1. VERONICA POLICHT JOHANNA NELSON, MENTOR OFFICE OF SCIENCE, SULI SLAC NATIONAL ACCELERATOR LABORATORY Researching and Designing a Sample Heater for Beam Line 6-2c

2. Facilities: Beam Line 6-2c G.J. Nelson, et al., 2011, AIP, vol. 98, p. 173109 Schematic of the Transmission X-ray Microscope optics

3. 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.

4. 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

5. 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

6. Method Desired Characteristic ????? Controlled Confined Measurable Temperature Range (50 - 500 ºC) Removable Size Range Possible Sample Types Cost Level of In House Manufacturing Difficulty

7. Desired Characteristic Infrared Heat Lamp Infrared LaserSilicon-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 HeatersResistive Heaters o Investigate various heating types o Research heating methods via scholarly databases o Investigate commercially available heaters; speak with engineers o Construct decision matrix based upon findings o Draft a preliminary 3D model

8. Desired Characteristic Infrared Heat LampInfrared LaserSilson Silicon-based MEMS Omega Kapton®-based Resistive Mellen Cylindrical Ceramic-based Furnace ControlledPower supply ConfinedMust use optics to confine heat to small spot size Use 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 MeasurableCan 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 calibrate; use a thermocouple Temperature Range (50 - 500 ºC) Some IR heaters can heat samples to 700 ºC Can heat above 1200 º CBelow 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 ºCBelow 1100 ºC RemovableWould 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 RangeSize 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 Flat samples onlyFlat or gently curved samples only Cylindrical samples only; those in capillary tubes Cost>$239.00> $15,000$81.40$31.00N/A Level 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

9. Results ControlledConfinedMeasurable Temperature Range (50 - 500 ºC) Removable Size Range Possible Sample Types Cost Level of In House Manufacturing Difficulty Weight122313133 Rank (1-best, 5-worst) Weighted Rank Heat Lamp15354433472 Laser11115515559 Silicon12421152343 Kapton13521221241 Ceramic1414335 143 411 st Choice: Kapton-based resistive 2 nd Choice: Ceramic-based resistive 43

10. 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 cylinder OMEGA Kapton Insulated Flexible Heater: www.omega.com Mellen Company Half-cylinder Ceramic Heater: www.mellencompany.com

11. SketchUp: OMEGA Kapton Flexible Heater

12. SketchUp: In-house Macor-Ceramic Heater

13. Acknowledgments I would like to thank Johanna Nelson Joy Hayter, Mike Toney, & Sumohan Misra e r SLAC and SULI staff, and the Department of Energy