19º Congresso Brasileiro de Engenharia e Ciência dos Materiais – CBECiMat, 21 a 25 de novembro de 2010, Campos do Jordão, SP, Brasil

YTTRIUM ALUMINUM GARNET (YAG) OBTAINED BY RARE-EARTH MIXED

OXIDE (RE2O3)

D. F. Castro1, C. Santos1,4*, J. K. M. F. Daguano1, D. Rodrigues Jr1.,

P.A. Suzuki1,2, O.M.M. Silva3
1*
Universidade de São Paulo - Escola de Engenharia de Lorena (USP - EEL)
Polo Urbo-industrial, gleba AI-6, s/n, CEP 12600-970, Caixa Postal 116, Lorena - SP,
Brazil.
2
Laboratório Nacional de Luz Síncrotron (LNLS)
3
Centro Técnico Aeroespacial – Divisão de Materiais (CTA-IAE-AMR)
4
Centro Universitário de Volta Redonda (UNIFOA-MEMAT)
claudinei@demar.eel.usp.br

ABSTRACT
In this work, the substitution of commercial Y2O3 by a rare earth mixed oxide, RE2O3,
to form Yttrium aluminum Garnet-Y3Al5O12, was investigated. Al2O3:Y2O3 and
Al2O3:RE2O3 powder-mixtures, in a molar ratio of 60:40, were milled and
subsequently cold uniaxialy-pressed. Compacts were sintered at 1000, 1400 or
16000C, for 120 minutes. RE2O3 oxide was characterized by high-resolution
synchrotron X-ray diffraction (HRXRD) and compared to Y2O3. X-ray diffraction
pattern of the RE2O3 indicates a true solid solution formation. Rietveld refinement of
the sintered YAG and (RE)AG reveled a similar crystal structure to the YAGs
obtained by the use of Al2O3-Y2O3 or Al2O3-RE2O3 respectively. Microstructural
analysis of both, YAG or (RE)AG, revealed similar grain sizes of about 2.5μm
besides mechanical properties, with hardness of 400HV and fracture toughness of
3.8MPa.m1/2. It could be, thus, demonstrated that pure Y2O3 can be substituted by
the rare-earth solid solution, RE2O3, in the formation YAGs, presenting similar
microstructural and mechanical properties.
Key-words: ceramics, Y3Al5O12; rare-earth oxides; characterization, X-ray diffraction

INTRODUCTION
Yttrium aluminum garnet, YAG, have been very investigated because to its
optical and mechanical properties(1-4). Furthermore, this oxide is very used as
intergranular phase for sintering of SiC and Si3N4 ceramics(5-7). The presence of
intergranular phases rich in YAG leads to improvement of mechanical properties,
such as bending strength and fracture toughness, maintaining high oxidation and
creep resistance at high temperatures(8,9). Furthermore, YAG ceramics is know by the
its good optical properties because of transparence and presence of bands of
(2-4,10,11)
emission when doped with rare earth, have been used in laser factoring .

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Y3Al5O12 crystallize as typical cubic structure, space group Ia3d and lattice parameter
a = 12.000Å(12).
The mixed rare-earth oxide, RE2O3, where RE stands for yttria and rare-earth
elements, is produced at USP-EEL from the mineral Xenotime. In this process,
Xenotime, basically a yttrium and rare-earth phosphate, (Y, RE)PO4, is mixed with
NaOH and heated up to 700oC, allowing the following reaction to occur:
(Y, RE)PO4 + 6NaOH → Na3(Y, RE)O3 + Na3PO4 + 3H2O (A)
The product is broken and milled in a ball-mill, until the particle size is reduced
to a size smaller than 75 μm (200 mesh). The material is then lixivated and precipited
with oxalic acid and finally calcined. The final product is a mixed-oxide, mainly
composed of Y2O3, Yb2O3, Er2O3, Dy2O3 and smaller amounts of other rare-earth
oxides. Its cost is about 20% of the commercial Y2O3(7).
It has been demonstrated that this mixed-oxide, instead of pure Y2O3, can be
used as sintering additive for SiC and Si3N4 ceramics, resulting in a dense ceramic
material with comparable microstructures and mechanical properties(5-7,13-15).
Recently, α-SiAlONs (or α’) ceramics have been developed using this RE2O3 as
stabilizing agent of the α’-phase. In comparison to the Y2O3-based SiAlONs, similar
microstructures and mechanical properties have been obtained(14) with high oxidation
and creep resistance.
Since the lattice parameters of yttria and rare-earth oxides are very close,
because of similar ionic radii, an important question that arises is if the mixed oxide
forms a solid solution or not. The formation of a solid solution could avoid the
seggregation of elements during the sintering process. Also, it is important to know if
the crystal structure of the YAG prepared using RE2O3 is similar to that produced
using pure Y2O3., because since the discovery of stimulated emission in Nd-doped
yttrium–aluminum garnet (YAG) crystal, the rare earth doped YAG crystals have
been the most widely used solid-state laser materials(10,11).
The high-resolution powder X-ray diffraction technique with synchrotron
radiation as source is an appropriate technique for the investigations of small
variations in the crystal structure promoted by partial atomic substitutions, due to its
high intensity and collimated beam characteristics.
Thus, the aim of this work was the development and the comparison of the
crystal structure of Yttrium aluminum garnet (YAG) prepared with RE2O3-Al2O3 or

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Y2O3-Al2O3, by high-resolution X-ray diffraction and refinement by the Rietveld

method. Some physical properties, as densification and mechanical properties for
both YAGs are compared.

EXPERIMENTAL PROCEDURE
Compositions
High purity commercial Al2O3 (SG-1000, Almatis–USA), Y2O3 (H.C.Starck-
Germany) and RE2O3 (USP-EEL–Brazil) were used as starting powders. The yttrium
and rare-earth oxide mixture, RE2O3, was produced at USP-EEL, based on the
investigations reported by Ribeiro(7). The chemical composition of the RE2O3 mixture
is listed in Table 1. Powder batches of Al2O3:Y2O3 and Al2O3:RE2O3 maintaining a
molar ratio of 60:40 were prepared.

Table 1. Composition of the yttria and rare-earth oxide mixture, RE2O3.

oxide wt.% oxide wt.%
Y2O3 44.60 Gd2O3 1.17
Yb3O3 19.71 Tb2O3 0.82
Er2O3 13.94 Sm2O3 0.38
Dy2O3 10.25 Ce2O3 0.09
Ho2O3 3.27 Eu2O3 0.02
Tm2O3 2.83 Nd2O3 0.12
Lu2O3 2.62 La2O3 0.01

Processing and characterizations

Powder batches were prepared by ball-milling for 4 h using ethanol and sintered
ZrO2-balls as milling media. After mixing, the powder batches were dried and then in
an oven at 90°C for 24h. Prior to sintering, the powder mixtures were sieved through
a 60 mesh screen. Green bodies were obtained by cold uniaxial pressing under a
pressure of 80MPa. Samples with 15mm of diameter, were sintered in air, at 1000,
1400 and 16000C, with a heating and cooling rate of 10oC/min, and a isothermal time
of 120 minutes.
The theoretical density of the samples was calculated according to the rule of
mixtures. The final density after sintering was measured by the immersion method in
distilled water, using Archimedes principle.
Scanning Electron Microscopy (SEM) images were obtained using a LEO
1450VP microscope. For the microstructural analysis, the sintered specimens were

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cut, ground, and polished. Subsequently, the polished surfaces were thermal etched
at 13000C for 4 minutes.

High-resolution X-ray diffraction characterization (HRXRD)

High-resolution powder X-ray diffraction measurements were performed using
the XRD1-D12A beam-line at the Brazilian Synchrotron Light Laboratory (LNLS) in
Campinas, Brazil. A multi-axis Hubber diffractometer was used in a two circle
configuration (ω−2θ). The measurements were carried out using a monochromatized
10keV (λ = 1.2398Å) energy beam. The beam size over the sample was
approximately 1x0.5mm2. The sieved powders with sizes smaller than 20μm were
carefully pulverized over a flat plate holder that was kept in planar rotation in order to
randomize the particle distribution that contributes to the Bragg reflection. The
diffracted X-rays were collected by a (200) germanium analyzer crystal and
scintillation detector combination. The patterns were obtained at room temperature in
q-space (q=4π*sin θ*λ–1=d–1) in order to optimize the number of points for each peak.
The data were obtained in the 6.00≤q≤79.00 intervals with 0.01 steps using 1s of
counting time and then converting them into 2θ. The refinement of the crystal
structure was performed by the Rietveld method using FullProf program(16).

Mechanical properties
The hardness and fracture toughness of the low-porosity YAG ceramics
(obtained at 16000C) was determined by Vicker´s indentations with a load of 500gf
for 30s. In order to obtain good statistical sampling, 21 indentations were made per
sample. The fracture toughness was determined by the measurement of the crack
lengths created by the Vicker´s indentations. The calculation of the fracture
toughness was done using a relation proposed by Evans et al(17).
RESULTS AND DISCUSSION
Characterization of RE2O3
Fig. 1(a) shows the result of the refinement of the crystal structure of the
commercial Y2O3. It was verified that all peaks belong to Y2O3. The peaks are sharp
and the value of the full-width at half-maximum (FWHM) determined for the most
intense (222) peak was about 0.04 deg.

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Fig. 1. Rietveld refinement of: (a) Y2O3 and (b) RE2O3. The (+) marks show the
measured data and the line the calculated pattern. The vertical bars show positions
of the Bragg reflections. The differences between calculated and measured data are
shown by the line below the bars.

The high-resolution X-ray diffraction pattern of the mixed oxide (RE2O3) powder
is shown in the Fig. 1(b). It was found that all peaks are related to the Y2O3-type
structure. It can be noted, that the peaks are less intense and broader than that of
the pure Y2O3 (Fig. 1(a)). The width for the most intense (222) peak was determined
to be 0.50 deg. Comparing the diffraction patterns of Y2O3 (Fig.1(a)) and of RE2O3
(Fig.1(b)), the width of the (222) peak of the mixed oxide is more than ten times
larger than that of the pure yttria. The intensity of the (222) peak is 8.5 times smaller
than that of pure yttria. It could also be noted that the peaks of the mixed oxide were
well-adjusted to a pseudo-Voigt profile function. The well-defined peaks are evidence
of a true solid solution formation. The refined structural parameters for yttria and the
mixed oxide are shown in Table 2.
The lattice parameter determined for the mixed oxide was slightly smaller than
that of pure yttria. This can be explained by the smaller mean lattice parameter of the
rare earth oxides which compose the mixed oxide. Taking into account the lattice
parameters of yttria and the principal rare-earth oxides present in the mixed oxide,
above 5 wt.% [Y2O3: a = 10.60Å; Yb2O3: a = 10.43 Å; Er2O3: a = 10.54 Å; Dy2O3: a =
10.66 Å](18) and its respective proportion (see Table 1) the mean lattice parameter
results in a = 10.57 Å. This value is close to that obtained for the mixed oxide. Thus,
these results indicate that the mixed oxide formed by yttria and the rare-earth oxides
form a true solid solution, rather than a physical mixture of oxides.

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Table 2. Characteristics and refined parameters of the Y2O3 and RE2O3 oxides.
Y2O3 mixed oxide, RE2O3
System cubic cubic
o
Space Group I a –3 (n 206) I a –3 (no 206)
a (Å) 10.60796(3) 10.588(1)
Y1 in 8b (1/4, 1/4, 1/4)
Y2 in 24d (x, 0, 1/4) x = 0.9673(1) x = 0.970(6)
O in 48e (x, y, z) x = 0.3915(8) x = 0.394(4)
y = 0.1538(8) y = 0.155(3)
z = 0.3800(8) z = 0.388(4)
Rp (%) 9.23 11.3
Rwp (%) 15.4 14.0
Rexp (%) 11.3 10.9
2
Chi 1.877 1.657

Characterization of YAG ceramics

The relative density of the sintered samples is presented in Fig. 2. The
densification behavior of both samples was also similar. The relative densities of
(RE)AG specimen were slightly higher than that of YAG samples. Furthermore, the
results of densification indicates that the ceramics only present high relative density
at high temperatures, near 1600oC, which the result of relative density were 95.3% e
96.0, for YAG and REAG, respectively.

100
(% of Theoretical Density)

YAG
REAG
Relative Density

90

80

70

60

1000 1100 1200 1300 1400 1500 1600

0
Sintering Temperature ( C)
Fig 2. Relative density of YAG ceramics as function of sintering temperature.

Crystallographic characterizations
Fig.3 shows the XRD patterns of Y3Al5O12 and RE3Al5O12, sintered at 16000C.

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O O - Y3Al5O12 1 - (RE)3Al5O12
0
1
T = 1600 C T=1600°C
O O O O 1 1 1 1 1 1 1
O O O O 1
O O O O O
O 1 1 1 1 1 11

20 30 40 50 60 70 20 30 40 50 60 70
2θ (°) 2θ (°)

Fig.3. XRD patterns of the YAG and REAG samples sintered at 16000C.

Comparing YAG and REAG XRD-patterns, the similarity of the two oxides can
be noted. Due to the similar ionic radii of the rare earth elements present in the oxide
mixture RE2O3, a solid solution is formed, causing a shift in the lattice parameters of
the YAG and REAG. Both, exhibits closed lattice parameters of 11.99(2)Å and
12.01(5)Å, respectively. The small differences between the lattice parameters are
due to the different average ionic radius of the rare earth elements in RE2O3 and that
of yttrium in Y2O3. Furthermore, the distortions of the crystal lattice in REAG caused
by the different ionic radii lead to the broadening of the peaks in regard to pure YAG.
Fig. 4 shows XRD patterns of the Y2O3-Al2O3 samples sintered at different
temperatures (1000, 1400 and 16000C). Fig. 5 shows XRD patterns of the RE2O3-
Al2O3 samples sintered at different temperatures (1000, 1400 and 16000C).
Y3Al5O12 - YAG
30000
o
o λ = 1,1276 A x o T = 1000 C
20000 Al2O3 Y2O3
E = 10,9952 eV

10000 x x
oo o x o x
x x xx x x
Intensity (counts)

0
60000
o
T = 1400 C
40000

20000

80000
*
o
* Y3Al5O12 T = 1600 C
60000
40000

* * ** ** * ** * ** *
* * * * * ** ** * * * * * **
20000
0 * *
10 20 30 40 50 60 70 80
o
2θ ( )
Fig. 4. XRD patterns of the Al2O3-Y2O3 sintered samples

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RE3Al5O12 - (RE)AG
8000
λ = 1,1276 A o x o
6000 o RE2O3 Al2O3 T = 1000 C
E = 10,9952 eV
4000
o x o o

Intensity (counts)
2000 x o x x
x x x x x
0
20000
o
T = 1400 C
10000

40000
30000 * * (RE)3Al5O12 o
T = 1600 C
20000
* **
* ** * * * * *** **
10000
0 * ** * * * * * * * * **
10 20 30 40 50 60 70 80
o
2θ ( )
Fig. 5. XRD patterns of the Al2O3-RE2O3 sintered samples

Samples sintered at 10000C present only Al2O3 and Y2O3 as crystalline phases
indicating no transformation in Y3Al5O12. On the other hand, at 1400 and 16000C, a
total transformation of Al2O3 and Y2O3 crystalline phases in YAG (Y3Al5O12) occurs,
as expected.
Similarly, samples prepared with Al2O3 e RE2O3 and sintered at 10000C
presented only Al2O3 and (RE)2O3 as crystalline phases. Furthermore, at 16000C,
“REAG”, (RE)3Al5O12 was observed as single crystalline phase present in structure. In
an observation of the XRD pattern of samples sintered at 14000C, it is possible to
observe the presence of the different crystalline phase, which is indicated to be some
transitory crystalline phase of the Y3Al5O12, unstable in this range of temperature.
But, as indicated in XRD of the 16000C, this phase is integrally transformed in stable
RE3Al5O12 phase.
The XRD patterns of RE3Al5O12 indicate that this phase crystallize in an
isomorphic and similar Y3Al5O12 structure. The lattice parameter calculated for
Y3Al5O12 and RE3Al5O12 were, respectively, 11.99(2)Å and 12.014(5)Å. The
difference presented in this values corroborated with the expectative of that samples
obtained with RE2O3 (RE3Al5O12) can be a solid solution, where metallic ions of rare
earth occupying substitutional positions of Y+3 in YAG lattice, demonstrating similar
behavior to the RE2O3 in relation to the Y2O3.

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Microstructure and mechanical properties

SEM micrographs of the sintered samples are shown in Fig. 6. Similar
microstructures for both samples, YAG and REAG, are observed. The images exhibit
equiaxial YAG grains, with an average grain size of about 2.5μm. The hardness and
the fracture toughness of the YAGs samples, sintered at 16000C, determined at
room-temperature are summarized in Table 3.

(a ) (b)
Fig 6. SEM micrographs of YAG samples sintered at 16000C using: (a) Y2O3 and (b)
RE2O3.

Table3. Properties of the sintered samples.

Average Grain Size
(μm) Vicker’s Hardness Fracture toughness
Sample
(HV) KIC (MPa.m1/2)

YAG – 16000C 2.3 ± 0.4 398 ± 32 3.7 ± 0.4

(RE)AG – 16000C 2.5 ± 0.3 413 ± 27 4.0 ± 0.3

High densification obtained after sintering can explain these results. Sintered
samples containing REAl5O12 show a discrete tendency to superior densification at
16000C Mechanical properties indicate that RE2O3 can substitute Y2O3, in
development of the YAG’s, but, optical measurements must be executed for total
confirmation of this possibility due to this propertie`s importance in the final use of
this material.

CONCLUSIONS
The high-resolution synchrotron X-ray diffraction measurements of the mixed
oxide, RE2O3, formed by yttria and rare-earth oxides, indicates the formation of a true

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solid solution rather than a physical mixture of independent oxides. Furthermore, the
diffraction patterns of YAGs produced using RE2O3 or Y2O3 as sintering additive
revealed similar structural parameters. The results of the densification, microstructure
and mechanical properties for both materials were close, suggesting the high
potencial for the use of the mixed oxide RE2O3 in substitution of pure Y2O3 in the
formation of Y3Al5O12, resulting in a cost reduction of the final product.

ACKNOWLEDGMENTS
The authors acknowledge Brazilian Synchrotron Light Laboratory (LNLS) for the
high-resolution synchrotron X-ray diffraction measurements under proposal D12A-
XRD1-2047. This work received financial support by FAPESP under Grant no
04/04386-1 and 05/51485-8.

REFERENCES

1. HRENIAK D., STREK W., Synthesis and optical properties of Nd-doped Y3Al5O12
nanoceramics, Journal of Alloys and Compounds 341 (2002) 183–186.
2. LU J., UEDA K.-I., YAGI H., YANAGITANI T., AKIYAMA Y., KAMINSKII A. A.,
Neodymium doped yttrium aluminum garnet (Y3Al5O12) nanocrystalline ceramics - a
new generation of solid state laser and optical materials, Journal of Alloys and
Compounds 341 (2002) 220–225.
3. IKESUE A., Polycrystalline Nd:YAG ceramics lasers, Optical Materials 19 (2002)
183–187
4. TACHIWAKI T., YOSHINAKA M., HIROTA K., IKEGAMI T., YAMAGUCHI O,
Novel synthesis of Y3Al5O12 (YAG) leading to transparent ceramics, Solid State
Communications, 119, (2001), 603-606.
5. STRECKER K., GONZAGA R., RIBEIRO S., HOFFMANN M. J., Substitution of
Y2O3 by a rare earth oxide mixtures as sintering additive of Si3N4 ceramics, Mat.
Lett.; 45 (2000) 39-42.
6. SANTOS C., RIBEIRO S., STRECKER K., SILVA C. R. M., Substitution of pure
Y2O3 by a mixed concentrate of rare earth oxides (CRE2O3) as sintering additive of
Si3N4: a comparative study of the mechanical properties, J. Mater.Process.Techn.,
142 (3) (2003) 697- 701.

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7. RIBEIRO S., Estudo comparativo das propriedades do nitreto de silício sinterizado

com óxido de ítrio/ óxido de silício e concentrado de óxidos de ítrio e terras
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O.M.M. , SILVA C.R.M., compressive creep behavior of hot-pressed Si3N4-CRE2O3-
Al2O3 ceramics, Mater. Res. Bull. 39 (9) (2004) 1279-89.
9. SANTOS C., STRECKER K., PIORINO NETO F., LANNA M.A., SILVA O.M.M.,
SILVA C.R.M., Oxidation behavior of hot-pressed Si3N4 ceramics using CRE2O3-AlN
and CRE2O3-Al2O3 as sintering additives, Mater. Sci. Forum (2005) Vols. 498-499
pp. 569-574.
10. GEUSIC J.E., MARCOS H.M., VAN UITERT L.G., Appl. Phys. Lett. 4 (1964)
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11. KAMINSKII A.A., Crystalline Lasers: Physical Processes and Operating
Schemes, CRC Press, Boca Raton, FL, 1996, Chapter 1.
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C.R.M.; SiAlON ceramics with elongated grain morphology using an alternative
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C. R. M., “Stabilization of α-SiAlONs using a rare-earth mixed oxide (RE2O3) as
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YAG (YTTRIUM ALUMINUM GARNET) OBTIDO POR USO DE ÓXIDO MISTO DE

ÍTRIA E TERRAS RARAS, RE2O3

RESUMO
Nesse trabalho, a substituição de Y2O3 comercial por um óxido misto de terras raras,
na formação de YAG, Yttrium aluminum Garnet-Y3Al5O12, foi investigada. Misturas
de pós de Al2O3:Y2O3 e Al2O3:RE2O3 na razão molar de 60:40, foram preparadas por
moagem e sobsequente prensagem uniaxial a frio. Compactos foram sinterizados a
1000, 1400 ou 16000C, por 120 minutos. O óxido RE2O3 foi caracterizado por
difração de raios X de alta resolução (HRXRD) e comparados com Y2O3. Analise de
raios X do RE2O3 indicam a formação de uma solução sólida. O refinamento da
estrutura pelo método de Rietveld, realizado nas amostras sinterizadas de YAG e
(RE)AG revelaram uma estrutura cristalina similar assim como a microestrutura, com
tamanho médio de grão em torno de 2.5μm. Como complemento, dureza e
tenacidade a fratura foram da ordem de 400HV e 3.8MPa.m1/2respectivamente.
Assim pôde ser verificado que o Y2O3 puro pode ser substituído pela solução sólida
de itria e terras raras, RE2O3, na formação de YAGs, apresentando microestrutura e
propriedades mecânicas similares.

Palavras-chave: cerâmica, Y3Al5O12; óxido de terras raras, caracterização, Difração

de raios X.

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