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Doped Yttrium Aluminium Borate

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Doped Yttrium Aluminium Borate (19) & (11) EP 2 354 208 A1 (12) EUROPEAN PATENT APPLICATION (43) Date of publication: (51) Int Cl.: 10.08.2011 Bulletin 2011/32 C09K 11/64 (2006.01) C09K 11/68 (2006.01) C09K 11/77 (2006.01) (21) Application number: 10152615.0 (22) Date of filing: 04.02.2010 (84) Designated Contracting States: (72) Inventors: AT BE BG CH CY CZ DE DK EE ES FI FR GB GR • Klimant, Ingo HR HU IE IS IT LI LT LU LV MC MK MT NL NO PL 8200 Labuch (AT) PT RO SE SI SK SM TR • Borisov, Sergey Designated Extension States: 8010 Graz (AT) AL BA RS • Gatterer, Karl 8041 Graz (AT) (71) Applicants: • Technische Universität Graz (74) Representative: Babeluk, Michael 8010 Graz (AT) Patentanwalt • B. Braun Melsungen AG Mariahilfer Gürtel 39/17 34212 Melsungen (DE) 1150 Wien (AT) (54) Luminescent material comprising chromium(III) doped yttrium aluminium borate (57) The invention concerns a luminescent material (BO3)4 with 0.03 ≤ x ≤ 0.30, preferably 0.06 ≤ x ≤ 0.12. exhibiting a temperature-dependent luminescence de- The luminescent material is preferably used as a tem- cay time, wherein the luminescent material comprises perature-sensitive component of a temperature-sensi- chromium(III) doped yttrium aluminium borate. The lumi- tive paint or coating or as a temperature sensing com- nescent material meets the chemical formula YAl3-xCrx ponent of a temperature sensor. EP 2 354 208 A1 Printed by Jouve, 75001 PARIS (FR) 1 EP 2 354 208 A1 2 Description could be used as coating in order to produce a special colour changing effect. (See also WO 2007/128016 A2) BACKGROUND OF THE INVENTION [0006] In US 6,303,386 B2 a device for the tempera- ture-compensated determination of a chemical parame- [0001] The invention relates to a luminescent material 5 ter is disclosed. The temperature sensor contains a tem- (thermographic phosphor) exhibiting a temperature-de- perature indicator comprising a luminescent metal com- pendent luminescence decay time. plex containing ruthenium(II) having a temperature-de- pendent decay time. DESCRIPTION OF PRIOR ART [0007] Apart from thermographic phosphors, organo- 10 metallic complexes which possess temperature-depend- [0002] Temperature is one of the most important pa- ent luminescence were found to be very useful probes. rameters to know in various fields of science and tech- Recently, they became increasingly popular and were nology, and in everyday life. Contactless sensing is par- applied in dually-sensing materials as shown for example ticularly attractive for various applications where inva- in Borisov, S. M.; Wolfbeis, O. S. Anal. Chem. 2006, 78, siveness is undesirable. 15 5094-5101 and in pressure- sensitive paints as disclosed [0003] Major contactless techniques include optical in Demas, J. N.; DeGraff, B. A.; Coleman, P. B. Anal. pyrometry, IR thermography and phosphor thermometry. Chem. 1999, 71, 793A- 800A. Such materials usually rely Among them, optical pyrometry is only suitable for meas- on the use of ruthenium(II) polypyridyl complexes and urements at high temperatures (> 600 °C). On the other europium(III) tris-β-diketonates. Not surprisingly, all side, much lower temperatures and particularly those 20 these luminophors have their pros and cons and more around room temperature (RT) are of great practical in- advanced materials are highly desired. terest. For example, precise temperature determination is essential in marine research, geochemical studies, SUMMARY OF THE INVENTION medicine, aeronautics, to mention only a few areas. Moreover, temperature is a key parameter in optical25 [0008] An"ideal" luminescentmaterial for sensingtem- sensing since the response of virtually all such sensors perature should fulfill the following requirements: is temperature-dependent. IR thermography has be- come very widespread but is still rather expensive and i) have high brightness; may suffer from various artifacts. Luminescent temper- ature-sensitive materials represent a promising alterna- 30 ii) possess excitation in visible or NIR part of the tive here. They respond to temperature by altering the spectrum; luminescence intensity or the decay time. Thermograph- ic phosphors are well established and have been in use iii) have high temperature sensitivity in the desired for decades. However, most of them are intended for range; sensing high temperatures and become useless at am- 35 bient temperatures. iv) be photostable; [0004] The suitable phosphors for RT sensing include e.g. manganese(IV)-doped magnesium fluoroger- v) have negligible cross-sensitivity to other analytes manate Mg4FGeO6, chromium(III)-doped yttrium-alu- such as e.g. oxygen; 40 minium garnet Y3Al5O12, aluminium oxide (ruby), spinel MgAl2O4 and yttrium-aluminium perovskite YAlO3, as vi) be commercially available or simple to manufac- well as europium(III)-doped lanthanum oxysulphide ture; and La2O2S-Suitable RT sensing phosphors are disclosed e.g. in Brübach, J.; Feist, J. P.; Dreizler, A. "Characteri- vii) have relatively long luminescence decay time (> zation of manganese-activated magnesium fluoroger- 45 1 Ps up to 100 ms) to lifetime interrogation. manate with regards to thermographic phosphor ther- mometry" Meas. Sci. Technol. 2008, 19, 025602 (11pp) [0009] It is an object of the present invention to present and also in Aizawa, H.; Ohishi, N.; Ogawa, S.; Watanabe, a new luminescent material, which fulfills the above men- E.; Katsumata, T.; Komuro, S.; Morikawa, T.; Toba, E. tioned requirements. "Fabrication of ruby sensor probe for the fiber- optic ther- 50 [0010] The invention achieves this object by a lumi- mometer using fluorescence decay" Rev. Sci. Instrum. nescent material which consist of or comprises chromium 2002, 73, 3089-3092. (III) doped yttrium aluminium borate (YAB). More prefer- [0005] In Fuchs, E.; Gatterer, K. "Colour change of co- ably the material is based on solid state yttrium aluminium doped yttrium aluminium borate crystals under illumina- borate as a host matrix material with chromium(III) ions tion with different white light sources" Cent. Eur. J. Chem. 55 as dopant. Surprisingly chromium(III) doped yttrium alu- 2008,6, 497-504 yttrium aluminium borate (YAB) crystals minium borate (YAB) fulfills all requirements i) to vii) and were co-doped with e.g. Cr and Nd or with Cr and Ho is, therefore, a thermographic phosphor of choice for resulting in a colour change. A microcrystalline powder sensing of ambient temperatures. 2 3 EP 2 354 208 A1 4 [0011] According to the invention the luminescent ma- Mg4FGe06 can not be efficiently excited in the red part terial meets the chemical formula YAl3-xCrx(BO3)4 with of the spectrum. 0.03 ≤ x ≤ 0.30, preferably 0.06 ≤ x ≤ 0.12. That means [0017] The Cr3+-doped YABs were obtained in two dif- about 1 to 10%, preferably 2 to 4% of aluminium ions are ferent methods. In the first method the crystals are grown substituted by chromium ions. 5 from the solution in high temperature flux potassium mo- [0012] According to a first preferred variant the lumi- lybdate. This method results in high purity crystals how- nescent material is a single crystal material, preferably ever is rather slow. Moreover, micrometer-sized powders obtained by high temperature flux growth from an oxide are strongly preferred for practical applications. There- mixture comprising Y2O3, Al2O3, B2O3 and Cr2O3. fore, grinding of the crystals is advantageous. [0013] According to a second preferred variant the lu- 10 [0018] On the other side, micrometer-sized powders minescent material is a micro crystalline powder, prefer- can be directly obtained via the combustion route from ably obtained by a solution combustion synthesis, e.g. the corresponding nitrates and boric acid. This method with urea as a fuel. is easier to upscale and is less time consuming. However, it results in microcrystalls with small impurities of other BRIEF DESCRIPTION OF THE DRAWINGS 15 phases with influence the properties of the phosphor to a minor extent. [0014] The invention will be further described below [0019] Fig. 3 shows dependences of the luminescence with reference to the enclosed drawings showing in decay time and luminescence intensity on the amount of Cr3+ ions which substitute Al3+ in YAB. Evidently, con- Fig. 1 Emission spectra of the Cr3+ and Mn4+ -doped 20 centration quenching is observed even at rather low con- 3+ thermographic phosphors (λexc = 405 nm); centration of Cr which is indicated by the decrease in luminescence decay time. However, the luminescence Fig. 2 Excitation spectra of the Cr3+ and Mn 4+ -doped intensity does increase with increasing of Cr3+ doping thermographic phosphors; since the amount of the absorbed light becomes signifi- 25 cantly higher. As can be seen (Fig. 3), the intensity drops Fig. 3 Dependence decay time and luminescence in- after more than 4% of aluminum ions (x = 0.12) are sub- tensity of the YAl3-xCrx(BO3)4 powders on the stituted by chromium. Thus, YABs where 2-4% of alumi- amount of Cr3+; num is substituted can be a good compromise between luminescence brightness and the degree of concentra- Fig. 4 Relative luminescence brightnesses (corrected 30 tion quenching. emission spectra) of the Cr3+-doped thermo- [0020] Brightness of the Cr 3+-doped YAB powder (x = graphic phosphors (λexc = 405 nm); 0.09) under 405 nm excitation was compared to the brightness of other thermographic phosphors. The phos- Fig. 5 Temperature dependence of the luminescence phors powders were excited with at 405 nm and the emis- decay time for Cr 3+ - doped YAB materials; and 35 sion spectra (corrected for the sensitivity of the photode- tector) were compared (Fig. 4). The brightnesses relative 4+ Fig. 6 Temperature sensitivities of the visible light-ex- to that of Mn -doped Mg4FGeO6 (= 1) were determined citable thermographic phosphors. to be 0.47, 0.34, 0.32 and 0.04 for Cr 3+-doped YAB, ruby, Cr3+-doped spinel and Cr3+-doped YAG, respectively. DETAILED DESCRIPTION OF THE PREFERRED EM- 40 Evidently, Cr3+-doped YAB shows excellent brightness 4+ BODIMENT which is comparable to that of Mn -doped Mg4FGO6 (lamp phosphor).
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