The document discusses solid-state synthesis of mixed metal oxides. It introduces solid state chemistry and synthesis, which involves producing solids by combining substances through high-temperature reactions. Specific aims are to synthesize new mixed metal oxide compounds with distinct properties for various applications. The methodology described involves using silica tubes lined with carbon and heating powdered metal reactants at high temperatures for 1-2 weeks to form novel crystals. Future work plans to carry out reactions combining tin, lead, antimony and bismuth, and synthesize new mixed metal oxides according to predicted products.

1. Solid-State Synthesis of Mixed-
Metal OxidesPaola G. Caballero León
Anthony Hernández Rivera
Dr. Lukasz Koscielski
RISE Program
University of Puerto Rico at Cayey

2. Introduction
Solid State
Chemistry
 Materials Science
 Synthesis, structure, and properties of
solid materials
Solid State
Synthesis
 Production of a solid substance by
combining simpler substances through
a chemical process.
High
Temperature
Reaction in
Solvents
 “Shake and Bake” Procedure
 Involves precipitating the solid
from a solvent

3. Technological Applications
• Solid State Electronics
– Semiconductors
• Transistors
• Silicon Chips
• Photocells
• Cooperative Magnetic Behavior
– Ferromagnetism and Antiferromagnetism
• Reactions
– Catalysts (Salamat et al. 2011)

4. Specific Aims
• Synthesize new mixed metal oxide
compounds that exhibit distinct properties
resulting in a variety of applications for a
wide range of fields.
• Synthesize a mixed metal oxide with the
pyrochloric structure of A2B2O7
(Salamat et al. 2011)

5. Problem and Hypothesis
• Problem
– Can novel mixed metal oxide crystals be
obtained from a high temperature reaction of
solid powder reactants?
• Hypothesis
– Due to the wide array of stoichiometric
proportions, novel mixed metal oxide crystals
can be obtained from a high temperature
reaction of solid powder reactants.

6. Solid State Synthesis
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b4a10066707a/tumblr_mir3lqoHhO1qa5bbmo1_50
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Liquid 1000 C “solution”

8. Predicting Products
1. Choose Reactants: Sn and Pb
2. Stoichiometry: 3Sn: 5Pb
3. Oxidation States: Sn+2, Sn+4, Pb+2, Pb+4 ,
O-2
4. Possible Products:
Reactants Products
3Sn+2, 5Pb+2 Sn3Pb5O8
3Sn+2, 5Pb+4 Sn3Pb5O11
3Sn+4, 5Pb+2 Sn3Pb5O13
3Sn+4, 5Pb+4 Sn3Pb5O16

9. MIXED METAL OXIDE
REACTIONS

10. Group 14/14
1. Reaction 1: Sn and Pb
2. Stoichiometry: 9Sn: 15Pb
3. Oxidation States: Sn+2, Sn+4, Pb+2, Pb+4 ,
O-2
4. Possible Products:
Reactants Products
9Sn+2, 15Pb+2 Sn9Pb15O24
9Sn+2, 15Pb+4 Sn9Pb15O39
9Sn+4, 15Pb+2 Sn9Pb15O33
9Sn+4, 15Pb+4 Sn9Pb15O48

11. Group 14/14
1. Reaction 2: Sn and Pb
2. Stoichiometry: 13Sn: 6Pb
3. Oxidation States: Sn+2, Sn+4, Pb+2, Pb+4 ,
O-2
4. Possible Products:
Reactants Products
13Sn+2, 6Pb+2 Sn13Pb6O19
13Sn+2, 6Pb+4 Sn13Pb6O25
13Sn+4, 6Pb+2 Sn13Pb6O32
13Sn+4, 6Pb+4 Sn13Pb6O38

12. Group 15/15
1. Reaction 3: Sb and Bi
2. Stoichiometry: 7Sb: 21Bi
3. Oxidation States: Sb+3, Sb+5, Bi+3, O-2
4. Possible Products:
Reactants Products
7Sb+3, 21Bi+3 Sb7Bi21O42
7Sb+5, 21Bi+3 Sb7Bi21O49

13. Group 15/15
1. Reaction 4: Sb and Bi
2. Stoichiometry: 11Sb: 3Bi
3. Oxidation States: Sb+3, Sb+5, Bi+3, O-2
4. Possible Products:
Reactants Products
11Sb+3, 3Bi+3 Sb11Bi3O21
11Sb+5, 3Bi+3 Sb11Bi3O32

14. Group 14/15
Reactants Products
7Bi+3 , 9Sn+2 Bi14Sn18O39
7Bi+3 , 9Sn+4 Bi14Sn18O57
Reaction #1
1. Chosen Reactants: Sn, Bi
2. Stoichiometry: 7Bi:9Sn
3. Oxidation States: Bi+3, Sn+2, Sn+4
4. Possible Products:

15. Group 14/15
Reactants Products
13Pb+2, 23Bi+3 Pb26Bi46O95
13Pb+4, 23Bi+3 Pb26Bi46O121
Reaction #2
1. Chosen Reactants: Pb, Bi
2. Stoichiometry: 13Pb:23Bi
3. Oxidation States: Pb+2, Pb+4, Bi+3
4. Possible Products

16. Group 14/15
Reactants Products
33Pb+2, 21Sb+3 Pb66Sb42O129
33Pb+2, 21Sb+5 Pb66Sb42O171
33Pb+4, 21Sb+3 Pb66Sb42O195
33Pb+4, 21Sb+5 Pb66Sb42O237
Reaction #3
1. Chosen Reactant: Pb, Sb
2. Stoichiometry: 33Pb:21Sb
3. Oxidation States: Pb+4, Pb+4, Sb+3, Sb+5
4. Possible Products

17. Group 14/15
Reactants Products
12Sn+2, 17Sb+3 Sn24Sb34O75
12Sn+2, 17Sb+5 Sn24Sb34O109
12Sn+4, 17Sb+3 Sn24Sb34O99
12Sn+4, 17Sb+5 Sn24Sb34O133
Reaction #4
1. Chosen Reactant: Sn, Sb
2. Stoichiometry: 12Sn: 17Sb
3. Oxidation States: Sn+2, Sn+4, Sb+3, Sb+5
4. Possible Products

18. Group 14/15
Reactants Products
2Sn+2, 2Bi+3 Bi2Sn2O5
2Sn+4, 2Bi+3 Bi2Sn2O7
Reaction #5
1. Chosen Reactant: Bi, Sn
2. Stoichiometry: 2Sn:2Bi
3. Oxidation States: Sn+2, Sn+4, Bi+3
4. Possible Products
Pyrochloric
Structure

19. Methodology
1. Silica tubes are used because
of its ability to withstand
extreme pressures (10atm)
2. Pairs of tubes are split in half
using a special acetylene
flame.
3. Using the acetylene
flame, the bottom side of the
tube is ideally molded so the
reactants don’t pour out.
4. 2-3 drops of acetone are
added to the tubes, and the
bottom part of the tube is
flamed using a Bunsen
burner.
5. This step is repeated on three
separate occasions, in order
to create a three carbon lining
layer.
6. Finely powdered starting
materials are individually
added to the tubes and then
place in an oven at 500˚C-
1000˚C for approximately 1-2
weeks.

20. Methodology
Silica Tube
Acetilene
Flame
Carbon
Lining
http://www.uruguaye
duca.edu.uy/UserFil
es/P0001/Image/ima
genes/Bunsen.jpg
http://www.ustudy.in/sites
/default/files/images/oxy-
acetylene_weld_torch.jpg

21. Methodology

22. Limitations
• Non-operational Ovens
• Limited time

23. Future Work
• Load our respective reactions using finely
powdered starting materials available at
the laboratory, elements: Sn, Pb, Sb, and
Bi (groups 14/15, 14/14, and 15/15).
• Synthesize new mixed-metal oxide
compounds according to the established
reactions.

24. Acknowledgements
• Dr. Lukasz Koscielski
• Gerardo Ramos
• RISE Program
• University of Puerto Rico at Cayey