2006 International Conference on

Nanotechnology, April 26-28, 2006

Atlanta, GA

Using a Defocused Argon Ion Beam to

Prepare Coated Paper Cross-Sections

J-M RodierProject ManagerSappi Fine Paper NA sappi

Presentation AgendaPresentation Agenda

• Background Cross-Section Preparation• Description of Non-Focused Technology• Sample Prep/Instrument Parameters• Images• Conclusion

Background

Cross-Section Preparation

• Freeze Fracture• Embedding• Focused Ion Beam

Freeze-Fracture

• Method– Use liquid nitrogen to freeze sample– Razor blade to cut sample

• Positive– Quick and easy

• Negatives– Difficult to obtain information– Physical contact

Embedding

• Method– Sample embedded in resin

• Usually 12-36 hrs– Cut using microtome

• Diamond• Glass knife

– Etch sample• Chemicals to etch resin from sample

Embedding

• Positives– Clean coating image– Large Areas (Montage)

• Negatives– Labor intensive– Physical contact the sample– Cannot observe

• Fiber layer without sample damage• Ink/Varnish/Coating Interface well• Coating packing due to resin

Focused Beam technology

• Published Reports• Positives

– Clean non-physical cut– No heat damage– Ability to prepare for other techniques

• Negatives– Small Area– Physically Manipulate sample– Equipment Costs

Defocused Ion Beam Technology

Defocused technology

• Argon Ion Beam (Non-contact)• Uses a mask to block beam• No foreign material required• Larger area than focused ion beam• Not labor intensive• Drawbacks

– Sample prep time 8-10 hours• Working on 3-6 hours

Sample Preparation

• Si Wafers needed as heat sink• Sandwich mode

– Lightweight samples– Burn through top wafer– Taped at far edge

• Offset Mode– Heavyweight samples– Burn through sample– Taped at far edge

Si/Sample Sandwich

Sample Holder

Mask and Sample Holder

Instrument Parameters

• JEOL SM-09010 Cross Section Polisher (CP) – Argon Beam 5-6 kV

• JEOL 5900 LV – BEI– Acceleration voltage adjusted for image

quality– Spot size adjusted for image quality

Images

Si Wafer

Paper

Si Wafer

Ink/Varnish

Coating

Fiber

Coating

Ink/Varnish

Conclusion

Conclusion

• De-focused technology useful• In situ analysis of base sheet and coating • Analysis of felt and wire side on same

sample • Not labor intensive • Negative

– Sample Throughput– Equipment Costs (Cheaper than FIB)

Acknowledgements

• Mike Robinson - coauthor• JEOL

Thank You PRESENTED BY

J-M RodierProject MangerSappi Fine Paper NAjm.rodier@sappi.com

Questions