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Final solid state synthesis paola and anthony
- 1. Solid-State Synthesis ofMixed- Metal OxidesPaola G. Caballero León Anthony Hernández Rivera Dr. Lukasz Koscielski RISE Program University of Puerto Rico at Cayey
- 2. Introduction Solid State Chemistry MaterialsScience 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 • SolidState Electronics – Semiconductors • Transistors • Silicon Chips • Photocells • Cooperative Magnetic Behavior – Ferromagnetism and Antiferromagnetism • Reactions – Catalysts (Salamat et al. 2011)
- 4. Specific Aims • Synthesizenew 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.
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- 8. Predicting Products 1. ChooseReactants: 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
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- 10. Group 14/14 1. Reaction1: 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. Reaction2: 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. Reaction3: 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. Reaction4: 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 tubesare 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.
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- 22. Limitations • Non-operational Ovens •Limited time http://www.carolroth.com/wp-content/uploads/2013/04/MP900400674.jpg
- 23. Future Work • Loadour 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. LukaszKoscielski • Gerardo Ramos • RISE Program • University of Puerto Rico at Cayey
- 25. Solid-State Synthesis ofMixed- Metal OxidesPaola G. Caballero León Anthony Hernández Rivera Dr. Lukasz Koscielski RISE Program University of Puerto Rico at Cayey
Editor's Notes
- #4 Cooperative Magnetic Behavior- this more complicated phenomenon occurs only in the solid state where interactions between the magnetic moments of adjacent metal ions in the infinite non-molecular structure can occur. Ferromagnetic- are not only able to develop very large magnetization in a magnetic field, but they remain permanently magnetized when removed from the field Antiferromagnetic- behave in a manner opposite
- #6 One of the shortcomings of this procedure is that it is often difficult to predict the stoichiometry of the product. For this reason, solid state synthesis is considered an exploratory field of science.
- #22 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.