Solid-state synthesis and

characterization of low-melting
mixed-metal oxides
GERARDO P. RAMOS OTERO
PRINCIPAL INVESTIGATOR: DR. L. KOSCIELSKI

Uni versi ty of Puerto Ri co at Cayey

Outline
Solid-state Chemistry Background
Solid-state Synthesis Methodology
Future Work
Acknowledgements

Solid-state Chemistry Background
Solid-state Chemistry
Solid-state Synthesis
High Temperature
Starting Materials (powders, granules, crystals)
Process
Bond Disruption (high temperatures)
Rearrangement
Reformation (cooling)
Solid-state Chemistry Background
Low melting mixed metal oxides
Ternary Compounds
M
x
M
y
O
z

Oxides
At least one oxygen atom and one
other element in its chemical formula
Oxygen in the oxidation state of 2
Electrical conductivity and optical
transparency
Solid-state Chemistry Background
Low Melting Metals

Solid-state Synthesis
Methodology
Synthesis
Vessel Preparation
Silica Tubes
Loading of Reagents
Silica Tubes
Atmosphere
Glove-box
Heating of Reactions
Computer-controlled furnace
Heating Step
Plateau Step
Slow-cooling Step
Trial and Error Approach

Solid-state Synthesis
Methodology
Structural Determination
X-ray Spectroscopy
Powders and Crystals
Elemental Composition
Stoichiometry


Product
Powder
Powder X-ray
diffraction
Novel
Compound
Reload into silica
tubes with
crystallizing
agent
Crystal
Single-crystal
X-ray diffraction
Previously
Synthesized
Crystal
Single-crystal
X-ray diffraction
Solid-state Synthesis
Methodology
Physical Properties Determination
Depends on the compound
Resistivity
Magnetic Properties
Thermopower

Ternary low-melting mixed-
metal oxides already created
Ternary low-melting mixed-metal oxides already created
13/13 13/14 13/15 14/14 14/15 15/15
-Ga
4
GeO
8
BiAlO
3
Bi
2
Ge
3
O
9

In
4
Sn
3
O
12
BiGaO
3
Bi
2
GeO
5

PbAl
2
O
4
BiInO
3
-Bi
2
Sn
2
O
7

PbGa
2
O
4
GaAsO
4
Bi
2
Sn
2
O
7

AlPO
4
Pb
2
[As
2
O
5
]
GaPO
4
PbAs
2
O
4

AlSbO
4
PbAs
2
O
6

GaSbO
4


Loaded Reactions
Groups 14/14
Reaction
Stoichiometry Possible
Products
Quantity Loaded
(g)
Sn Pb Sn Pb
1 2 5
Sn
2
Pb
5
O
7

Sn
2
Pb
5
O
12

Sn
2
Pb
5
O
9

Sn
2
Pb
5
O
14

0.005 0.0218
2 1 3
SnPb
3
O
4

SnPb
3
O
7

SnPb
3
O
5

SnPb
3
O
8

0.004 0.2094
3 2 3
Sn
2
Pb
3
O
5

Sn
2
Pb
3
O
8

Sn
2
Pb
3
O
7

Sn
2
Pb
3
O
10

0.008 0.0210

Loaded Reactions
Groups 14/15
Synthesize new ternary compounds that contain two
metals and an oxygen atom using previous synthesis
methodology.
2In
2
O
3
+ 3SnO
2
In
4
Sn
3
O
12
(Already synthesized)
2Ga
2
O
3
+ 3GeO
2
Ga
4
Ge
3
O
12

Characterize these compounds structurally via powder
and single-crystal X-ray diffraction methods.
Determine selected physical properties such as magnetic
susceptibilities, conductivity, resistivity, and thermopower.
Future Work
1,400
o
C, 10h

1,400
o
C, 10h

Future Work
Synthesis Methodology:
1. M + M
2
O
3
at 226.85
o
C for 10d
2. M
2
O
3
+ MO
2
at 1000
o
C for 2-3h

Future Work
Method 1
Future Work
Method 2
Acknowledgments
University of Puerto Rico at Cayey
RISE Program (Research Initiative for Scientific Enhancement)
BRIC
III (Instituto de Investigaciones Interdisciplinarias)

Dr. L. Koscielski

Solid-state synthesis and
characterization of low-melting
mixed-metal oxides
GERARDO P. RAMOS OTERO
PRINCIPAL INVESTIGATOR: DR. L. KOSCIELSKI

Uni versi ty of Puerto Ri co at Cayey

Conductivity and Resistivity
X-ray Spectroscopy