Solid-State Synthesis of Mixed-
Metal OxidesPaola G. Caballero León
Anthony Hernández Rivera
Dr. Lukasz Koscielski
RISE Pr...
Introduction
Solid State
Chemistry
 Materials Science
 Synthesis, structure, and properties of
solid materials
Solid Sta...
Technological Applications
• Solid State Electronics
– Semiconductors
• Transistors
• Silicon Chips
• Photocells
• Coopera...
Specific Aims
• Synthesize new mixed metal oxide
compounds that exhibit distinct properties
resulting in a variety of appl...
Problem and Hypothesis
• Problem
– Can novel mixed metal oxide crystals be
obtained from a high temperature reaction of
so...
Solid State Synthesis
http://www.ru.all.biz/img/ru/catalog/177627.jpeg
http://24.media.tumblr.com/97f580680077f7af7abd
b4a...
Predicting Products
1. Choose Reactants: Sn and Pb
2. Stoichiometry: 3Sn: 5Pb
3. Oxidation States: Sn+2, Sn+4, Pb+2, Pb+4 ...
MIXED METAL OXIDE
REACTIONS
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. Poss...
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. Poss...
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 Pr...
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 Pr...
Group 14/15
Reactants Products
7Bi+3 , 9Sn+2 Bi14Sn18O39
7Bi+3 , 9Sn+4 Bi14Sn18O57
Reaction #1
1. Chosen Reactants: Sn, Bi...
Group 14/15
Reactants Products
13Pb+2, 23Bi+3 Pb26Bi46O95
13Pb+4, 23Bi+3 Pb26Bi46O121
Reaction #2
1. Chosen Reactants: Pb,...
Group 14/15
Reactants Products
33Pb+2, 21Sb+3 Pb66Sb42O129
33Pb+2, 21Sb+5 Pb66Sb42O171
33Pb+4, 21Sb+3 Pb66Sb42O195
33Pb+4,...
Group 14/15
Reactants Products
12Sn+2, 17Sb+3 Sn24Sb34O75
12Sn+2, 17Sb+5 Sn24Sb34O109
12Sn+4, 17Sb+3 Sn24Sb34O99
12Sn+4, 1...
Group 14/15
Reactants Products
2Sn+2, 2Bi+3 Bi2Sn2O5
2Sn+4, 2Bi+3 Bi2Sn2O7
Reaction #5
1. Chosen Reactant: Bi, Sn
2. Stoic...
Methodology
1. Silica tubes are used because
of its ability to withstand
extreme pressures (10atm)
2. Pairs of tubes are s...
Methodology
Silica Tube
Acetilene
Flame
Carbon
Lining
http://www.uruguaye
duca.edu.uy/UserFil
es/P0001/Image/ima
genes/Bun...
Methodology
Limitations
• Non-operational Ovens
• Limited time
Future Work
• Load our respective reactions using finely
powdered starting materials available at
the laboratory, elements...
Acknowledgements
• Dr. Lukasz Koscielski
• Gerardo Ramos
• RISE Program
• University of Puerto Rico at Cayey
Solid State Synthesis of Mixed-Metal Oxides
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Solid State Synthesis of Mixed-Metal Oxides

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  • Solid-state chemistry, also sometimes referred to as materials chemistry, is the study of the synthesis, structure, and properties of solid phase materials.Objective- Synthesizing Mixed Metal Oxides Crystals (solids)A large number of the most interesting inorganic compounds in the solid state , and especially in crystalline form, are prepared at high temperatures (>500C)One of the most widely used procedures (“shake and bake”) involves mixing two or more finely powdered starting materials, placing the mixture in a sealed inert container, and heating the entire container in an oven at +500˚C.
  • Solid State Synthesis of Mixed-Metal Oxides

    1. 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. 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. 3. Technological Applications • Solid State Electronics – Semiconductors • Transistors • Silicon Chips • Photocells • Cooperative Magnetic Behavior – Ferromagnetism and Antiferromagnetism • Reactions – Catalysts (Salamat et al. 2011)
    4. 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. 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. 6. Solid State Synthesis http://www.ru.all.biz/img/ru/catalog/177627.jpeg http://24.media.tumblr.com/97f580680077f7af7abd b4a10066707a/tumblr_mir3lqoHhO1qa5bbmo1_50 0.jpg Liquid 1000 C “solution”
    7. 7. 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
    8. 8. MIXED METAL OXIDE REACTIONS
    9. 9. 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
    10. 10. 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
    11. 11. 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
    12. 12. 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
    13. 13. 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:
    14. 14. 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
    15. 15. 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
    16. 16. 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
    17. 17. 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
    18. 18. 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.
    19. 19. 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
    20. 20. Methodology
    21. 21. Limitations • Non-operational Ovens • Limited time
    22. 22. 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.
    23. 23. Acknowledgements • Dr. Lukasz Koscielski • Gerardo Ramos • RISE Program • University of Puerto Rico at Cayey

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