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Propriétés Structurales, Vibrationnelles Et Diélectriques De Matériaux À Base D’Oxyde De Tellure

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Propriétés Structurales, Vibrationnelles Et Diélectriques De Matériaux À Base D’Oxyde De Tellure UNIVERSITE DE LIMOGES Faculté des Sciences et Techniques Ecole Doctorale Science Technologie Santé Laboratoire Science des Procédés Céramiques et Traitements de Surface (SPCTS-UMR-6638-CNRS). N°38-2003 THESE Pour obtenir le grade de DOCTEUR DE L’UNIVERSITE DE LIMOGES Discipline : Matériaux Céramiques et Traitements de Surface Présentée et soutenue publiquement par Olivier NOGUERA Le 4 novembre 2003 Propriétés structurales, vibrationnelles et diélectriques de matériaux à base d’oxyde de tellure. Directeurs de Thèse : Thérèse MERLE-MEJEAN, Professeur, IUFM Limoges Andreï MIRGORODSKY, Professeur, Université de Limoges Rapporteurs : Alain BULOU, Professeur, Université du Maine, Le Mans Patrick SIMON, Directeur de Recherche, CNRS, CRMHT Orléans Examinateurs : Jean-François BAUMARD, Professeur, ENSCI Limoges Jean-Claude CHAMPARNAUD-MESJARD, Professeur, Université de Limoges Olivier MASSON, Maître de Conférence, Université de Limoges Mikhaïl SMIRNOV, Chercheur, Université de Saint-Pétersbourg (Russie) Philippe THOMAS, Chargé de Recherche, CNRS, SPCTS Limoges Invité : Bernard FRIT, Professeur en retraite, Université de Limoges Remerciements Ce travail de recherche fut réalisé à l’Université des Sciences et Techniques de Limoges et plus particulièrement dans le laboratoire Sciences des Procédés Céramiques et Traitement de Surface (SPCTS, UMR 6638 CNRS) dirigé par le professeur Jean-François BAUMARD. Qu’il soit assuré de ma respectueuse reconnaissance pour m’avoir accueilli au sein de son laboratoire et pour avoir présidé ce jury. De la même façon je suis reconnaissant à la région LIMOUSIN qui a bien voulu financer ce travail de recherche. Je remercie également messieurs Alain BULOU, professeur à l’Université du Maine, et Patrick SIMON, Directeur de Recherche au Centre de Recherche sur les Matériaux à Hautes Températures d’Orléans (CRMHT, UPR 4212 CNRS), d’avoir accepté de juger ce travail. Je tiens aussi à remercier madame Thérèse MERLE-MEJEAN, Professeur à l’IUFM de Limoges, et monsieur Andreï MIRGORODSKY, professeur à l’Université des Sciences et Techniques de Limoges, qui ont su trois années durant me faire partager leur connaissance de la spectrométrie vibrationnelle et de la chimie des matériaux et égayer ce travail de quelques anecdotes savoureuses. Ces sincères remerciements s’adressent aussi à Phiphi qui fut de bons conseils le cas échéant, notamment en ce qui concerne les questions oenologiques, et à Micha, chercheur à l’université de Saint-Pétersbourg (Russie), pour, outre ses compétences en modélisation des spectres vibrationnels et en calculs ab initio, sa fameuse vodka. D’autre part, ce travail s’est déroulé dans un laboratoire où une multitude de personnes se croisent tous les jours et je souhaiterais rendre hommage à tous ces gens, et bien plus encore à certaines, qui ont rendu fort agréable mon passage au laboratoire et qui auront contribué à la réussite grandiose de ce travail. Enfin, je voudrais témoigner toute ma reconnaissance et adresser mes plus vifs remerciements à Rantanplan. 2 Résumé en français Les verres des matériaux à base d’oxyde de tellure présentent des propriétés d’optique non linéaire exceptionnelles. Afin de déterminer l’origine de ces propriétés, il est nécessaire de procéder à une étude systèmatique et fondementale des caractéristiques structurales, spectrochimiques et dynamiques de ces matériaux. Pour cette étude, tout en nous appuyant sur des résultats de diffraction des rayons X antérieurs, la spectrométrie vibrationnelle (diffusion Raman et absorption infrarouge) a été privilegiée. Nous avons étudié les différentes variétés polymorphiques du dioxyde de tellure (paratellurite TeO 2-α, tellurite TeO 2-β et TeO 2-γ) et des matériaux à base d’oxyde de tellure comportant des cations de valences différentes (I, II et IV). Il ressort de cette étude que l’environnement des atomes de tellure subit des modifications plus ou moins importantes selon la nature du cation ajouté. L’ensemble des réseaux cristallins est construit à partir de deux briques élémentaires pouvant s’associer pour 2- former des anions complexes : des molécules TeO 2 et des ortho-anions [TeO 3] . Ces briques élémentaires sont retrouvées dans les réseaux vitreux et la présence d’une immisciblité dans les verres de tellurites comportant un cation faible est suggérée. L’énergie de formation et les géométries d’équilibres de polymères (TeO 2)n (n=2-6) simulés par calculs ab initio sont présentées ainsi que l’évaluation de l’hyperpolarisabilité de ces polymères. Bien que nous n’en soyons qu’à la phase préliminaire de cette étude, il semble que la paire libre (5s 2) des atomes de tellure ne puisse expliquer à elle seule les propriétés d’optique non linéaire extraordinaires des matériaux à base d’oxyde de tellure. Mots clés : dioxyde de tellure, tellurites, spectrométries vibrationnelles, verres, modélisation, calculs ab initio. 3 Abstract Owing to some remarkable properties the tellurium oxide based materials attract considerable attention from both fundamental and engineering sides. In particular, the tellurium oxide based glasses present the highest non-linear susceptibility among the known glasses. In order to determine the origin of these properties, we must realize a systematic and fundamental study of the structural, spectrochemical and dynamic caracteristics of these materials by means of vibrational spectroscopy (Raman diffusion and infrared absorption) with respect of the X-ray results. The structural and vibrational study of the tellurium dioxide polymorphs (paratellurite α-TeO 2, tellurite β-TeO 2 and γ-TeO 2) and tellurite materials indicate that the short order atomic arrangement evolution is related to the cation valences. The cristalline networks are built up from two structural fragments : the TeO 2 molecules and 2- 2k- the [TeO 3] ortho-anions which can be associated to form complex anions [Te nOm] . These fragments are also observed in the glassy networks but not the complex anions. Immiscibility effects are suggested to be inherent in tellurites glasses with weak cations. Equilibrium geometry, spectroscopic spectra and dielectric properties of polymer molecules (TeO 2)n (with n=2-6) were studied within ab initio calculations. It appears that the electronic lone pair is not the only parameter which explains the extraordinary non-linear susceptibility of the tellurium oxide based materials. Key words : tellurium dioxide, tellurites, vibrational spectroscopy, glasses, modelisation, ab initio calculations. 4 Table des matières Introduction générale. ................................................................................................ 20 Première partie : Généralités, Techniques expérimentales & Méthodes de modélisation et de simulation..................................................................................... 25 A. Produits de départ. .............................................................................................................. 26 1. Le dioxyde de tellure : TeO 2.............................................................................................. 26 a) Rappels. ........................................................................................................................... 26 b) Expérimental. .................................................................................................................. 27 2. Les oxydes métalliques...................................................................................................... 28 a) Le monoxyde de zinc (ZnO). .......................................................................................... 28 b) Le monoxyde de plomb (PbO). ....................................................................................... 28 c) Le dioxyde de titane (TiO 2). ............................................................................................ 28 d) Le dioxyde d’étain (SnO 2). .............................................................................................. 29 e) La zircone (ZrO 2). ........................................................................................................... 29 3. Le carbonate de thallium. .................................................................................................. 29 B. Conditions de synthèse. ...................................................................................................... 29 1. Préparations des phases définies du système TeO 2-Tl 2O. ................................................. 29 2. Préparations des phases définies du système TeO 2-ZnO................................................... 30 3. Préparations de la phase Pb 2Te 3O8. ................................................................................... 30 4. Préparations des phases MTe 3O8 (M=Ti, Sn et Zr). .......................................................... 30 5. Préparations des compositions vitreuses. .......................................................................... 31 C. Méthodes d’analyses........................................................................................................... 31 1. Caractérisation structurale. ................................................................................................ 31 2. Spectroscopie vibrationnelle.............................................................................................. 32 a) Diffusion Raman. ............................................................................................................ 33 (i) Description classique.............................................................................................................
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