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VERONICA POLICHTJOHANNA NELSON, MENTOR
OFFICE OF SCIENCE, SULISLAC NATIONAL ACCELERATOR
LABORATORY
Researching and Designing a Sample Heater for Beam Line
6-2c
Facilities: Beam Line 6-2c
G.J. Nelson, et al., 2011, AIP, vol. 98, p. 173109
Schematic of the Transmission X-ray Microscope optics
Problem: Why Sample Heater?
Biological & chemical events occur at temperatures higher than room temperature (RT) Human body temperature: 37.0 °C (RT is 20-25 °C) In situ conditions for some reactions
Material morphology & behavior at elevated temperatures Material stress and failure
Implementing a sample heater for TXM imaging broadens the temperature range a sample can
be observed in, making the possible sample conditions more dynamic.
Sample Heaters: Desired Characteristics
In terms of heat character: Controllable Confined Measureable Perform between/up to 50-500 °C
Heater apparatus: Removable Size considerations
Adaptable to several sample types Ease of ability to manufacture and/or
acquire necessary parts Relatively Low Cost
Available space
Example Samples
• Sealed capillary with catalytic(?) sample within• cylindrical
• Battery cell sample, for imaging is placed between holderplates • Relatively flat
Holderplates designed by Johanna Nelson for use in imaging battery samples at Beam Line 6-2c
Method
Desired Characteristic
? ? ? ? ?
Controlled
Confined
Measurable
Temperature Range (50 - 500 ºC)
Removable
Size Range
Possible Sample Types
Cost
Level of In House Manufacturing Difficulty
Desired Characteristic
Infrared Heat Lamp
Infrared Laser Silicon-based MEMS
Kapton®-based Resistive
Ceramic-based Resistive
Controlled
Confined
Measurable
Temperature Range (50 - 500 ºC)
Removable
Size Range
Possible Sample Types
Cost
Level of In House Manufacturing Difficulty
Method
Infrared Heaters Resistive Heaterso Investigate various heating typeso Research heating methods via
scholarly databaseso Investigate commercially available
heaters; speak with engineerso Construct decision matrix based upon
findingso Draft a preliminary 3D model
Desired Characteristic
Infrared Heat Lamp Infrared Laser Silson Silicon-based MEMS
Omega Kapton®-based Resistive
Mellen Cylindrical Ceramic-based Furnace
Controlled Power supply Power supply Power supply Power supply Power supplyConfined Must use optics to confine
heat to small spot sizeUse optics to manipulate laser beam; already small
spot size
Heater region is 0.5mm x 0.5mm; high drop off from electrode pattern to outer
silicon
Heat is confined to electrode region; heating
area begins 3.17 mm (1/8”) from outer edge of heater
Confined within the cylinder; holes necessary
for x-ray transmission through sample may be concern for stray heat
Measurable Can calculate temperature incident on sample face and use a thermocouple on IR
source
Calculate the temperature at the sample interface using
the Planck radiation function; use an imaging
spectrograph
Can calculate the local resistance; calibrate the
heater; use a thermocouple on the heater face
Can calculate the local resistance; calibrate the
heater; use a thermocouple on the heater face
Can calibrate; use a thermocouple
Temperature Range (50 - 500 ºC)
Some IR heaters can heat samples to 700 ºC
Can heat above 1200 º C Below 400 ºC; currently use a Au electrode, in the
process of R&D for a Pt electrode which would
operate at higher temperatures
Below 200 ºC Below 1100 ºC
Removable Would be installed off-stage or on the side of the TXM
Installed off TXM; would be difficult to remove and
install
Placed with sample on electrode side; removable
Placed on sample, side doesn’t matter; removable
Placed around sample; depending upon the model would be clamped around
or slid over the sample
Size Range Size of IR heaters varies greatly; estimate size would
be a 10” cube
Requires a rather large optical stage as well as several satellite data-
gathering components; very large and bulky
Minimum dimensions are 10 mm x 5 mm x 0.5 mm
(height x width x thickness)
Minimum size 12.7 mm x 12.7 mm (0.5” x 0.5”)
Minimum diameter 19.05 mm (0.75”), any length
Possible Sample Types
All; difficulty for those to be rotated for tomography
All; difficulty for those to be rotated for tomography
Flat samples only Flat or gently curved samples only
Cylindrical samples only; those in capillary tubes
Cost >$239.00 > $15,000 $81.40 $31.00 N/ALevel of In House Manufacturing Difficulty
High; optics and fabrication of cassegrain reflector
High; optics and mounting large components
High; nanofabrication required
Medium; require nanofabrication but less
difficult than silicon-based
Medium; require machining Macor ceramic and
threading wire through
Results: Summary Table
Results
Controlled Confined MeasurableTemperature
Range (50 - 500 ºC)
Removable Size Range
Possible Sample Types Cost
Level of In House Manufacturing
Difficulty
Weight 1 2 2 3 1 3 1 3 3
Rank (1-best, 5-worst) Weighted
Rank
Heat Lamp 1 5 3 5 4 4 3 3 4 72
Laser 1 1 1 1 5 5 1 5 5 59
Silicon 1 2 4 2 1 1 5 2 3 43
Kapton 1 3 5 2 1 2 2 1 2 41
Ceramic 1 4 1 4 3 3 5 1 43
41
1st Choice: Kapton-based resistive
2nd Choice: Ceramic-based resistive
43
Conclusion
Two solutions:• For flat and gently
curved samples will implement a Kapton-based heater• Chose heater manufactured
by OMEGA
• For samples contained in a capillary will implement a ceramic-based cylindrical cylinderOMEGA Kapton Insulated Flexible Heater: www.omega.com
Mellen Company Half-cylinder Ceramic Heater: www.mellencompany.com
SketchUp: OMEGA Kapton Flexible Heater
SketchUp: In-house Macor-Ceramic Heater
Acknowledgments
I would like to thank • Johanna Nelson
• Joy Hayter, Mike Toney, & Sumohan Misra • er
SLAC and SULI staff, and the Department of Energy