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User Facility of the Sustainable Energy Initiative
Galyna KrylovaResearch Assistant Professor
Dept. of Chemistry and Biochemistry
University of Notre Dame
SEI SeminarAugust 29, 2011
Actinide Facility
• Instruments- Single Crystal XRD- Powder XRD- Calorimeter- In-situ/Ex-situ Raman
Single Crystal XRD (Bruker)• Details and capabilities:- CCD area detector
- Low temperature (liquid nitrogen stream) device.
- Microfocus sealed tube
- Latest type of Montel mirror.
- Mo Kα radiation (wavelength of 0.71073 Å). -SOL-XE energy dispersive X-ray detector
• Typical uses: - Determination of crystallographic structure of novel organic,
inorganic, and organometallic materials
• Anticipated cost to use:
• Availability to Actinide - 100%• Current Location- 303 Stinson-Remick• Permanent Location – 303 Stinson-Remick
• Picture of instrument
• Picture of results from instrument
Unit ND Assisted ND Unassisted External sample 50 90 120
Powder XRD (Bruker)• Details and capabilities:- SOL-XE energy dispersive X-ray detector
- Rotating sample stage.
- Vertical goniometer, Theta/2Theta or Theta/Theta geometry
- Max. usable angular range: 2Theta ≤ 168°
- Smallest addressable increment: 0.0001°
- Maximum angular speed: 20°/s
• Typical uses: - Routine crystallographic phase identification
• Anticipated cost to use:
• Availability to Acinide - 100%• Current Location- 303 Stinson-Remick• Permanent Location – 303 Stinson-Remick
• Picture of instrument
• Picture of results from instrument
Unit ND Assisted ND Unassisted External scan 42 15 120
20 30 40 50 60 70 80 901000
10000
100000
Inte
nsity,
a.u
.)
Pt
Pt
Pt
Pt
Au
Au
Au
branched Pt / AuCl3
2
Au
Si
Calorimeter (Setaram)• Details and capabilities: - Isothermal Differential Heat Flow
- Temperature range: 500 ˚C – 1000 ˚C.
- Temperature Accuracy +/- 0.1%
- Enthalpy accuracy +/- 1%
- Resolution: 50 µW
- Cells: 28 ml (quartz cell) - 20 ml (platinum crucible)
• Typical uses: - The heats of formation of complex actinide materials containing transuranic elements.
- Drop solution calorimetry with gas flow above the sample and/or gas bubbling through the molten solvent,
- Direct reaction calorimetry to form alloys and compounds,
- Aluminothermic and other oxidation-reduction reactions,
- Gas-solid, gas-liquid, and liquid-liquid reactions.
• Anticipated cost to use:
• Availability to Actinide - 100%• Current Location- 303 Stinson-Remick• Permanent Location – 303 Stinson-Remick
• Picture of instrument
• Picture of results from instrument
Unit ND Assisted ND Unassisted External sample 140-185 30-82 ~625
Raman (Bruker)• Details and capabilities:- Spectral range 100-3100cm-1
- Resolution 5cm-1
- Working distance 60mm
- Laser power 400mW
- Max. power at sample 280mW
- Video camera for in-situ observation
- Two optical fiber probes
- Temperatures up to 220°C
• Typical uses: - In-situ studies of reactive intermediates in solution phase syntheses- Ordinary Raman uses for the second probe
• Anticipated cost to use:
• Availability to Actinide - 100%• Current Location- Not delivered • Permanent Location – 303 Stinson-Remick
• Picture of instrument
• Picture of results from instrument
10060011001600210026003100
Wavenumber cm-1
Unit ND Assisted ND Unassisted External
hour 75 25 100
day 430 50 680