WO2001049605A2 - Procede de preparation de borates de terre rare et utilisation des borates obtenus en luminescence - Google Patents
Procede de preparation de borates de terre rare et utilisation des borates obtenus en luminescence Download PDFInfo
- Publication number
- WO2001049605A2 WO2001049605A2 PCT/FR2000/003525 FR0003525W WO0149605A2 WO 2001049605 A2 WO2001049605 A2 WO 2001049605A2 FR 0003525 W FR0003525 W FR 0003525W WO 0149605 A2 WO0149605 A2 WO 0149605A2
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- rare earth
- borate
- borates
- bicarbonate
- carbonate
- Prior art date
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- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 45
- -1 rare earth borates Chemical class 0.000 title claims abstract description 30
- 238000004020 luminiscence type Methods 0.000 title claims abstract description 12
- 150000001642 boronic acid derivatives Chemical class 0.000 title abstract description 17
- 238000004519 manufacturing process Methods 0.000 title abstract description 6
- 239000000203 mixture Substances 0.000 claims abstract description 21
- 239000004327 boric acid Substances 0.000 claims abstract description 14
- BVKZGUZCCUSVTD-UHFFFAOYSA-M Bicarbonate Chemical compound OC([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-M 0.000 claims abstract description 13
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims abstract description 13
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000002244 precipitate Substances 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims description 41
- 238000002360 preparation method Methods 0.000 claims description 18
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 16
- 150000002910 rare earth metals Chemical class 0.000 claims description 16
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 claims description 15
- 229910052688 Gadolinium Inorganic materials 0.000 claims description 9
- 229910021529 ammonia Inorganic materials 0.000 claims description 8
- 229910052684 Cerium Inorganic materials 0.000 claims description 7
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims description 7
- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 0.000 claims description 7
- 150000003839 salts Chemical class 0.000 claims description 7
- 239000001099 ammonium carbonate Substances 0.000 claims description 6
- 229910052727 yttrium Inorganic materials 0.000 claims description 6
- 229910052693 Europium Inorganic materials 0.000 claims description 5
- 239000012429 reaction media Substances 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims description 5
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 4
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 4
- 229910052746 lanthanum Inorganic materials 0.000 claims description 4
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims description 4
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 3
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 claims description 3
- 229910052706 scandium Inorganic materials 0.000 claims description 3
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 claims description 3
- 229910052691 Erbium Inorganic materials 0.000 claims description 2
- 229910052765 Lutetium Inorganic materials 0.000 claims description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 2
- 229910052771 Terbium Inorganic materials 0.000 claims description 2
- 229910052775 Thulium Inorganic materials 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 235000012501 ammonium carbonate Nutrition 0.000 claims description 2
- 229910052787 antimony Inorganic materials 0.000 claims description 2
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims description 2
- 229910052797 bismuth Inorganic materials 0.000 claims description 2
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 2
- UYAHIZSMUZPPFV-UHFFFAOYSA-N erbium Chemical compound [Er] UYAHIZSMUZPPFV-UHFFFAOYSA-N 0.000 claims description 2
- OHSVLFRHMCKCQY-UHFFFAOYSA-N lutetium atom Chemical compound [Lu] OHSVLFRHMCKCQY-UHFFFAOYSA-N 0.000 claims description 2
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 239000010703 silicon Substances 0.000 claims description 2
- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 claims description 2
- 238000001354 calcination Methods 0.000 abstract description 5
- 238000002156 mixing Methods 0.000 abstract description 4
- 125000001424 substituent group Chemical group 0.000 description 9
- 239000002245 particle Substances 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 239000002019 doping agent Substances 0.000 description 4
- 239000002243 precursor Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 239000002585 base Substances 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 230000018109 developmental process Effects 0.000 description 3
- 230000001376 precipitating effect Effects 0.000 description 3
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 230000005284 excitation Effects 0.000 description 2
- 230000005669 field effect Effects 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 230000005070 ripening Effects 0.000 description 2
- 238000004626 scanning electron microscopy Methods 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- OVSKIKFHRZPJSS-UHFFFAOYSA-N 2,4-D Chemical compound OC(=O)COC1=CC=C(Cl)C=C1Cl OVSKIKFHRZPJSS-UHFFFAOYSA-N 0.000 description 1
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 229910052777 Praseodymium Inorganic materials 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 229910052769 Ytterbium Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 150000001412 amines Chemical group 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- NKCVNYJQLIWBHK-UHFFFAOYSA-N carbonodiperoxoic acid Chemical compound OOC(=O)OO NKCVNYJQLIWBHK-UHFFFAOYSA-N 0.000 description 1
- HQNHTEJTBUTVAE-UHFFFAOYSA-N cerium(3+);borate Chemical compound [Ce+3].[O-]B([O-])[O-] HQNHTEJTBUTVAE-UHFFFAOYSA-N 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000004320 controlled atmosphere Methods 0.000 description 1
- 238000001962 electrophoresis Methods 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 238000007650 screen-printing Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000012800 visualization Methods 0.000 description 1
- NAWDYIZEMPQZHO-UHFFFAOYSA-N ytterbium Chemical compound [Yb] NAWDYIZEMPQZHO-UHFFFAOYSA-N 0.000 description 1
- BXJPTTGFESFXJU-UHFFFAOYSA-N yttrium(3+);trinitrate Chemical class [Y+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O BXJPTTGFESFXJU-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B35/00—Boron; Compounds thereof
- C01B35/08—Compounds containing boron and nitrogen, phosphorus, oxygen, sulfur, selenium or tellurium
- C01B35/10—Compounds containing boron and oxygen
- C01B35/12—Borates
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7712—Borates
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7766—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals
- C09K11/778—Borates
Definitions
- the present invention relates to a process for the preparation of rare earth borates and the use of these borates in luminescence.
- the object of the invention is therefore to provide an improved process making it possible in particular to lead to borates of rare earth and phasically pure cerium.
- the process for the preparation of a rare earth borate according to the invention is characterized in that it comprises the following stages:
- the invention also relates to a process for the preparation of a rare earth hydroxyborocarbonate, precursor of a rare earth borate, characterized in that it comprises the following stages:
- the process of the invention relates to the preparation of borates or hydroxyborocarbonates of rare earth.
- rare earth is understood for the whole of this description the elements of the group constituted by yttrium, scandium and the elements of the periodic classification with atomic number included inclusively between 57 and 71.
- rare earth borate is meant the products of formula LnBO ⁇ (orthoborate), Ln denoting the rare earth as defined above.
- rare earth hydroxyborocarbonate is meant the products of formula LnB (OH) z (CO) y , this hydroxyborocarbonate can be more or less hydrated. It is understood that the process of the present invention also applies to the preparation of borates or hydroxyborocarbonates " mixed of rare earths, of formulas given above and in which Ln consists of a mixture of two or more rare earths. The process of the present invention can be used very particularly for the preparation of a borate or a hydroxyborocarbonate of yttrium, lanthanum, lutetium, scandium or gadolinium. One can also mention more particularly the preparation of a ytterbium or cerium borate.
- the process also applies to the preparation of doped or substituted rare earth borates of formula Ln-
- the purpose of this doping or substituent element is to give borate luminescence properties or to reinforce them and it can be chosen from the group comprising aluminum, silicon, antimony, bismuth, rare earths and in particular in this case cerium, terbium, lanthanum, gadolinium , europium, thulium, erbium and praseodymium.
- the value of x can be up to 0.5.
- rare earths appear in this group, it goes without saying that the rare earth used as dopant or substituent will be different from the rare earth constituting the borate.
- the process of the invention obviously applies to the preparation of the hydroxyborocarbonates which are precursors of the abovementioned doped or substituted borates.
- the method of the invention comprises a first step in which a rare earth salt and boric acid are mixed.
- the rare earth salt can be an inorganic or organic salt. Water-soluble salts are preferably used.
- a rare earth salt nitrate may be mentioned more particularly.
- a salt from each of the rare earths concerned will of course be used.
- boric which comprises, in addition, a salt of the doping or substituent element and what has been said above for the rare earth salts also applies here.
- Boric acid can be used in the form of a solution or, preferably, in the solid form.
- the mixing can be done with a fast mixer.
- a fast mixer any system allowing rapid introduction of the reagents into the reactor, in particular by a piston system, and rapid and homogeneous contacting of these reagents.
- a Y-shaped tube can thus be used as a mixer of this type.
- the mixing can be carried out at room temperature or by heating.
- the mixture thus obtained is acidic, it can be neutralized up to a pH value of 4 or around 4, for example by adding an ammonia solution.
- the second stage of the process of the invention consists in reacting the mixture obtained in the preceding stage with a carbonate or a bicarbonate (the carbonate or the bicarbonate must be soluble in water).
- alkali carbonates can be mentioned. More particularly, ammonium carbonate or bicarbonate can be used.
- the reaction is carried out in the presence of a base.
- a base As usable base, mention may be made of alkali or alkaline-earth hydroxides, ammonia, secondary, tertiary or quaternary amines. Ammonia is preferably used.
- the salt of the dopant or substituent can also be introduced during the reaction if this has not been done during from the previous step.
- the reaction is carried out by regulating the pH.
- the pH of the reaction medium is adjusted to a fixed value. This regulation can be done by varying the amount of base used for the reaction. This fixed value is preferably between 4 and 6.
- the reaction can be carried out at room temperature or hot.
- a ripening step can then be carried out. This step consists in maintaining the reaction medium at a given temperature, preferably hot, at a constant pH and at the value described above, optionally under a controlled atmosphere. The duration of this ripening is generally at least 15 minutes and at most 8 hours.
- a precipitate is obtained which is separated from the reaction medium by any known means, for example by filtration and which, optionally, is washed and then dried.
- a product based on a rare earth hydroxyborocarbonate is thus obtained, which can also comprise the doping or substituent element.
- This calcination is generally carried out at a temperature between 500 ° C and 1400 ° C, more particularly between 500 and 1100 ° C. It is possible to carry out this calcination in air or in reducing atmospheres (hydrogen for example) or neutral (argon) or mixtures thereof.
- the procedure is carried out by mixing the hydroxybprocarbonate obtained above with the abovementioned element or elements in solid form, for example in the form of oxide, carbonate, hydroxycarbonate, in particular in the form of SiO 2 , AI 2 O 3 , AI (OH) CO 3 .
- the borate obtained can be in the form of spherical, cubic or parallelepipedic particles.
- the average particle size is at most 10 ⁇ m, more particularly at most 5 ⁇ m and, even more particularly, it can be between 0.5 and 5 ⁇ m.
- the sizes mentioned here are determined by the laser diffraction technique using a granulator of the COULTER type (LS 230).
- the particles have a homogeneous morphology, that is to say that the majority of them, and preferably all of them, have this same morphology.
- the process of the invention has several advantages.
- the reaction time is reduced.
- it allows you to work in a more concentrated environment with optimized amounts of reagents.
- it makes it possible to work with a reduced amount of carbonate, which results in the absence of foaming during the reaction.
- the process of the invention makes it possible in particular to prepare a rare earth borate doped with cerium.
- the cerium content of this borate can be at most 8% (x as defined above at most 0.08), it can more particularly be between 1 and 5%.
- This borate is in the form of a pure phase.
- the X-ray analysis of the product calcined at 1100 ° C. shows only a single phase which corresponds to the mesh of the rare earth borate LnBO 3 .
- This phasic purity implies that the cerium is stabilized in the 3 + state in the borate.
- the borate comprises a constituent rare earth, that is to say the rare earth which forms with boron the matrix of the product and other than the dopant or substituent, which is yttrium or gadolinium or else a combination of the two; in the latter case the borate is a mixed borate of yttrium and gadolinium.
- Borates as obtained by the process described above can be used as phosphors. They can be used in particular in low voltage luminescence, in particular in the manufacture of any device implementing this low voltage luminescence, such as screens with field effect. They also exhibit luminescence properties under electromagnetic excitation in the wavelength range used in plasma systems and in mercury vapor lamps. Thus, they can be used as phosphors in plasma systems (display screen or lighting system) or in trichromatic lamps.
- the invention also relates to luminescent devices, of the screen type with field effect for example, incorporating the borates described above or as obtained by the process of the invention.
- the phosphors are arranged on the screens subjected to low energy excitation.
- the invention relates to plasma systems in the manufacture of which borates can be used. The use of phosphors in the manufacture of low voltage luminescence devices or plasma systems is done according to well known techniques for example by screen printing, electrophoresis or sedimentation.
- a solution consists of a mixture of yttrium nitrates, of gadolinium and of europium, of the following composition (in atomic%): Y: 72% Gd: 23% Eu: 5%
- crystallized boric acid is mixed, and the solution of rare earth nitrates (TR), in proportions such that the molar ratio B / TR is equal to 1.5.
- TR rare earth nitrates
- the mixture thus formed is then neutralized to pH 4.4 with 6N ammonia, then the concentration of the mixture is adjusted to 0.6 mol / liter of TR elements by adding water.
- the temperature of the reaction medium is kept constant and equal to 60 ° C.
- This mixture is then kept heated and stirred for 40 minutes.
- the precipitate is then filtered on B ⁇ chner, then washed with 2 liters of cold boric acid solution at 2 g / liter (0.03 mol / liter).
- the solid obtained is dried at 60 ° C for 1 night, then calcined at 900 ° C for 1 hour 15 minutes.
- the amount of bicarbonate solution added is such that the HCO 3 7TR molar ratio is equal to 1.6.
- This mixture is then kept heated to 60 ° C and stirred for 2 hours 50 minutes, while regulating its pH to 4.6 by adding 6N ammonia.
- the concentration of the suspension obtained is then 0.22 mole LnBO 3 / liter.
- the precipitate is then filtered on B ⁇ chner, then washed with 2 liters of cold water.
- the solid obtained is dried at 60 ° C for 1 night, then calcined at 900 ° C for 1 hour.
- the powder obtained after slight disagglomeration corresponds, by X-ray diffraction analysis, to a pure rare earth orthoborate, LnBO3 with particles of cubic shape, as shown by the analysis by scanning electron microscopy.
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Luminescent Compositions (AREA)
- Gas-Filled Discharge Tubes (AREA)
- Vessels And Coating Films For Discharge Lamps (AREA)
Abstract
Description
Claims
Priority Applications (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP00993705A EP1242309B1 (fr) | 1999-12-29 | 2000-12-14 | Procede de preparation de borates de terre rare et utilisation des borates obtenus en luminescence |
DE60005999T DE60005999T2 (de) | 1999-12-29 | 2000-12-14 | Verfahren zur herstellung von seltenerdboraten und verwendung der hergestellten boraten in lumineszenz |
JP2001550148A JP4723150B2 (ja) | 1999-12-29 | 2000-12-14 | 希土類ホウ酸塩の製造方法、及びそのホウ酸塩の発光体への応用 |
US10/169,023 US7208130B2 (en) | 1999-12-29 | 2000-12-14 | Process for preparing rare earth borates, and use of the borates obtained in luminescence |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
FR99/16644 | 1999-12-29 | ||
FR9916644A FR2803281B1 (fr) | 1999-12-29 | 1999-12-29 | Procede de preparation de borates de terre rare et utilisation des borates obtenus en luminescence |
Publications (2)
Publication Number | Publication Date |
---|---|
WO2001049605A2 true WO2001049605A2 (fr) | 2001-07-12 |
WO2001049605A3 WO2001049605A3 (fr) | 2002-01-31 |
Family
ID=9553958
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/FR2000/003525 WO2001049605A2 (fr) | 1999-12-29 | 2000-12-14 | Procede de preparation de borates de terre rare et utilisation des borates obtenus en luminescence |
Country Status (9)
Country | Link |
---|---|
US (1) | US7208130B2 (fr) |
EP (1) | EP1242309B1 (fr) |
JP (1) | JP4723150B2 (fr) |
KR (1) | KR100487454B1 (fr) |
CN (1) | CN1282606C (fr) |
DE (1) | DE60005999T2 (fr) |
FR (1) | FR2803281B1 (fr) |
TW (1) | TW490440B (fr) |
WO (1) | WO2001049605A2 (fr) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2007042653A1 (fr) * | 2005-10-13 | 2007-04-19 | Rhodia Operations | Borate de terre rare submicronique, son procede de preparation et son utilisation comme luminophore |
Families Citing this family (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN100391847C (zh) * | 2005-04-05 | 2008-06-04 | 内蒙古包钢稀土高科技股份有限公司 | 稀土盐的制备方法及装置 |
CN102517013B (zh) * | 2011-11-24 | 2014-12-03 | 合肥工业大学 | 一种光子转换材料及其制备方法 |
US9062220B2 (en) * | 2012-11-30 | 2015-06-23 | Honeywell International Inc. | Luminescent borates, luminescent materials and articles incorporating such borates |
TR202004482A1 (tr) * | 2020-03-23 | 2021-10-21 | Vertratech Kimya Sanayi Ve Ticaret Ltd Sirketi | Amorf ve nano yapılı lutesyum borat hekzahidratın sentezi ve kararlı kolloidal dispersiyonlarını hazırlama yöntemi |
RU2761209C1 (ru) * | 2021-04-06 | 2021-12-06 | Федеральное государственное бюджетное учреждение науки Институт химии Дальневосточного отделения Российской академии наук (ИХ ДВО РАН) | Способ получения боратов лантана, легированных европием и тербием |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
FR2743555A1 (fr) * | 1996-01-17 | 1997-07-18 | Rhone Poulenc Chimie | Borate de terre rare et son precurseur, leurs procedes de preparation et l'utilisation du borate comme luminophore |
FR2752833A1 (fr) * | 1996-09-03 | 1998-03-06 | Rhone Poulenc Chimie | Procede de preparation d'un borate de terre rare par reaction d'au moins un sel de terre rare, d'acide borique et d'une base |
Family Cites Families (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS5499800A (en) * | 1978-01-23 | 1979-08-06 | Agency Of Ind Science & Technol | Carboborate and production thereof |
JPS60231410A (ja) * | 1984-04-27 | 1985-11-18 | Res Assoc Util Of Light Oil | 新規なボロシリケート |
JPS62148590A (ja) * | 1985-12-23 | 1987-07-02 | Nichia Kagaku Kogyo Kk | ホウ酸インジウム螢光体 |
JP2721205B2 (ja) * | 1987-11-18 | 1998-03-04 | 株式会社東芝 | 非晶質酸化物磁性体及び磁心及び磁気記録媒体 |
FR2623790B1 (fr) * | 1987-11-26 | 1990-11-30 | Rhone Poulenc Chimie | Procede de preparation de borures de terres rares |
EP0341106B1 (fr) * | 1988-04-22 | 1992-09-09 | Rhone-Poulenc Chimie | Procédé de préparation de borures de terres rares |
JPH07197022A (ja) * | 1993-12-29 | 1995-08-01 | Tokyo Kagaku Kenkyusho:Kk | ホウ酸塩系蛍光体 |
US6197218B1 (en) * | 1997-02-24 | 2001-03-06 | Superior Micropowders Llc | Photoluminescent phosphor powders, methods for making phosphor powders and devices incorporating same |
-
1999
- 1999-12-29 FR FR9916644A patent/FR2803281B1/fr not_active Expired - Fee Related
-
2000
- 2000-12-14 EP EP00993705A patent/EP1242309B1/fr not_active Expired - Lifetime
- 2000-12-14 KR KR10-2002-7008565A patent/KR100487454B1/ko not_active IP Right Cessation
- 2000-12-14 CN CNB008185859A patent/CN1282606C/zh not_active Expired - Fee Related
- 2000-12-14 US US10/169,023 patent/US7208130B2/en not_active Expired - Fee Related
- 2000-12-14 DE DE60005999T patent/DE60005999T2/de not_active Expired - Lifetime
- 2000-12-14 JP JP2001550148A patent/JP4723150B2/ja not_active Expired - Fee Related
- 2000-12-14 WO PCT/FR2000/003525 patent/WO2001049605A2/fr active IP Right Grant
-
2001
- 2001-03-06 TW TW089128130A patent/TW490440B/zh active
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
FR2743555A1 (fr) * | 1996-01-17 | 1997-07-18 | Rhone Poulenc Chimie | Borate de terre rare et son precurseur, leurs procedes de preparation et l'utilisation du borate comme luminophore |
FR2752833A1 (fr) * | 1996-09-03 | 1998-03-06 | Rhone Poulenc Chimie | Procede de preparation d'un borate de terre rare par reaction d'au moins un sel de terre rare, d'acide borique et d'une base |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2007042653A1 (fr) * | 2005-10-13 | 2007-04-19 | Rhodia Operations | Borate de terre rare submicronique, son procede de preparation et son utilisation comme luminophore |
US8980130B2 (en) | 2005-10-13 | 2015-03-17 | Rhodia Operations | Submicron rare-earth borates and preparation/luminoshors thereof |
Also Published As
Publication number | Publication date |
---|---|
EP1242309B1 (fr) | 2003-10-15 |
US7208130B2 (en) | 2007-04-24 |
CN1424981A (zh) | 2003-06-18 |
EP1242309A2 (fr) | 2002-09-25 |
TW490440B (en) | 2002-06-11 |
FR2803281B1 (fr) | 2002-03-29 |
DE60005999D1 (de) | 2003-11-20 |
KR20020074467A (ko) | 2002-09-30 |
DE60005999T2 (de) | 2004-09-02 |
KR100487454B1 (ko) | 2005-05-06 |
JP2003519073A (ja) | 2003-06-17 |
JP4723150B2 (ja) | 2011-07-13 |
US20030161776A1 (en) | 2003-08-28 |
WO2001049605A3 (fr) | 2002-01-31 |
FR2803281A1 (fr) | 2001-07-06 |
CN1282606C (zh) | 2006-11-01 |
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