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1
Spray Pyrolysis of Oxide Materials
Master Thesis in nanotechnology
Student: Roger Moen
Supervisor: Prof. Mari-Ann Einarsrud
Co-supervisors: Prof. Tor Grande and Ruth Astrid Strøm
Om du ønsker, kan du sette inn navn, tittel på foredraget, o.l. her.
2
Topic
Prepare nanopowders by spray pyrolysis with varying
chemical and process parameters and determine their
effect on powder characteristics
– Chemical parameter: complexing agent
– Process parameters: precursor solution feeding rate and carrier gas
flow
3
Previous work
• Y2O3:Eu3+
• Precursor solution concentration
– Little effect
• Complexing agents
– Affects reaction rate, tap density, crystallite size, morphology and
emission spectrum
4
Materials
• Y2O3 and Y2O3:Eu3+.
• Precursors: Y(NO3)3 and Eu(NO3)3.
• Complexing agents: Maleic acid and EDTA
5
Applications
Y2O3
• Refractory coatings
• Precursor for many
materials (e.g.
superconductors)
• Host material for many
RE elements
• Sensors
• Additive in paints and
plastics
Y2O3:Eu3+
• Red emitting phosphor in
displays and biological
imaging
6
Preparation
• Steps
– Atomization of precursor solution
– Evaporation of solvent
– Thermolysis
7
Characterization
• TGA
• XRD
– Crystallite size
– Purity
• SEM
– Morphology
• PL (doped samples only)
– Absorption and emission spectra
• Gas adsorption
– Specific surface area
8
9
Crystallite sizes
Carrier gas flow rate (m3/h)
15 30 60
Feeding
flowrate
(mL/min)
75 15 16 15
150 16 15 15
300 16 16
• Uncomplexed precursor solution
• Calcined
10
Crystallite sizes
Carrier gas flow rate (m3/h)
15 30 60
Feeding
flowrate
(mL/min)
75 12 13
150 12
300 15 15
• Complexing agent: maleic acid
• Calcined
11
Crystallite sizes
Carrier gas flow rate (m3/h)
15 30 60
Feeding
flowrate
(mL/min)
75 14 17 14
150 15 18 14
300 17 19 16
• Complexing agent: EDTA
• Calcined
12
Yield
Carrier gas flow rate (m3/h)
15 30 60
Feeding
flowrate
(mL/min)
75 9 33 64
150 35 55 42
300 88 64 56
• Uncomplexed precursor solution
13
Yield
Carrier gas flow rate (m3/h)
15 30 60
Feeding
flowrate
(mL/min)
75 52 63 52
150 45 63 40
300 62 55 15
• Complexing agent: maleic acid
14
Yield
Carrier gas flow rate (m3/h)
15 30 60
Feeding
flowrate
(mL/min)
75 40 55 58
150 49 57 51
300 46 50 43
• Complexing agent: EDTA
15

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TKP 4190

  • 1. 1 Spray Pyrolysis of Oxide Materials Master Thesis in nanotechnology Student: Roger Moen Supervisor: Prof. Mari-Ann Einarsrud Co-supervisors: Prof. Tor Grande and Ruth Astrid Strøm Om du ønsker, kan du sette inn navn, tittel på foredraget, o.l. her.
  • 2. 2 Topic Prepare nanopowders by spray pyrolysis with varying chemical and process parameters and determine their effect on powder characteristics – Chemical parameter: complexing agent – Process parameters: precursor solution feeding rate and carrier gas flow
  • 3. 3 Previous work • Y2O3:Eu3+ • Precursor solution concentration – Little effect • Complexing agents – Affects reaction rate, tap density, crystallite size, morphology and emission spectrum
  • 4. 4 Materials • Y2O3 and Y2O3:Eu3+. • Precursors: Y(NO3)3 and Eu(NO3)3. • Complexing agents: Maleic acid and EDTA
  • 5. 5 Applications Y2O3 • Refractory coatings • Precursor for many materials (e.g. superconductors) • Host material for many RE elements • Sensors • Additive in paints and plastics Y2O3:Eu3+ • Red emitting phosphor in displays and biological imaging
  • 6. 6 Preparation • Steps – Atomization of precursor solution – Evaporation of solvent – Thermolysis
  • 7. 7 Characterization • TGA • XRD – Crystallite size – Purity • SEM – Morphology • PL (doped samples only) – Absorption and emission spectra • Gas adsorption – Specific surface area
  • 8. 8
  • 9. 9 Crystallite sizes Carrier gas flow rate (m3/h) 15 30 60 Feeding flowrate (mL/min) 75 15 16 15 150 16 15 15 300 16 16 • Uncomplexed precursor solution • Calcined
  • 10. 10 Crystallite sizes Carrier gas flow rate (m3/h) 15 30 60 Feeding flowrate (mL/min) 75 12 13 150 12 300 15 15 • Complexing agent: maleic acid • Calcined
  • 11. 11 Crystallite sizes Carrier gas flow rate (m3/h) 15 30 60 Feeding flowrate (mL/min) 75 14 17 14 150 15 18 14 300 17 19 16 • Complexing agent: EDTA • Calcined
  • 12. 12 Yield Carrier gas flow rate (m3/h) 15 30 60 Feeding flowrate (mL/min) 75 9 33 64 150 35 55 42 300 88 64 56 • Uncomplexed precursor solution
  • 13. 13 Yield Carrier gas flow rate (m3/h) 15 30 60 Feeding flowrate (mL/min) 75 52 63 52 150 45 63 40 300 62 55 15 • Complexing agent: maleic acid
  • 14. 14 Yield Carrier gas flow rate (m3/h) 15 30 60 Feeding flowrate (mL/min) 75 40 55 58 150 49 57 51 300 46 50 43 • Complexing agent: EDTA
  • 15. 15