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