Solid State Synthesis of
Mixed Metal Oxides
Tornés-Blanco Anibal
Alicea-Pauneto Abneil
Colón-Rivera Ramón
González-Piñeiro Ann
INTRODUCTION
Background Info
❏ Solid-state synthesis
❏ Branch of material chemistry : Mix &
match solids.
❏ Why is this study so important?
❏ Obtain new compounds with unique
properties to aid the technologically
dependent world we live in.
Cornerstone of technology
❏ Superconductors such as high purity silicon and catalysts like platinum,
took a pivotal role in the industrialization process during the 20th century.
Chen et al. 2015
“In recent years, electrochemical capacitors,
also known as supercapacitors, have
received a large amount of attention as an
important power storage device due to their
high power density, fast recharge capability
and long cycle life .”
Related Works
Koscielski et al. 2012
Problem
❏ Synthesize new compounds from the combination of
different metals from the families 13, 14, 15, chalcogens
(group 16) and intrinsic Oxygen.
Hypothesis
❏ After heat application, oxidation reactions will occur and
hopefully, crystals will appear .
❏ This is a trial and error experimentation
METHODOLOGY
Reactions
Ternary Quaternary
1 In : 1 Sb 1 S : 1 Bi : 1 In
1 In : 1 Bi 1 Pb : 1 Sn : 1 S
2 In : 1 Sn 2 In : 1 Sn : 1S
2 In : 1 Pb 2 In : 1 Sn : 2 S
Ternary Quaternary
5 In : 3 Sb 1 Co : 2 In : 1 S
5 Sn : 3 Pb 1 Co : 1 Bi : 1 S
5 Bi : 3 Pb 1 In : 2 Co : 2 S
1 Bi : 2 Pb 1 In : 1 Bi : 1 S
Methodology
Element Selection
& Weighing
Carbon CoatingSilica Tube Split
http://chemistry.stac
kexchange.com/que
stions/18968/why-
does-a-glass-tube-
show-white-bands-
after-being-heated-
with-a-torch
http://instrumentosdelaboratorio.org/bal
anza-de-laboratorio
http://oxypetrol.c
om/
https://www.flickr
.com/photos/fall
enangel8/25032
98659/
Methodology
Transfer the reaction
to the tube
Heat in the GSL-
1100x “Lisa”
”
Results Analysis
via Microscope
http://instrumentosdela
boratorio.org/espatula-
de-laboratorio
Heating Curve
Cooling
Heating
Liquid/Solid
Results
We
found
Crystals!
But not the type we
expected...
Ternary Reactions I
5 In : 3 Sb 5 Sn : 3 Pb
Ternary Reactions II
5 Bi : 3 Pb 1 Bi : 2 Pb
Ternary Reactions III
1 In : 1 Sb 1 In : 1 Bi
Ternary Reactions IV
2 In : 1 Sn 2 In : 1 Pb
Conclusions
❏ The results were partially positive making allusions to our
hypothesis.
❏ We obtained Oxide Powder.
Limitations
❏ Time Limitation
❏ Only one high temperature vacuum tube furnace,
named ¨Lisa¨ .
❏ Oxygen insulating equipment
Future Work
❏ Try new combinations of ternary and quaternary
compounds
❏ Analyze the data collected with the appropriate
instrumentation
References
Chen S, Xue M, Li Y, Zhu L, Zhang D, Fang Q, Qiu S. 2015. Porous ZnCo2O4
nanoparticles derived from a new mixed-metal organic framework for supercapacitors.
Royal Society of Chemistry (RSC) (2) . [2014 Oct 17, cited 2015 April 29] 2:(177-
183). DOI: 10.1039/c4qi00167b
C. Z. Yuan, L. Yang, L. R. Hou, L. F. Shen, X. G. Zhang and X. W. Lou, Energy
Environ. Sci., 2012, 5, 7883.
Koscielski L, Ringe E, Van Duyne R, Ellis D, Ibers J. 2012. Single-Crystal
Structures, Optical Absorptions, and Electronic Distributions of Thorium
Oxychalcogenides ThOQ (Q= S, Se, Te). American Chemical Society
dx.doi.org/10.1021/ic300510x | Inorg. Chem. 2012, 51, 8112−8118.
Acknowledgements
● RISE Program at UPR Cayey
● Omar Padilla
● Christopher Bernard
● Andres Diaz
● Maria Rivera
● Roberto González
● Dr. Lukasz Koscielski

Solid State Synthesis of Mixed Metal Oxides

  • 1.
    Solid State Synthesisof Mixed Metal Oxides Tornés-Blanco Anibal Alicea-Pauneto Abneil Colón-Rivera Ramón González-Piñeiro Ann
  • 2.
  • 3.
    Background Info ❏ Solid-statesynthesis ❏ Branch of material chemistry : Mix & match solids. ❏ Why is this study so important? ❏ Obtain new compounds with unique properties to aid the technologically dependent world we live in.
  • 4.
    Cornerstone of technology ❏Superconductors such as high purity silicon and catalysts like platinum, took a pivotal role in the industrialization process during the 20th century. Chen et al. 2015 “In recent years, electrochemical capacitors, also known as supercapacitors, have received a large amount of attention as an important power storage device due to their high power density, fast recharge capability and long cycle life .”
  • 5.
  • 6.
    Problem ❏ Synthesize newcompounds from the combination of different metals from the families 13, 14, 15, chalcogens (group 16) and intrinsic Oxygen.
  • 7.
    Hypothesis ❏ After heatapplication, oxidation reactions will occur and hopefully, crystals will appear . ❏ This is a trial and error experimentation
  • 8.
  • 9.
    Reactions Ternary Quaternary 1 In: 1 Sb 1 S : 1 Bi : 1 In 1 In : 1 Bi 1 Pb : 1 Sn : 1 S 2 In : 1 Sn 2 In : 1 Sn : 1S 2 In : 1 Pb 2 In : 1 Sn : 2 S Ternary Quaternary 5 In : 3 Sb 1 Co : 2 In : 1 S 5 Sn : 3 Pb 1 Co : 1 Bi : 1 S 5 Bi : 3 Pb 1 In : 2 Co : 2 S 1 Bi : 2 Pb 1 In : 1 Bi : 1 S
  • 10.
    Methodology Element Selection & Weighing CarbonCoatingSilica Tube Split http://chemistry.stac kexchange.com/que stions/18968/why- does-a-glass-tube- show-white-bands- after-being-heated- with-a-torch http://instrumentosdelaboratorio.org/bal anza-de-laboratorio http://oxypetrol.c om/ https://www.flickr .com/photos/fall enangel8/25032 98659/
  • 11.
    Methodology Transfer the reaction tothe tube Heat in the GSL- 1100x “Lisa” ” Results Analysis via Microscope http://instrumentosdela boratorio.org/espatula- de-laboratorio
  • 12.
  • 13.
  • 14.
    We found Crystals! But not thetype we expected...
  • 15.
    Ternary Reactions I 5In : 3 Sb 5 Sn : 3 Pb
  • 16.
    Ternary Reactions II 5Bi : 3 Pb 1 Bi : 2 Pb
  • 17.
    Ternary Reactions III 1In : 1 Sb 1 In : 1 Bi
  • 18.
    Ternary Reactions IV 2In : 1 Sn 2 In : 1 Pb
  • 19.
    Conclusions ❏ The resultswere partially positive making allusions to our hypothesis. ❏ We obtained Oxide Powder.
  • 20.
    Limitations ❏ Time Limitation ❏Only one high temperature vacuum tube furnace, named ¨Lisa¨ . ❏ Oxygen insulating equipment
  • 21.
    Future Work ❏ Trynew combinations of ternary and quaternary compounds ❏ Analyze the data collected with the appropriate instrumentation
  • 22.
    References Chen S, XueM, Li Y, Zhu L, Zhang D, Fang Q, Qiu S. 2015. Porous ZnCo2O4 nanoparticles derived from a new mixed-metal organic framework for supercapacitors. Royal Society of Chemistry (RSC) (2) . [2014 Oct 17, cited 2015 April 29] 2:(177- 183). DOI: 10.1039/c4qi00167b C. Z. Yuan, L. Yang, L. R. Hou, L. F. Shen, X. G. Zhang and X. W. Lou, Energy Environ. Sci., 2012, 5, 7883. Koscielski L, Ringe E, Van Duyne R, Ellis D, Ibers J. 2012. Single-Crystal Structures, Optical Absorptions, and Electronic Distributions of Thorium Oxychalcogenides ThOQ (Q= S, Se, Te). American Chemical Society dx.doi.org/10.1021/ic300510x | Inorg. Chem. 2012, 51, 8112−8118.
  • 23.
    Acknowledgements ● RISE Programat UPR Cayey ● Omar Padilla ● Christopher Bernard ● Andres Diaz ● Maria Rivera ● Roberto González ● Dr. Lukasz Koscielski

Editor's Notes

  • #2 Anibal
  • #4 Abneil This synthesis consist in the mix of two solids. This is an important study because it lets us synthesize new compounds to characterize and to evaluate new properties po
  • #5 Anibal Superconductors have high capacity to conduct electricity such as silicon as the word expresses. Inside of your computer or maybe even your television set are little black boxes called chips. Scientists flatten silicon crystals into little circles called wafers. These wafers are then stamped with the image of a computer chip.
  • #6 Here we have the sample of a work related to what we did, this was done by Koscieslky and collaborators and they managed to characterize physical and chemical properties of a thorium derived compound
  • #7 Ramon Quaternary: 2 metals, chalcogen and intrinsic Oxygen Ternary: 2 metals with Intrinsic Oxygen
  • #8 Ann Redox occurs Important factor : We do not know what combination or quantitiy we need to form crystals, Difficult because the combinations are endless Predictions are what make this proyect so challening
  • #10 Anibal Similar elements to have the same melting point and a constant heating curve during experimentation
  • #11 Ramon 1) The element was selected and determined the mass of each reactant by calculations. 2) First, we have a silica tube of 4 feet. Then, we have 1 feet. Second, the feet divided into 6” with the oxygen acetylene torch. 3) The Carbon Coating we administer 1 drop of acetone to the silica tube and then burn it in the bunsen burner. It was repeated 2 more times. We use the Acetone to have the crystals separated of the tube. The purpose is that the light do not react with the compounds.
  • #12 Abneil 1)Transfer reactants with the specific amount calculated to react in terms of their ratio 2)Tubes into furnace Lisa to melt one of the solids to make 3) Analyze in dissecting
  • #13 Ann As mentioned previously we need reactants close to melting points between each, For each reaction heating , be it ternary or quaternary it is neccesary to build a heating curve This heating curve will determine at which temperature compounds will mix At this constant temperature the reactants will mix in their liquid states. Cooling produces crystals and a faster cooling will not give enough time for crystal growth
  • #15 Anibal
  • #16 Ramon In Chemistry, powder are tiny particles that have crystal structure. In the images of each reaction we saw powder. Powder: tiny particles that are above the floor and in the air. (Dictionary)
  • #17 Ramon
  • #18 Ramon
  • #19 Ramon
  • #20 Abneil We did not obtained the kind of crystals we were expecting. We obtain Oxide Powder.
  • #21 Ann Unfortunately, we had various limitations Not much time to make 16 reactions, only achieved 8 of them. The quaternary was not possible since every reaction had to be exposed to about 7 days or more Intrinsic oxygen could not be calculated.