Poster presented at the COST Action 539- ELENA, 3rd Workshop, Bled, Slovenia, September 2, 200

Gómez, Luz Stella

Marinković, Katarina

Martin, I.

Milošević, Olivera

Rabanal, Maria Eugenia

English

Serbian Academy of Science and Arts Digital Archive (DAIS)

Institute of Technical SciencesSerbian Academy of Sciences and ArtsUniversidad Carlos III de MadridStructural and Morphological Properties of Nanostructured Y2 O3 :Eu3+ Phosphor Particles Prepared Through Aerosol SynthesisXRD20 40 60 80 100Y1.9Eu0.1O3JCPDS 25-101162244040022222112000C11000C10000Cas prepared, 900OCIntensity, (a.u)2θ, 020 40 60 80 1 00Y 1.8E u 0.2O 3JC P D S 25-1 0116224404002222111 2 0 0 0C1 1 0 0 0C1 0 0 0 0Ca s p re p a re d , 9 0 0 0CIntesity,(a.u.)2 θ,0SEMY1.9 Eu0.1 O3 /9000CY1.8 Eu0.2 O3 /1000oCConclusionY2 O3 :Eu3+ particles produced via the aerosol route are on the submicronic level with spherical and filled morphology.All the samples, the as-prepared and thermally treated once, are composed of pure cubic Y2 O3 :Eu3+ phase (Ia3). The increase of lattice parameters, related to the incorporation of Eu3+ ions into the yttria host lattice is proved.    Microstructural parameters obtained through Rietveld refinement indicate the presence of nanostructures with crystallite size around 20nm. These results are in good agreement with TEM.Rougher particle surface evident in the thermally treated samples corresponds to larger primary crystallite size. Y1.8 Eu0.2 O3 /12000CAcknowledgements:The authors gratefully acknowledge the COST539-STSM02469  (K.Marinkovic), Ministry for Education and Science of Spain - Sabatic Grant SAB2004-0035 (O.Milosevic) and The Ministry of Science and Environment Protection, Republic of  Serbia (Project No. 142010). We thank Luis Puebla and Juan Luis Baldonedo from the Microscopy center "Luis Bru" of Universidad Complutense de Madrid, Spain for the  collaboration in TEM investigations.(Y0.95 Eu0.05 )2 O3-cubic system-space group: Ia3 (206)-lattice parameter: 10.604 K. Marinkovic1, M.E.Rabanal2, L. S. Gomez2, I. Martin2, O. Milosevic11Institute of Technical Sciences of Serbian Academy of Sciences and Arts, K.Mihailova 35/IV, 11000 Belgrade, Serbia 2Universidad Carlos III de Madrid, Avda. de la Universidad 30, 28911 Leganes, Madrid, SpainReferences[1] C.H. Lee, K.Y. Jung, J.G. Choi, Y.C. Kang, Mat. Sci. Eng., B 116 (2005) 59-63[2] O. Milosevic, L. Mancic, M.E. Rabanal, J.M. Torralba, B. Yang, P. Townsend, J. Electrochem. Soc., 152, (9) G707-G713(2005)Abstract Improved phosphor particles of Eu-doped yttrium oxide, a  well-known red phosphor, are employed in modern high-resolution display devices such as plasma display panels (PDP) and field  emission displays (FED) [1]. Utilization in such devices requires particles with spherical shape, fine size, narrow size distribution and non-aggregation characteristics since it ensures high resolution and high brightness [2]. Spray pyrolysis is a feasible method for obtaining the needed phosphor particle characteristics in view of the fact that when a precursor solution is atomized and fed into a furnace, solvent evaporation, drying, solute precipitation and  chemical decomposition occur successively on a droplet level, leading to the formation of particles with required compositional and structural characteristics. In this work yttrium oxide doped with europium (5 at% and 10 at%) was directly prepared by spray  pyrolysis at 900°C, additionally annealed and  characterized by means of XRD, SEM/EDS and TEM. The effects of different doping concentrations and synthesis parameters were monitored.Microstructural data from refinement by program Fullprof [3] and program Profit [4]86.84774.1723,77(±0.7)4,99(±1.3)10,621(4)10,608(5)120049.37845.5485,94(±1.3)5,99(±1.3)10,620(3)10,606(7)110032.43623.2929,72(±0.8)10,70(±1.4)10,620(2)10,605(1)100022.54819.04227,00(±1.9)18,70(±1.6)10,622(1)10,611(1)900S2S1S2S1S2S1cs, nmstraina, ÅTemperature, °CS1 – Y1.9 Eu0.1 O3 system; S2 – Y1.8 Eu0.2 O3 systemSEM images reveal that as-prepared particles are spherical, non- agglomerated and with smooth surface although  some particles with irregular morphology randomly appear.Y1.9 Eu0.1 O3 /11000CThermally treated samples show that the spherical particle morphology is maintained throughout the thermal treatment and that the higher temperature regime provokes further crystallization and growth of primary particles.COST 539 – 3WP ELENA 2007, September 2nd, Bled, SloveniaSpray pyrolysisPiezoelectric pellets f=1.3 MHzAir flow1 l/minY(NO3)3 x 6H2 O Eu(NO3)3 x 5H2 ONitrate precursor solutionzone II700 ºCzone I200 ºCzone III900 ºCIntraparticleReactionSolvent EvaporationDensificationDropletsDry particles Porous or hollow particlesSolid product particlesreactorPowder collection and additional thermaltreatment (1000- 1200°C for 12h)Characterization- XRD- (Fullprof, Profit)- SEM/EDS- TEMTEMNanostructures with crystallite size around 20 nm are in good agreement with XRD refinement. Low resolution transmission electron images of filled, spherical particles ranging between 130nm to 500nm are related to secondary nanoparticles.Y1.8 Eu0.2 O3 /9000CY1.8 Eu0.2 O3 /9000CPrimary particles with longer length in the range of 71.23± 18.4 nm can be resolved

Structural and Morphological Properties of Nanostructured Y2O3:Eu3+ Phosphor Particles Prepared Through Aerosol Synthesis

Gomez, Luz Stella

Digital Repository of the Institute of Technical Sciences of SASA

Institute of Technical Sciences
Serbian Academy of Sciences and Arts
Universidad Carlos III 
de Madrid
Structural and Morphological Properties of Nanostructured
 
Y2
 
O3
 
:Eu3+
 
Phosphor 
Particles Prepared Through Aerosol Synthesis
XRD
20 40 60 80 100
Y1.9Eu0.1O3
JCPDS 25-1011
62
244
0
40
0
22
2
22
1
12000C
11000C
10000C
as prepared, 900OC
In
te
ns
ity
, (
a.
u)
2θ, 0
20 40 60 80 1 00
Y 1.8E u 0.2O 3
JC P D S 25-1 011
62
244
0
40
0
22
2
21
1
1 2 0 0 0C
1 1 0 0 0C
1 0 0 0 0C
a s p re p a re d , 9 0 0 0C
In
te
si
ty
,(a
.u
.)
2 θ,0
SEM
Y1.9
 
Eu0.1
 
O3
 
/9000C
Y1.8
 
Eu0.2
 
O3
 
/1000oC
Conclusion
Y2
 
O3
 
:Eu3+
 
particles produced via the aerosol route are on the submicronic
 
level 
with spherical and filled morphology.
All the samples, the as-prepared and thermally treated once, are composed of 
pure cubic Y2
 
O3
 
:Eu3+
 
phase (Ia3). The increase of lattice parameters, related to 
the incorporation of Eu3+
 
ions into the yttria
 
host lattice is proved.    
Microstructural
 
parameters obtained through Rietveld
 
refinement indicate the 
presence of nanostructures with crystallite size around 20nm. These results are 
in good agreement with TEM.
Rougher particle 
surface evident 
in the thermally 
treated samples 
corresponds to 
larger primary 
crystallite size. 
Y1.8
 
Eu0.2
 
O3
 
/12000C
Acknowledgements:
The authors gratefully acknowledge the COST539-STSM02469
 
 
(K.Marinkovic), Ministry for Education and Science of Spain -
 
Sabatic
 
Grant SAB2004-0035 (O.Milosevic) and The Ministry of Science and 
Environment Protection, Republic of  Serbia (Project No. 142010). We 
thank Luis Puebla
 
and Juan Luis Baldonedo
 
from the
 
Microscopy center 
"Luis Bru" of Universidad Complutense
 
de Madrid, Spain
 
for the
 
 
collaboration in TEM investigations.
(Y0.95
 
Eu0.05
 
)2
 
O3
-cubic system
-space group: Ia3 (206)
-lattice parameter: 10.604 
K. Marinkovic1, M.E.Rabanal2, L. S. Gomez2, I. Martin2, O. Milosevic1
1Institute of Technical Sciences of Serbian Academy of Sciences and Arts, K.Mihailova 35/IV, 11000 Belgrade, Serbia 
2Universidad Carlos III de Madrid, Avda. de la Universidad 30, 28911 Leganes, Madrid, Spain
References
[1] C.H. Lee, K.Y. Jung, J.G. Choi, Y.C. Kang, Mat. Sci. Eng., B 116 (2005) 59-63
[2] O. Milosevic, L. Mancic, M.E. Rabanal, J.M. Torralba, B. Yang, P. Townsend, J. Electrochem. Soc., 152, (9) G707-G713(2005)
Abstract 
Improved phosphor particles of Eu-doped yttrium oxide, a
 
 
well-known red phosphor, are employed in modern high-resolution 
display devices such as plasma display panels (PDP) and field
 
 
emission displays (FED) [1]. Utilization in such devices requires 
particles with spherical shape, fine size, narrow size distribution 
and non-aggregation characteristics since it ensures high resolution 
and high brightness [2]. Spray pyrolysis is a feasible method for 
obtaining the needed phosphor particle characteristics in view of 
the fact that when a precursor solution is atomized and fed into
 
a 
furnace, solvent evaporation, drying, solute precipitation and
 
 
chemical decomposition occur successively on a droplet level, leading 
to the formation of particles with required compositional and 
structural characteristics. In this work yttrium oxide doped with 
europium (5 at% and 10 at%) was directly prepared by spray
 
 
pyrolysis at 900°C, additionally annealed and  characterized by 
means of XRD, SEM/EDS and TEM. The effects of different doping 
concentrations and synthesis parameters were monitored.
Microstructural
 
data from refinement by program Fullprof
 
[3] and program Profit [4]
86.84774.1723,77(±0.7)4,99(±1.3)10,621(4)10,608(5)1200
49.37845.5485,94(±1.3)5,99(±1.3)10,620(3)10,606(7)1100
32.43623.2929,72(±0.8)10,70(±1.4)10,620(2)10,605(1)1000
22.54819.04227,00(±1.9)18,70(±1.6)10,622(1)10,611(1)900
S2S1S2S1S2S1
cs, nmstraina, ÅTemperature, °C
S1
 
– Y1.9
 
Eu0.1
 
O3
 
system; S2
 
– Y1.8
 
Eu0.2
 
O3
 
system
SEM images reveal that 
as-prepared particles 
are spherical, non-
 
agglomerated and with 
smooth surface although  
some particles with 
irregular morphology 
randomly appear.
Y1.9
 
Eu0.1
 
O3
 
/11000C
Thermally treated samples 
show that the spherical 
particle morphology is 
maintained throughout the 
thermal treatment and 
that the higher 
temperature regime 
provokes further 
crystallization and growth 
of primary particles.
COST 539 –
 
3WP ELENA 2007, September 2nd, Bled, Slovenia
Spray pyrolysis
Piezoelectric 
pellets 
f=1.3 MHz
Air flow
1 l/min
Y(NO3)3
 
x 6H2
 
O 
Eu(NO3)3
 
x 5H2
 
ONitrate 
precursor 
solution
zone II
700 ºC
zone I
200 ºC
zone III
900 ºC
Intraparticle
Reaction
Solvent 
Evaporation
Densification
Droplets
Dry particles Porous or 
hollow particles
Solid product 
particles
reactor
Powder collection 
and additional 
thermal
treatment (1000- 
1200°C for 12h)
Characterization
- XRD
- (Fullprof, Profit)
- SEM/EDS
- TEM
TEM
Nanostructures with crystallite 
size around 20 nm are in good 
agreement with XRD refinement. 
Low resolution 
transmission electron 
images of filled, 
spherical particles 
ranging between 130nm 
to 500nm are related to 
secondary nanoparticles.
Y1.8
 
Eu0.2
 
O3
 
/9000C
Y1.8
 
Eu0.2
 
O3
 
/9000C
Primary particles with longer 
length in the range of 71.23± 
18.4 nm can be resolved


http://dais.sanu.ac.rs/bitstream/id/20716/305.pdf

Structural and Morphological Properties of Nanostructured Y2O3:Eu3+ Phosphor Particles Prepared Through Aerosol Synthesis

Abstract

Similar works

Full text

Available Versions

Serbian Academy of Science and Arts Digital Archive (DAIS)

Digital Repository of the Institute of Technical Sciences of SASA