Synthesis of Nanoparticles of Hybrid Synthesis of Nanoparticles of - - PowerPoint PPT Presentation

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Synthesis of Nanoparticles of Hybrid Synthesis of Nanoparticles of Hybrid Frameworks Using Hydrothermal and Frameworks Using Hydrothermal and Emulsion Methods Emulsion Methods Alison Morrison Chemical Engineering, SBCC Mentors: Zeric Hulvey

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SLIDE 1

Synthesis of Nanoparticles of Hybrid Synthesis of Nanoparticles of Hybrid Frameworks Using Hydrothermal and Frameworks Using Hydrothermal and Emulsion Methods Emulsion Methods

Funded by: Department of Energy and Air Products

Alison Morrison

Chemical Engineering, SBCC Mentors: Zeric Hulvey and Josh Furman Faculty Advisor: Prof. Tony Cheetham

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Nanoparticles of Hybrid Frameworks

Separations Catalysis Hydrogen storage

Hybrid Framework Structures

Metal centers with organic linkers (ligands) Low density, high porosity materials

Applications Nanoscale

New properties emerge Very few examples of nanoscale hybrid frameworks

Li, H.; Eddaoudi, M.; O’Keeffe, M.; Yaghi, O.M. Nature 1999, 402, 276.

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SLIDE 3

Research Objectives

Synthesize hybrid frameworks using hydrothermal

methods

Use emulsion method to make nanomaterials Combine both methods to synthesize nanoparticles

  • f hybrid frameworks

Rowsell, J. L. C.; Yaghi, O. M. Angew. Chem. Int. Ed. 2005, 44, 4670-4679.

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Tools for Analysis

  • SEM – Scanning electron microscopy
  • XRD – X-ray diffraction: powder and

single crystal

http://www.mrl.ucsb.edu/mrl/centralfacilities/xray/instruments/XPERT- MPD.html http://www.dur.ac.uk/crystallography.group/images/smart6k.jpg http://www.mrl.ucsb.edu/mrl/centralfacilities/micr

  • scopy/index.html#sem
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SLIDE 5

Hydrothermal Method

Teflon liner Stainless steel autoclave

Time Temperature Concentration pH Metal salt Solvent

Variables Purpose

  • Increased pressure and

temperature

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SLIDE 6

Hydrothermal Results

  • Synthesized single crystals of

Zn(C2N3H2)(CH3COO)

  • ZnO2N4 octahedra and

ZnO2N2 tetrahedra connected by triazolate and acetate ions

  • Investigating possible

porosity

N C O H

  • Focused on 1,2,4-triazole
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Precipitation Method

Co(NO3)2 H2O NaOH H2O Mixing Co(OH)2 Na+ NO3

  • Centrifuge

Rinse H2O Co(OH)2 Heat Co3O4

Characteristics

  • Untemplated method
  • uncontrolled particle

size and shape

  • Used as a control for comparison

to the emulsion sample

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Emulsion Method

CTAB N-butanol isooctane CTAB N-butanol isooctane Co(NO3)2 H2O NaOH H2O Mixing Heat Co3O4 Mixing Ultra- sound Precipitate Co(OH)2

  • Templated method
  • Allows control over the size and

shape of particles formed

Characteristics

  • Templated method
  • controls particle size

and shape

surfactant Water droplet Oil Co2+ NO3

  • N+ Br -
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SLIDE 9

Precipitation vs. Emulsion SEM Images

Precipitation sample

  • f Co3O4

Emulsion sample of Co3O4

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SLIDE 10

Combination of the Emulsion and Hydrothermal Methods

+ =

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SLIDE 11

Conclusions

Future work

  • Continue work on combining the emulsion and the hydrothermal

methods

Accomplishments

  • Synthesized a new hybrid framework
  • Emulsion reactions reduced particle size and increased uniformity
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SLIDE 12

Acknowledgements

Samantha Freeman Liu-Yen Kramer

  • Dr. Nick Arnold
  • Prof. Evelyn Hu

The Cheetham Group

  • Dr. Ghizzoni and Young
  • Mr. Wopat

Jessica Morrison

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SLIDE 13

Thank you for your time!