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Process for Preparing Metal Halides by the Sol-Gel Method

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Process for Preparing Metal Halides by the Sol-Gel Method Europaisches Patentamt (19) European Patent Office Office europeenpeen des brevets EP 0 71 3 840 B1 (12) EUROPEAN PATENT SPECIFICATION (45) Date of publication and mention (51) mt ci.6: C01 F 1 1/20, C01 F 1 1/22, of the grant of the patent: C01F 11/34, C01F 17/00, 29.09.1999 Bulletin 1999/39 C01B9/00, C01B9/04, C03C (21) Application number: 95420313.9 C01B9/08, 17/22, C01F5/28 (22) Date of filing: 15.11.1995 (54) Process for preparing metal halides by the sol-gel method Verfahren zur Herstellung von Metallhalogeniden mittels Sol-Gel-Verfahren Procede de preparation des halogenures metalliques par voie sol-gel (84) Designated Contracting States: (74) Representative: Fevrier, Murielle Frangoise E. BE CH DE ES FR GB IT LI NL KODAK INDUSTRIE Departement Brevets - CRT (30) Priority: 23.11.1994 FR 9414309 Zone Industrielle - B.P. 21 71102 Chalon-sur-Saone Cedex (FR) (43) Date of publication of application: 29.05.1996 Bulletin 1996/22 (56) References cited: EP-A- 0 125 721 US-A- 5 051 278 (73) Proprietors: • KODAK-PATHE • NOUVEAU JOURNAL DE CHIMIE, vol. 5, no. 10, F-75594 Paris Cedex 12 (FR) 1981 GAUTHIER-VILLARS, pages 479-484, J. L. Designated Contracting States: NAMY ET AL. 'Smooth synthesis and FR characterization of divalent samarium and • EASTMAN KODAK COMPANY ytterbium derivatives' Rochester, New York 14650-2201 (US) • JOURNAL OF MATERIALS SCIENCE LETTERS, Designated Contracting States: vol. 11, no. 3, February 1992 LONDON GB, pages BE CH DE ES GB IT LI NL 152-154, XP 000248754 C. RUSSEL 'Preparation of LiF, CaF2 and YF3 by thermal decomposition (72) Inventor: Poncelet, Olivier Jean Christian, of the metal trifluoroacetates' Kodak-Pathe F-71102 Chalon sur Saone Cedex (FR) DO o ^- 00 CO Note: Within nine months from the publication of the mention of the grant of the European patent, any person may give notice the Patent Office of the Notice of shall be filed in o to European opposition to European patent granted. opposition a written reasoned statement. It shall not be deemed to have been filed until the opposition fee has been paid. (Art. a. 99(1) European Patent Convention). LU Printed by Jouve, 75001 PARIS (FR) 1 EP 0 713 840 B1 2 Description tained by the decomposition of a metal fluoride precur- sor. [0001] The present invention concerns a process for [0012] For example, in US patent 4 492 721 , magne- obtaining metal halides, in particular rare earth and/or sium fluoride layers are obtained by the decomposition alkaline earth halides, and novel materials in powder, 5 of fluorinated organic compounds of magnesium, such film or bulk material form obtained from these metal hal- as magnesium trifluoroacetate. ides. [0013] US patents 5 051 278 and 5 271 956 describe [0002] Metal halides are compounds which have a process for forming films of metal fluorides, in partic- been known for a long time. For example, alkaline earth ular binary and ternary alkaline earth or lanthanide flu- fluorides (group I IA), 4th period transition metal fluorides 10 orides. or rare earth fluorides (group NIB) are known. These This process consists of forming a coating solution con- metal fluorides have interesting electrical, magnetic and taining a non-fluorinated organometallic compound, a optical properties. solvent and afluorination agent and coating this solution [0003] Alkaline earth fluorides have low refractive in- on a support. The film thus obtained is then heated at a dexes, which enables them to be used in an anti-reflec- is temperature of approximately 500°C in order to decom- tive layer on supports with a high reflective index. pose the products contained in the coating solution into [0004] The layers obtained from these fluorides in pure metal fluoride. In order to obtain a uniform layer, a general have low dielectric constants, are transparent temperature increase is effected with a gradient of and have excellent mechanical properties. around 50°C/min. [0005] All these special properties mean that metal 20 [0014] US patents 5 208 101 and 5 268 196 describe fluorides are compounds which are advantageous for a process for forming layers comprising alkali metal or piezoelectric, ferromagnetic or anti-ferromagnetic, elec- alkaline earth fluorides using sol-gel technology. This tro-optical, pyroelectrical or non-linear optics applica- process consists of forming a layer on a glass substrate tions. using a coating solution containing a light metal oxide [0006] Mixed rare earth and alkaline earth metal hal- 25 precursor, a non-aqueous solvent and water, heating ides are also known as luminescent substances used the layer in order to density the layer of light metal ox- for example to convert X-rays or gamma radiation into ides, and exposing this densified layer at a high temper- visible light. ature to a gaseous current containing fluorine. The den- [0007] Many publications describe the use of mixed sification of the oxide layer is effected at a temperature alkaline earth halides as luminescent substances, in 30 of around 500°C and the fluorination is effected at tem- particular in radiographic products. peratures of around 300°C. [0008] For example, European patent EP 149148 de- [0015] In all the known processes set out above, the scribes radiographic image recording screens which metal halide layers are obtained using high tempera- contain, in the storage layer, a mixed alkaline earth hal- tures, either to vaporise the metal halides or to decom- ide of general formula BaF(XY):Eu:Sr in which X and Y 35 pose a precursor of the metal halides, or to density the are halide atoms. These luminescent substances are base metal oxide layer and to halogenate this same lay- obtained by mixing BaF2, BaCI2, BaBr2, EuF3 and SrCI er. in a ball mill. The mixture is then baked red hot in a bro- [0016] All these processes enabling layers of metal mium vapour chamber for 1 to 5 hours at a temperature halides to be obtained have many drawbacks related to of between 800 and 1000°C. After cooling, the product 40 the necessity to use high temperatures. In particular, the is broken up, washed and then dried. In this way the choice of the support for the metal halide layer is very luminescent substance described above is obtained. limited. In addition, at high temperature, it is very difficult This technique, which is difficult to implement, does not to obtain homogeneous metal halide layers having con- make it possible to control the stoichiometry of the final trolled stoichiometry. product. 45 [001 7] The object of the present invention concerns a [0009] It is known that thin layers of luminescent sub- process for obtaining homogeneous metal halides at stances can be formed by chemical vapour phase dep- low temperature, in powder, layer, fibre or bulk material osition. Such layers are obtained with difficulty because form. of the differences in vapour tension and stability of each [0018] The present invention makes it possible to of the constituents. so eliminate the problems relating to the use of high tem- [0010] A process for obtaining layers of metal fluo- peratures. For example, the process of the present in- rides was described in US patent 3 475 192. Such a vention makes it possible to obtain metal halide layers process consists of coating, on a substrate, a magnesi- on amuch widervariety of supports, in particular organic um fluoride solution in a polar solvent and heating the supports which have very little resistance to high tem- substrate thus covered at between 100 and 1000°C. In 55 peratures. this process, it is necessary, in order to obtain a film, to [0019] The process for preparing alkaline earth and/ use a substrate which is resistant to high temperatures. or rare earth metal halides of the present invention con- [0011] It is known that metal fluoride layers can be ob- sists of forming a homogeneous solution by mixing one 2 3 EP 0 713 840 B1 4 or more rare earth and/or alkaline earth halogenoalkox- yield of such a synthesis depends in particular on the ides in an anhydrous organic solvent and adding to this steric hindrance of the alcohol used. The smaller the solution a quantity of water which is at least stoichiomet- steric hindrance, the faster will be the synthesis of the ric in order to hydrolyse the halogenoalkoxides. alkaline earth alkoxides. The alcohol is preferably cho- [0020] Within the scope of the invention, the halog- 5 sen from amongst methanol, ethanol or propanol. enoalkoxides and consequently the metal halides may [0032] The rare earth alkoxides can be synthesised contain one or more halogen atoms chosen from according to one of the following two methods. amongst fluorine, bromine, chlorine and iodine. [0033] The first method consists of reacting a rare [0021] Figure 1 is an FT-Raman spectrum of the bar- earth chloride, for example lanthane chloride, directly ium fluoroalkoxide used to obtain, according to the in- 10 with an alkali metal alkoxide, for example a sodium or vention, barium fluoride. lithium alkoxide. This synthesis has drawbacks related [0022] Figure 2 is an X-ray diffraction spectrum of a to the presence of chloride in the reaction medium. In barium fluoride powder obtained by hydrolysis of the addition, lanthanide chlorides are particularly stable barium fluoroalkoxide of Figure 1 . chemical species which are difficult to activate, which [0023] Figure 3 is an X-ray diffraction spectrum of a is gives rise to low reaction yields. europium fluoride powder obtained according to the [0034] A second method of synthesising rare earth process of the present invention. alkoxides consists of reacting the rare earth directly with [0024] Figure 4 is a spectrum obtained by energy dis- an alcohol such as 2-propanol or a functionalised alco- persive X-ray microanalysis, of the compound hol such as 2-methoxyethanol.
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