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S?ntese e caracteriza??o de rutenato de b?rioVital, Ang?lica Belchior 29 January 2015 (has links)
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Previous issue date: 2015-01-29 / Coordena??o de Aperfei?oamento de Pessoal de N?vel Superior (CAPES) / Compostos contendo rut?nio
possuem vasta aplica??o
em processos
catal?ticos. Muitas vezes esse metal ?
utilizado
em ?xidos porosos
, suporte,
com alta
estabilidade t?rmica. Os ?xidos mistos do tip
o perovskita (ABO
3
) apresentam boa
dispers?o met?lica
, elevada estabilidade t?rmica e qu?mica, sendo empregados em
processos oxidativos
. Em vista disso, este trabalho teve como objetivo principal
sintetizar e caracterizar o
catalisador de
rutenato de b?rio
(BaRuO
3
) com estrutura do
tipo perovskita. Para isso, foram utilizadas duas metodolog
ias de s?ntese
de BaRuO
3
, a
complexa??o combinada EDTA
-
Citrato e a coprecipita??o em meio oxalato. BaRuO
3
produzido passou por tratamentos t?rmicos a 950?C por 5, 10 e 15
horas.
O precursor
foi utilizado
na an?lise termogravim?trica (TG) para avaliar a estabilidade t?rmica, e os
p?s cer?micos
calcinados
foram caracterizados por:
difra??o de raios X (DRX) para
identifica??o
das fases formadas
, an?lise estrutural e avalia??
o do tamanho m?dio de
cristalitos; microscopia eletr?nica de varredura (MEV) para observa??o da morfologia;
espectroscopia de energia dispersiva (EDS) para determina??o da composi??o qu?mica
local. Observou
-
se que pela metodologia EDTA
-
Citrato o BaRuO
3
apr
esentou estrutura
rombo?drica com o grupo espacial R
-
3mH (ICSD:
10253) com morfologia heterog?ne
a
e com larga distribui??o de tamanho de cristais. Por outro lado, o ?xido sintetizado pelo
m?todo
de
coprecipita??o apresentou dois polimorfos, um com estrutura
hexagonal com
o grupo e
spacial P63/mmc (ICSD:84652) e
outro rombo?drico (ICSD:10253), com
morfologia homog?nea e maior controle de distribui??o de cristais. / Ruthenium compounds are widely use
d in catalytic processes. Often this
metal
is supported on porous oxides having high thermal stability.
Perovskite
-
type
o
xides
(ABO
3
) have good metal dispersion
,
high
thermal and chemical s
tability, it are
used in
oxidative processes
.
T
his study aimed
to synthesize and characterize
barium
ruthenate
(BaRuO
3
) with perovskite
-
type structure. For this, two methods
for
BaRuO
3
synthesis
have been used
,
combined complexation EDTA
-
Citrate
and oxalat
e coprecipitation.
BaRuO
3
produced underwent heat treatment at 950 ? C for 5, 10 and 15 hours.
The
precursor was used in thermogravimetric analysis (TG) to evaluate thermal stability
,
ceramic powders obtained were characterized by X
-
ray diffraction (XRD) t
o identify
the phases, structural analysis and assessment of the average size of crystallites;
scanning electron microscopy (SEM) to observe the morphology; energy dispersive
spectroscopy (EDS) to determine local chemical composition. It was observed that
BaRuO
3
for
EDTA
-
citrate methodology presented rhombohedral structure with space
group R
-
3mH (
ICSD
: 10253) heterogeneous morphology with a broad distribution and
crystal size.
thereby
, the oxide synthesized by
oxalate
coprecipitation method presented
two po
lymorphs, with hexagonal
structure with space group P63/
mmc (
ICSD
: 84652)
and a rhombohedral (
ICSD
: 10253) with homogeneous morphology and crystals
distribution control.
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Caractérisations cristallographiques et magnétiques de nouvelles phases oxygènées a base de ruthénium. Filiations structurales avec les perovskitesDussarrat, Christian 22 July 1996 (has links) (PDF)
L'investigation du système BaBiO3-BaRuO3 a permis de mettre en évidence trois nouvelles phases qui cristallisent dans trois différents polytypes de la perovskite. L'interprétation des propriétés magnétiques de ces phases, ainsi que des considérations cristallochimiques, montrent qu'il s'établit un phénomène de transfert de charge entre le ruthénium et le bismuth selon le schéma réactionnel: 2 Ru4+ + Bi5+->2 Ru5+ + Bi3+. L'activité catalytique de ces composés pour la réduction de NO a été étudiée. Cinq nouveaux composés ont ete isoles dans le système Ba(Sr)-Ru-O. Leurs structures sont caractérisées par des groupements [Ru3O12] ou [Ru2O9], formant des systèmes de basse dimensionnalité (clusters, système 2D). Des modèles structuraux ont été développés et ont permis d'établir des filiations structurales avec des structures type telles que K2NiF4, la perovskite 2H et Sr4PtO6. Les propriétés magnétiques ont été étudiées et pour certaines phases, interpretées en termes d'entités isolées selon un modèle d'Heisenberg.
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