Laboratoire des Matériaux Inorganiques - UPRES A-6002 Université Blaise Pascal - Aubière
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1 IFLUECE F GRUPS TE SPECTRAL CARACTERISTICS F Eu 3+ IS I YBRID RGAIC-IRGAIC MATERIALS SUTESIZED BY SL-GEL A.C FRAVILLE, D. ZAMB, R. MAIU Laboratoire des Matériaux Inorganiques - UPRES A-62 Université Blaise Pascal - Aubière
2 BJECTIVES Components of igh Emission Yield Rare Earth organic Complexes (Ln 3+ = Eu 3+, Tb 3+ ) igh Emission Yield under UV excitation Low Thermal and Mechanical resistance YBRID MATERIALS PWDERS AD FILMS Applications Lighting Displays marking
3 MATERIAL rganic Complexes of Europium and Terbium Sol-Gel made lica network Covalent bonding Luminescent ybrid materials of Class II
4 rganic Complexes of Europium and Terbium Eu 3+, Tb 3+ arrow emission bands Long lifetime TRASFER EERGY MECAISM rganic Ligand Large absorption bandwidth and high Intensity in the UV-Visible range Protected environment Energy transfer yield high S 1 T 1 S 1 BTC T 1 5 D 4 25 cm cm -1 5 D F P F P S Ligand Eu 3+ S Ligand Tb 3+ F P Absorption Fluorescence Phosphorescence o radiative transfer Emission Yield = Absorption efficiency Transfer energy efficiency Ln 3+ ligand Fluorescence efficiency
5 Association Mode CLASS II YBRIDS Strong chemical interactions of covalent or ionic-covalent nature Inorganic network rganic component Composite at the molecular level Increased Chemical Thermal and Mechanical stability rganic- Inorganic Interface precisely defined ADVATAGES igh level doping Isolation of active species ngle phase material omogeneous distribution of the emitting centers : ICREASES TE RADIATIVE RELAXATI PRCESS
6 SYTESIS rganic Chromophore Precursors 1. Bonding C l C Bonding C C l E t E t E t Functionalized monomer E t E t E t E t E t E t 2. Complexation Monomer M1a 3 C C 3 3. ydrolysis/condensation rganic Ligand 1a Luminescent ybrid Characterization - RM 1 / 13 C - Infra Red - Mass Spectroscopy - Molecular Modeling Total bonding reaction Monomer and ligand structure similar
7 STRUCTURE AD TEXTURE Eu 3+ Eu 3+ Eu 3+ Eu 3+ = Amorphous Materials Monolithic Gels (paque and Transparent) omogeneous texture Conservation of the electronic structure of the luminophore Conservation of the coordination mode of Ln 3+ Double covalent bonding ngle phase material with homogeneous distribution of organic and inorganic components
8 Position of triplet and singlet states Absorption of gels and free ligands Phosphorescnce Emission 1 * : 2λ du laser * T = 15 K λexc = 29, nm délai = 1 µs 8 % réflexion (u.a) 6 4 1a 1a Gd1a transition - 2 π π * Gd1a Absorption of hybrids and organic complexes 1 organic hybrid 8 S 1 Free ligand 292 nm (34247 cm -1 ) 294 nm (3414 cm -1 ) % réflexion (u.a.) 6 4 Gd1a Gd1a S 1 Gd complex 29 nm (34483 cm -1 ) 288 nm (34722 cm -1 ) 2 π π * T 1 Gd complex 362 nm (27624 cm -1 ) 369 nm (271 cm -1 )
9 Fluorescence sensitization of Eu 3+ ortb 3+ ions Excitation spectra of fluorescence 5 D fi 7 F 2 de l ion Eu 3+ Emission spectrum of Eu 3+ ion under UV excitation S S 1 T = 15 K λem = 616, nm émission de Eu1a T =15 K λexc = 337,1 nm délai = 75 µs Eu1a Eu1a (2) (1) (3) (1) 7 F 5 D 4 - (2) 7 F 5 L 6 - (3) 7 F 5 D 2 3 Energie (cm -1 ) λ max excitation 292 nm Eu1a 25 5L 6 5D 3 5D nm Eu1a D 2 5D 1 5D 5D 4 Conservation of the energy transfer mechanism 1 5 7F J F J Eu 3+ Tb 3+
10 Emission properties of Eu 3+ Emission spectra under UV excitation Infuence of the Sol-Gel matrix 5D 7F 2 T = 15 K λ exc = nm délai = 75 µs Shift of 5 D level towards high energies ν = 18 cm -1 7F 7 F 1 level splitting more important 5D 7F 1 5D 5D 7F 3 5D 7F 4 Eu1aT5 Energie (cm -1 ) 1692 Eu1a Eu1a , 16842, , Eu1a Eu1a Eu1aT5 Amorphous in character 5 D 7 F 2 (616, nm) transition predominates Enlargement of the transition 5 D 7 F 2 1/2 = 76 cm -1 Eu1a 17 cm -1 Eu1a
11 Lifetime and emission yield Fluorescence decays Emission yield,1 λ exc = nm λ em = 616. nm T = 15 K 12 1E-3 Eu1a 1 1E-4 8 Eu1a Log (I) 1E-5 1E-6 Eu1a 6 4 Eu1a Eu1aT1 Eu1aT2 Eu1aT5 Eu1aT1 Eu1aT2 1E Time (ms) % 2 increasing at 15 K at 3 K Eu1a Eu1a 1,22 ms 1,6 ms,85 ms Limited effect of groups
12 Selective Excitation Excitation spectra 7 F fi 5 D of 5 D fi 7 F 2 fluorescence at 15 K Emission spectra of Eu1a by selective excitation of sites A and B à 15 K Eu1a site A Eu1a - λem = 616, nm * raie laser site B * * site B lexc = 58,8 nm Eu1a- λem = 613,5 nm site A lexc = 58, nm Energie (cm -1 ) Energy (cm -1 ) D 1/2 (cm -1 ) Eu1a , Eu1a (site A) ,2 Eu1a (site B) ,2 2 Distinct distribution of sites and not connected between them.
13 rigin of the 2 distribution of sites 5 D 7 F 12 Lifetime site B λexc = 58,8 nm,1 1E-3 site B λexc = 58,8 nm λem = 615,5 nm site A λexc = 58, nm barycentre 7 F 1 (site A) = 16863,2 cm -1 (site B) = 16842,4 cm -1 Intensité (u.a.) 1E-4 1E-5 site A λexc = 58, nm λem = 613,5 nm 5 D 7 F 2 site B λexc = 58,8 nm 1E-6,,5 1, 1,5 2, 2,5 3, Temps (ms) t (site A) =,9 ms (site B) = 1,18 ms site A λexc = 58, nm D 1/2 (site A) = 15 cm -1 (site B) = 17 cm -1 te A with te B without UV EXCITATI SITE B
14 CRMPRE MDIFICATI Absorption cross section Energetic position of the triplet state C C C + 2,6-dicarboxy-4-phényl-pyridine acide 2 + C C C C 2,6-dicarboxy-4-phényléthynyl-pyridine acide 3 Br Br + CEt C C 2,6-di(3'-carboxypyrazolyl)-pyridine acide 4
15 Chromophore energy levels Excitation spectra of fluorescence 5 D fi 7 F 2 (Eu 3+ ) 294 nm 335 nm 338 nm 37 nm T = 15 K λem = 616, nm Eu1a Eu2a Eu3a Eu4a S 1 et T 1 levels position measured on Gd hybrid complexes S 1 T 1 Gd1a cm cm -1 (288 nm) (369 nm) Gd2a 333 cm cm -1 (33 nm) (434 nm) Gd3a cm cm -1 (358 nm) (465 nm) Gd4a cm cm -1 (336 nm) (396 nm) 2a 3a 4a
16 coupling effects Excitation spectra of 7 F fi 5 D (lem = 616, nm, T = 15 K) 5 D levels lifetime (λexc = 337,1 nm - T = 15 K) Eu4a Eu3a Eu2a Eu1a Europium Complexes organic hybrid Eu()1a 1,22 ms 1,6 ms Eu()2a,88 ms,68 ms Eu()3a,75 ms,69 ms Eu()4a 1,15 ms,64 ms te A te B energy 1/2 energy 1/2 (cm -1 ) (cm -1 ) (cm -1 ) (cm -1 ) Eu1a , ,2 Eu2a , ,1 Eu3a , ,4 Eu4a , ,5
17 Photoluminescence Yield Europium Complexes S 1 λexc = 337,1 nm 3 S 1 S T 1 S 1 T 1 5 L 6 5D Energie (cm-1) T 1 T 1 5 D 2 5D 1 5D 2 5 Eu1a Eu2a Eu3a Eu4a Eu1a Eu2a Eu3a Eu4a
18 DrTGA (mg/min) TGA-DTA AALYSIS Thermal stability gain from 115 C to 15 C, 35 -, ,2 -,3 71 C 254 C Température ( C) ,4 45 C Température ( C) % massique C,5 12 8, 1 TGA (%) Eu1a Eu1a 185 C -,5 -,1 -,15 -,2 DrTGA (mg/min) Eu1a Eu1a Eu1aT1 Eu1aT2 Eu1aT5 Eu1aT1 Eu1aT2 -, Temperature ( C) 2 % 2 increasing
19 SUMMARY rganic-inorganic Luminescent ybrids Sol-Gel Synthesis Covalent bonding Emission Properties Sol-Gel matrix effects (, ) UV sensitization mechanisms Potential Applications Luminescence Yield preserved Thermal resistance improved
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