Etude de la réactivité des dioxydes métalliques du groupe IVb en présence de carbone par une approche (micro)-structurale : Application à la modélisation des diagrammes de phases ternaires Me-C-O (où Me = Ti, Zr, Hf)

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groupe IVb en présence de carbone par une approche (micro)-structurale : Application à la modélisation des diagrammes de phases ternaires Me-C-O (où Me = Ti,

Zr, Hf)

Florian Réjasse

To cite this version:

Florian Réjasse. Etude de la réactivité des dioxydes métalliques du groupe IVb en présence de carbone par une approche (micro)-structurale : Application à la modélisation des diagrammes de phases ternaires Me-C-O (où Me = Ti, Zr, Hf). Matériaux. Université de Limoges, 2015. Français. �NNT : 2015LIMO0099�. �tel-01271089�

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Université de Limoges

École Doctorale Sciences et Ingénierie en Matériaux, Mécanique, Énergétique et Aéronautique (ED 522)

Laboratoire Sciences des Procédés Céramiques et Traitements de Surface Thèse pour obtenir le grade de

Docteur de l’Université de Limoges

Discipline / Spécialité : Matériaux céramiques et traitements de surface Présentée et soutenue par

Florian Réjasse

Le 2 décembre 2015

Etude de la réactivité des dioxydes métalliques du groupe IVb en présence de carbone par une approche (micro-)structurale – Application à la modélisation des diagrammes de phases ternaires Me-C-O (où Me = Ti, Zr, Hf)

Thèse co-dirigée par Alexandre Maître et Gilles Trolliard et encadrée par Olivier Rapaud

JURY :

Président du jury

M. LOISEAU Thierry – Directeur de Recherche – UCCS – Université de Lille Rapporteurs

MME. GUENEAU Christine – Ingénieur HDR – CEA Saclay

M. HEINTZ Jean Marc – Professeur – ICMCB – Université de Bordeaux Examinateurs

M. MAÎTRE Alexandre – Professeur – SPCTS – Université de Limoges M. TROLLIARD Gilles – Professeur – SPCTS – Université de Limoges

M. RAPAUD Olivier – Maître de Conférence – SPCTS – Université de Limoges

Thèse de doctorat

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INTRODUCTION GENERALE ... 17

CHAPITRE 1. SYNTHESE BIBLIOGRAPHIQUE ... 21

I PROPRIETES PHYSICO-CHIMIQUES ET STRUCTURALES DES SYSTEMES TI-C-O, ZR-C-O ET HF-C-O ... 21

I.1 PROPRIETES PHYSICO-CHIMIQUES DES CARBURES DU GROUPE IVB ... 22

I.2 PROPRIETES STRUCTURALES ... 23

I.2.1 Les carbures du groupe IVb ... 23

I.2.2 Les oxycarbures du groupe IVb ... 26

I.2.3 Le dioxyde de titaneet les phases de Magnéli ... 29

I.2.4 Le dioxyde de zirconium ... 32

I.2.5 Le dioxyde d’hafnium ... 33

II REACTIVITE DES PHASES OXYDES ET DES CARBURES DES METAUX DE TRANSITION DU GROUPE IVB .... 34

II.1 REACTIVITE DU SYSTEME TI-C-O ... 35

II.1.1 La réduction carbothermique du dioxyde de titane ... 35

II.1.2 L’oxydation du carbure de titane ... 38

II.2 REACTIVITE DU SYSTEME ZR-C-O ... 41

II.2.1 La réduction carbothermique de la zircone ... 41

II.2.2 La réaction ZrC/ZrO2 ... 43

II.2.3 L’oxydation du carbure de zirconium ... 45

II.3 REACTIVITE DU SYSTEME HF-C-O ... 47

II.3.1 La réduction carbothermique de l’hafnie ... 47

II.3.2 L’oxydation du carbure d’hafnium ... 48

III DEMARCHE SCIENTIFIQUE ... 49

CHAPITRE 2. METHODES EXPERIMENTALES... 57

I PRESENTATION DES METHODES DE CARACTERISATION PHYSICO-CHIMIQUES ... 57

I.1 DIFFRACTION DES RAYONS X ... 57

I.1.1 Principe général ... 57

I.1.2 Instrumentation ... 57

I.1.3 Position des raies de diffraction ... 58

I.1.4 Profils et largeurs des raies ... 59

I.1.5 Simulations des diagrammes et affinements de paramètres de maille ... 61

I.2 LA MICROSCOPIE ELECTRONIQUE ... 62

I.2.1 L’interaction électron-matière ... 62

I.2.2 La Microscopie Electronique en Transmission : MET ... 62

I.2.2.1 Préparation des échantillons ... 63

I.2.2.2 Imagerie conventionnelle ... 64

I.2.2.3 La diffraction électronique ... 64

I.2.3 La microscopie électronique à balayage (MEB) ... 64

I.3 ANALYSE CHIMIQUE ELEMENTAIRE ... 64

I.3.1 Dosage du carbone ... 64

I.3.2 Dosage de l’oxygène... 65

II SYNTHESE DES POUDRES DE CARBURE ET D’OXYCARBURE PAR REDUCTION CARBOTHERMIQUE ... 66

II.1 DEMARCHE EXPERIMENTALE ET PROTOCOLE DE SYNTHESE ... 66

II.2 CARACTERISATION DE LA POUDRE DE NOIR DE FUMEE ... 68

II.3 LE SYSTEME ZRO2-C ... 69

II.3.1 La poudre de zircone de départ ... 69

II.3.2 Traitements thermiques appliqués ... 70

II.4 LE SYSTEME HFO2-C ... 72

II.4.1 La poudre d’hafnie de départ ... 72

II.4.2 La cinétique de la réaction ... 75

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II.5.2 Traitements thermiques appliqués ... 78

III CONDITIONS D’ETUDE DES REACTIONS MEO2/MEC ... 79

III.1 ELABORATION DES MONOLITHES DE CARBURE DE TITANE ET DE DIOXYDE DE TITANE ... 80

III.1.1 Principe général du procédé de frittage flash ... 80

III.1.2 Frittage SPS du carbure de titane ... 82

III.1.3 Frittage du dioxyde de titane ... 83

III.2 TRAITEMENT DE RECUIT ... 84

III.2.1 Recuits par traitement thermique classique... 84

III.2.2 Recuit par fritttage sous charge : Hot Pressing ... 85

CHAPITRE 3. ETUDE DE LA REACTIVITE DES OXYDES ET DES CARBURES DU GROUPE IVB ... 89

I LES SYSTEMES ZR-C-O ET HF-C-O ... 90

I.1 ETUDE DES MECANISMES REACTIONNELS DE LA REDUCTION CARBOTHERMIQUE DE L’HAFNIE ET COMPARAISON AVEC CEUX MIS EN JEU LORS DE LA REDUCTION CARBOTHERMIQUE DE LA ZIRCONE ... 90

I.1.1 Le système HfO2-C ... 90

I.1.1.1 Etude de la réaction par diffraction des rayons X ... 90

I.1.1.2 Etude structurale des mécanismes réactionnels par microscopie électronique en transmission ... 93

I.1.2 Le système ZrO2-C ... 100

I.2 LE MECANISME REACTIONNEL GENERALISE DE LA REDUCTION CARBOTHERMIQUE D’OXYDES DU GROUPE IVB DE STRUCTURE MONOCLINIQUE ... 101

I.3 ETUDE DES DOMAINES DE STABILITE DES SOLUTIONS SOLIDES DES OXYCARBURES DE ZIRCONIUM ET D’HAFNIUM ... 105

I.3.1 Le système Zr-C-O ... 106

I.3.1.1 Caractérisations structurales ... 106

I.3.1.2 Caractérisations morphologiques ... 109

I.3.1.3 Caractérisations chimiques ... 111

I.3.1.4 Evolution structurale ... 114

I.3.1.5 Discussion ... 115

I.3.2 Le système Hf-C-O ... 117

I.3.2.1 Caractérisations structurales ... 117

I.3.2.2 Caractérisations morphologiques ... 119

I.3.2.3 Caractérisations chimiques ... 121

I.3.2.4 Evolution structurale ... 122

I.3.2.5 Discussion ... 123

II LE SYSTEME TI-C-O ... 125

II.1 LE SYSTEME PULVERULENT ... 125

II.1.1 La réduction carbothermique ... 125

II.1.2 Etude du domaine de stabilité de la solution solide d’oxycarbure de titane ... 125

II.1.2.1 Caractérisations structurales ... 125

II.1.2.2 Caractérisations morphologiques ... 128

II.1.2.3 Analyses chimiques ... 130

II.1.2.4 Evolution structurale ... 131

II.1.2.5 Discussion ... 132

II.2 LE SYSTEME MASSIF / ASSEMBLAGE REACTIONNEL ... 135

II.2.1 Caractérisations structurales... 137

II.2.2 Caractérisations microstructurales ... 141

II.2.3 Discussion ... 149

III CONCLUSION ... 153

CHAPITRE 4. ETUDE THERMODYNAMIQUE DES SYSTEMES TERNAIRES ME-C-O ... 157

I LA MODELISATION THERMODYNAMIQUE PAR LA METHODE CALPHAD ... 157

I.1 PRINCIPE DE LA METHODE CAPHAD ... 158

I.2 CHOIX DES MODELES THERMODYNAMIQUES ... 159

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I.3.3 Description des solutions ... 161

I.3.3.1 Les solutions de substitution désordonnées ... 161

I.3.3.2 La description des composés et solutions solides ordonnées ... 163

I.3.3.3 Le modèle associé ... 165

I.3.3.4 Les modèles ioniques ... 166

I.4 LA NOTATION DES STRUCTURES CRISTALLOGRAPHIQUES ... 167

I.5 PREVISION THERMODYNAMIQUE DES EQUILIBRES ET REPRESENTATION PAR LE CALCUL D’UN DIAGRAMME DE PHASES ... 169

II SYNTHESE DES ETUDES THERMODYNAMIQUES MENEES DANS LA LITTERATURE SUR LES SYSTEMES BINAIRES O-M ET C-M ... 170

II.1 LE SYSTEME C-O-ZR ... 170

II.1.1 Le diagramme binaire C-Zr ... 170

II.1.2 Le diagramme binaire O-Zr ... 173

II.2 LE SYSTEME C-HF-O... 175

II.2.1 Le diagramme binaire C-Hf... 175

II.2.2 Le diagramme binaire Hf-O ... 177

II.3 LE SYSTEME C-O-TI ... 179

II.3.1 Le diagramme binaire C-Ti ... 179

II.3.2 Le diagramme binaire O-Ti ... 181

III EXTRAPOLATION DES SYSTEMES BINAIRES DANS UN SYSTEME TERNAIRE ... 185

III.1 DEMARCHE SCIENTIFIQUE ... 185

III.2 PROCEDURE D’OPTIMISATION ... 186

III.3 MODELISATION DU SYSTEME TERNAIRE C-O-ZR ... 186

III.4 MODELISATION DU SYSTEME TERNAIRE C-HF-O ... 190

III.5 MODELISATION DU SYSTEME TERNAIRE C-O-TI ... 192

IV CONCLUSION ... 196

CONCLUSION GENERALE ... 201

REFERENCES BIBLIOGRAPHIQUES ... 207

ANNEXE 1 ... 217

ANNEXE 2 ... 218

ANNEXE 3 ... 219

ANNEXE 4 ... 220

ANNEXE 5 ... 221

ANNEXE 6 ... 223

ANNEXE 7 ... 224

ANNEXE 8 ... 228

ANNEXE 9 ... 233

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