one or more layers of magnetisable material homogeneously mixed with a bonding agent
- G11B5/70—Record carriers characterised by the selection of the material comprising one or more layers of magnetisable material homogeneously mixed with a bonding agent on a base layer
- G11B5/706—Record carriers characterised by the selection of the material comprising one or more layers of magnetisable material homogeneously mixed with a bonding agent on a base layer characterised by the composition of the magnetic material
- G11B5/70626—Record carriers characterised by the selection of the material comprising one or more layers of magnetisable material homogeneously mixed with a bonding agent on a base layer characterised by the composition of the magnetic material containing non-metallic substances
- G11B5/70642—Record carriers characterised by the selection of the material comprising one or more layers of magnetisable material homogeneously mixed with a bonding agent on a base layer characterised by the composition of the magnetic material containing non-metallic substances iron oxides
- G11B5/70678—Ferrites
- G11B5/70684—Ferro-ferrioxydes
- G11B5/70689—Magnetite
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/44—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of magnetic liquids, e.g. ferrofluids
- H01F1/445—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of magnetic liquids, e.g. ferrofluids the magnetic component being a compound, e.g. Fe3O4
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
- C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/42—Magnetic properties
Abstract
Description
PROCEDE DE PREPARATION DE COMPOSES MAGNETIQUES
TYPE OXYDES DE FER, PAR MELPN0-CHIMIE
L'invention se rapporte à un procédé de préparation des composés magnétiques type oxyde de fer.PROCESS FOR THE PREPARATION OF MAGNETIC COMPOUNDS
TYPE OXIDES OF IRON, BY MELPN0-CHEMISTRY
The invention relates to a process for the preparation of magnetic compounds such as iron oxide.
On sait que les oxydes de fer magnétiques sont essentiellement constitués par l'oxyde magnétite Fe3O4 et la maghémite y-Fe203 ; sous forme de poudre fine, l'oxyde magnétite trouve ses principales applications comme pigment, ou élément actif des fluides magnétiques ou de transport d'encre dans les systèmes de reproduction dits "à sec". La maghémite constitue l'élément actif des enregistrements sur bandes magnétiques.It is known that the magnetic iron oxides consist essentially of magnetite oxide Fe3O4 and maghemite y-Fe2O3; in the form of fine powder, the magnetite oxide finds its main applications as a pigment, or active element of magnetic fluids or ink transport in so-called "dry" reproduction systems. Maghémite is the active element of tape recordings.
L'oxyde magnétite est généralement préparé par réduction ménagée des oxydes Fe203 par l'hydrogène ou par oxydation ménagée à l'air de poudres de fer.Magnetite oxide is generally prepared by mild reduction of Fe 2 O 3 oxides by hydrogen or by air oxidation of iron powders.
La maghémite est généralement préparée en trois étapes à partir d'hydrate d'oxyde aciculaire aFe203.H20, déshydratation, réduction sous hydrogène vers 4000 C, puis oxydation contrôlée à 2500 C.The maghemite is generally prepared in three steps from acicular oxide hydrate aFe203.H20, dehydration, reduction in hydrogen at 4000 C, then controlled oxidation at 2500 C.
L'invention est relative à un procédé de préparation des oxydes magnétiques Fe304 et (/ou) y-Fe203 par broyage humide, en milieu aqueux et confiné, en présence de corps broyants en acier, d'oxyde de fer Fe203 de diverses origines. L'oxyde Fe203 utilisé peut-être soit un oxyde naturel, soit un oxyde provenant de la récupération des bains de décapage sidérurgiques (oxyde "ex-pickling").The invention relates to a process for the preparation of Fe304 and / or y-Fe2O3 magnetic oxides by wet milling, in an aqueous medium and confined, in the presence of steel grinding bodies, of Fe203 iron oxide of various origins. The Fe 2 O 3 oxide used may be either a natural oxide or an oxide from the recovery of steel pickling baths ("ex-pickling" oxide).
Les xemples suivants permettent d'illustrer la méthode utilisée
Exemple 1 : dans un broyeur formé d'une cuve cylindrique en acier de contenance 6 litres, sont introduits 14 kg de billes d'acier de diamètre environ 5 mm, 1,7 litre d'eau et 1 kg d'oxyde de fer a-Fe203. The following examples illustrate the method used
Example 1: in a mill formed of a cylindrical steel tank with a capacity of 6 liters, 14 kg of steel balls with a diameter of about 5 mm, 1.7 liters of water and 1 kg of iron oxide are introduced. -Fe203.
Le broyeur est fermé de façon la plus étanche possible, puis mis en rotation pour une durée de 48 heures.The mill is closed as tightly as possible, then rotated for a period of 48 hours.
A la fin de l'opération, la boue est séparée des billes par tamisage puis séchée à l'air ou à l'aide d'une rampe infrarouge, à une température ne dépassant pas 1500 C.At the end of the operation, the sludge is separated from the balls by sieving and then dried in air or with the aid of an infrared ramp, at a temperature not exceeding 1500 C.
Les caractéristiques du produit obtenu sont données dans le tableau I. A côté de l'effet mécanique attendu de réduction de taille des particules (augmentation de la finesse en perm.éabilité Fisher et de la surface spécifique, mesurée à l'appareil Strohleim), on constate en particulier une augmentation très notable du mo mellt magnétia,le massique (x 30 environ), sauf pour l'oxyde synthétique, ainsi qu'une augmentation de la teneur en
Fe2+.The characteristics of the product obtained are given in Table I. In addition to the expected mechanical effect of particle size reduction (increase of the Fisher permeability fineness and of the specific surface area, measured with the Strohleim apparatus), in particular, there is a very notable increase in the amount of magnesium, the mass (about 30), except for the synthetic oxide, as well as an increase in the content of
Fe 2+.
Les quantités relatives d'oxydes après l'application de ce broyage ont été estimées par radiocristallographie et par analyse thermomagnétique, à : 30 % d'oxyde a-Fe2O3, 60 % d'oxyde Fe3O4 et 10 % d'oxyde y-Fe203 ou d'hydroxydes de fer.The relative amounts of oxides after the application of this grinding were estimated by radiocrystallography and by thermomagnetic analysis, at 30% α-Fe 2 O 3 oxide, 60% Fe 3 O 4 oxide and 10% γ-Fe 2 O 3 oxide. of iron hydroxides.
Tous les pourcentages sont exprimés en poids Z. All percentages are by weight Z.
Exemple 2 : influence des conditions opératoires sur l'obtention des oxydes magnétiques est précisée dans l'exemple ci-après. Ces essais ont été effectués avec l'oxyde ex-pickling (repère 2 de l'exemple 1) dans les conditions reportées au tableau Il. Y figurent également les résultats obtenus.Example 2: Influence of the operating conditions on the obtaining of the magnetic oxides is specified in the example below. These tests were carried out with the ex-pickling oxide (reference 2 of Example 1) under the conditions reported in Table II. There are also the results obtained.
Ces essais montrent que la transformation de a-Fe203 en oxydes magnétiques ne se produit qu'en milieu aqueux confiné, en présence d'acier. Les caractéristiques m3gnétiques du produit final dependent également du temps de broyage, et des proportions relatives du poids des corps broyants, de l'oxyde, de la teneur en eau et du volume du broyeur.These tests show that the transformation of α-Fe 2 O 3 into magnetic oxides takes place only in a confined aqueous medium, in the presence of steel. The mechanical characteristics of the final product also depend on the grinding time, and the relative proportions of the weight of the grinding media, the oxide, the water content and the volume of the mill.
Le procédé selon l'invention peut être appliqué pour la production d'oxydes de fer magnétiques utilisables par exemple en reprograpbîe, ou comme constituants des fluides magnétiques. On peut également l'appliquer à la séparation magnétique des minerais de fer de leur gangue. The process according to the invention can be applied for the production of magnetic iron oxides usable for example in reprogramming, or as constituents of magnetic fluids. It can also be applied to the magnetic separation of iron ores from their gangue.
TABLEAU I
TABLE I
<SEP> AVANT <SEP> BROYAGE <SEP> APRES <SEP> BROYAGE
<tb> Essais <SEP> Composition <SEP> Caractéristiques <SEP> Caractéristique
<tb> <SEP> (origine) <SEP> Taille <SEP> Surface <SEP> Teneur <SEP> Moment <SEP> magnétique <SEP> Taille <SEP> Surface <SEP> Teneur <SEP> Moment <SEP> magnétique
<tb> <SEP> Fisher <SEP> spécifique <SEP> spécifique <SEP> massique <SEP> Fisher <SEP> spécifique <SEP> en <SEP> Fe2+ <SEP> massique
<tb> <SEP> m <SEP> m/g <SEP> % <SEP> A.m/kg.<SEP> m <SEP> m/g <SEP> % <SEP> A.m/kg
<tb> 1 <SEP> Fe2O3 <SEP> 3,50 <SEP> 1,55 <SEP> 0,55 <SEP> 1,5 <SEP> 0,40 <SEP> 11,3 <SEP> 7,2 <SEP> 45
<tb> <SEP> (naturelle)
<tb> 2 <SEP> F2O3 <SEP> 0,65 <SEP> 3,97 <SEP> 0,19 <SEP> 1,7 <SEP> 0,40 <SEP> 10,3 <SEP> 6,6 <SEP> 56
<tb> <SEP> (ex-pickling)
<tb> 3 <SEP> Fe2O3 <SEP> 0,70 <SEP> 3,90 <SEP> 0,12 <SEP> 1,0 <SEP> 0,50 <SEP> 8,6 <SEP> 0,8 <SEP> 15
<tb> <SEP> (synthétique)
<tb> 91
I
<SEP> BEFORE <SEP> MILLING <SEP> AFTER <SEP> MILLING
<tb> Tests <SEP> Composition <SEP> Characteristics <SEP> Characteristic
<tb><SEP> (origin) <SEP> Size <SEP> Surface <SEP> Content <SEP> Moment <SEP> Magnetic <SEP> Size <SEP> Surface <SEP> Content <SEP> Moment <SEP> Magnetic
<tb><SEP> Fisher <SEP> specific <SEP> specific <SEP> mass <SEP> Fisher <SEP> specific <SEP> in <SEP> Fe2 + <SEP> mass
<tb><SEP> m <SEP> m / g <SEP>% <SE> Am / kg. <SEP> m <SEP> m / g <SEP>% <SE> Am / kg
<tb> 1 <SEP> Fe2O3 <SEP> 3.50 <SEP> 1.55 <SEP> 0.55 <SEP> 1.5 <SEP> 0.40 <SEP> 11.3 <SEP> 7.2 <SEP> 45
<tb><SEP> (natural)
<tb> 2 <SEP> F2O3 <SEP> 0.65 <SEP> 3.97 <SEP> 0.19 <SEP> 1.7 <SEP> 0.40 <SEP> 10.3 <SEP> 6.6 <SEP> 56
<tb><SEP> (ex-pickling)
<tb> 3 <SEP> Fe2O3 <SEP> 0.70 <SEP> 3.90 <SEP> 0.12 <SEP> 1.0 <SEP> 0.50 <SEP> 8.6 <SEP> 0.8 <SEP> 15
<tb><SEP> (synthetic)
<tb> 91
I
<SEP> Variation <SEP> des <SEP> conditions <SEP> de <SEP> broyage <SEP> Taille <SEP> Surface <SEP> Teneur <SEP> en <SEP> Moment <SEP> magnétique <SEP> Perte <SEP> de <SEP> poids
<tb> <SEP> Fisher <SEP> spécifique <SEP> Fe2+ <SEP> massique <SEP> des <SEP> billes
<tb> <SEP> m <SEP> m/g <SEP> % <SEP> A.m/kg <SEP> (g)
<tb> Conditions <SEP> de <SEP> référence <SEP> de <SEP> l'exemple <SEP> 1 <SEP> 0,40 <SEP> 10,3 <SEP> 6,6 <SEP> 56 <SEP> 60
<tb> 14 <SEP> kg <SEP> de <SEP> billes <SEP> d'acier <SEP> remplacées <SEP> par
<tb> 20 <SEP> kg <SEP> de <SEP> billes <SEP> de <SEP> carbure <SEP> de <SEP> tungstène <SEP> 0,65 <SEP> 12,3 <SEP> - <SEP> 0,4 <SEP> 70
<tb> Durée <SEP> de <SEP> 7 <SEP> jours <SEP> au <SEP> lieu <SEP> de <SEP> 2 <SEP> jours <SEP> 0,30 <SEP> 12,3 <SEP> 16,0 <SEP> 70 <SEP> 91
<tb> Eau <SEP> remplacée <SEP> par <SEP> de <SEP> l'acétone <SEP> 0,50 <SEP> 15 <SEP> 1,3 <SEP> 9,8 <SEP> 4 <SEP> ouvertures <SEP> du <SEP> broyeur <SEP> pendant <SEP> les <SEP> 0,50 <SEP> 9,1 <SEP> 2,2 <SEP> 27 <SEP> 57
<tb> 2 <SEP> jours
<tb> Quantité <SEP> d'eau <SEP> portée <SEP> à <SEP> litres <SEP> 0,40 <SEP> 12,4 <SEP> 14,4 <SEP> 64 <SEP> 89
<tb> <SEP> Variation <SEP> of <SEP> conditions <SEP> of <SEP> grinding <SEP> Size <SEP> Surface <SEP> Content <SEP> in <SEP> Moment <SEP> magnetic <SEP> Loss <SEP > of <SEP> weight
<tb><SEP> Fisher <SEP> specific <SEP> Fe2 + <SEP> mass <SEP> of <SEP> beads
<tb><SEP> m <SEP> m / g <SEP>% <SEP> Am / kg <SEP> (g)
<tb><SEP> Conditions of <SEP> Reference <SEP> of <SEP> Example <SEP> 1 <SEP> 0.40 <SEP> 10.3 <SEP> 6.6 <SEP> 56 <SEP > 60
<tb> 14 <SEP> kg <SEP> of <SEP><SEP> steel <SEP> balls replaced by <SEP> by
<tb> 20 <SEP> kg <SEP> of <SEP> beads <SEP> of <SEP> carbide <SEP> of <SEP> tungsten <SEP> 0.65 <SEP> 12.3 <SEP> - <SEP > 0.4 <SEP> 70
<tb> Duration <SEP> of <SEP> 7 <SEP> days <SEP> at <SEP> place <SEP> of <SEP> 2 <SEP> days <SEP> 0.30 <SEP> 12.3 <SEP > 16.0 <SEP> 70 <SEP> 91
<tb> Water <SEP> replaced <SEP> with <SEP> of <SEP> acetone <SEP> 0.50 <SEP> 15 <SEP> 1.3 <SEP> 9.8 <SEP> 4 <SEP > openings <SEP> of <SEP> mill <SEP> during <SEP><SEP> 0,50 <SEP> 9,1 <SEP> 2,2 <SEP> 27 <SEP> 57
<tb> 2 <SEP> days
<tb> Quantity <SEP> of water <SEP> range <SEP> to <SEP> liters <SEP> 0.40 <SEP> 12.4 <SEP> 14.4 <SE> 64 <SEP> 89
<Tb>
Claims (3)
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
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FR8026991A FR2498587A1 (en) | 1980-12-16 | 1980-12-16 | Magnetic iron oxide powder mfr. - by wet grinding non magnetic iron oxide with steel balls in steel mill |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
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FR8026991A FR2498587A1 (en) | 1980-12-16 | 1980-12-16 | Magnetic iron oxide powder mfr. - by wet grinding non magnetic iron oxide with steel balls in steel mill |
Publications (2)
Publication Number | Publication Date |
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FR2498587A1 true FR2498587A1 (en) | 1982-07-30 |
FR2498587B1 FR2498587B1 (en) | 1984-11-02 |
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FR8026991A Granted FR2498587A1 (en) | 1980-12-16 | 1980-12-16 | Magnetic iron oxide powder mfr. - by wet grinding non magnetic iron oxide with steel balls in steel mill |
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FR (1) | FR2498587A1 (en) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0880149A1 (en) * | 1997-02-21 | 1998-11-25 | Ferrofluidics Corporation | Method for manufacturing ferrofluid |
EP0936635A1 (en) * | 1998-02-10 | 1999-08-18 | Ferrofluidics Corporation | Method for manufacturing oil-based ferrofluid |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3904540A (en) * | 1972-02-11 | 1975-09-09 | Pfizer | Magnetic impulse record member |
DE2710777A1 (en) * | 1976-03-12 | 1977-10-06 | Eastman Kodak Co | MAGNETIC RECORDING MATERIAL |
-
1980
- 1980-12-16 FR FR8026991A patent/FR2498587A1/en active Granted
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3904540A (en) * | 1972-02-11 | 1975-09-09 | Pfizer | Magnetic impulse record member |
DE2710777A1 (en) * | 1976-03-12 | 1977-10-06 | Eastman Kodak Co | MAGNETIC RECORDING MATERIAL |
Non-Patent Citations (2)
Title |
---|
CA1974 * |
CA1976 * |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0880149A1 (en) * | 1997-02-21 | 1998-11-25 | Ferrofluidics Corporation | Method for manufacturing ferrofluid |
US5958282A (en) * | 1997-02-21 | 1999-09-28 | Ferrofluidic Corporation | Low cost method for manufacturing ferrofluid |
EP0936635A1 (en) * | 1998-02-10 | 1999-08-18 | Ferrofluidics Corporation | Method for manufacturing oil-based ferrofluid |
US6068785A (en) * | 1998-02-10 | 2000-05-30 | Ferrofluidics Corporation | Method for manufacturing oil-based ferrofluid |
Also Published As
Publication number | Publication date |
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FR2498587B1 (en) | 1984-11-02 |
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