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Applications of Dispersive Raman Microscopy to Failure Analysis

Spring 2004 European Seminar Series

Acknowledgements
Raman spectra and images supplied by
John Wolfgong, Ph.D., Raytheon, McKinney, Texas

Collected on a Nicolet Almega with 532 and 785 nm lasers

The Role of Raman in Failure Analysis


Raman fills an important gap in the failure analysis lab
Provides molecular information on very small spots
Small particles becoming increasingly more important

SEM
Provides good image analysis and elemental information Often this is not enough to identify small organic particles or to diagnose failure modes in organic materials

FT-IR
Provides good molecular information Limited to about 10 m in size

Raman extends the limit for molecular materials to 1 m

Nondestructive Plus Sampling


Raman allows samples to be analyzed as is
Often you do not want to damage sample or the substrate
Nondestructive Plus

Can even measure directly through glass or plastic packaging

Real Life Examples


Failure analysis encompasses a wide range of samples and information needs. We will examine a few specific real-life examples to see how Raman was applied to solve the problem.

Braze Joint Crack Analysis


Problem statement: Determine at what point in the process the crack appeared. Crack was easily confirmed by visual inspection. Then further analyzed by embedding it in epoxy and cross sectioning it to determine the extent of the crack by visual inspection. The part goes through a processing step where it is coated with at Silicone conformal coating. If the crack had appeared before the coating it should be filled with Silicone conformal material, otherwise it would be expected to be empty. This could not be established with certainty by visual inspection.

Braze Joint Crack Analysis


Raman was used to analyze the contents of the crack.
532 nm laser was used no fluorescence. A reference spectrum of the epoxy potting compound was also collected to insure that it was not confused.

Potting Compound Reference

Conformal Coating Reference

Spectrum Obtained from within Area 2

Spectrum Obtained from within Area 1

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Braze Joint Crack Analysis


Potting Compound Reference

Conformal Coating Reference

Spectrum Obtained from within Area 2

Spectrum Obtained from within Area 1

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Raman easily confirmed that the crack occurred before the coating step.
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Troubleshooting Magnetically Actuated Clutches


Problem statement: Clutches passed all inspection tests and were found to be inoperable after 6 months of storage. Clutches could be freed up by pulling the clutches loose with pressure. What is causing the problem with the clutches?

Troubleshooting Magnetically Actuated Clutches


Initial investigation applied FT-IR microscopy to the lubricant
Turned up spectra of particles exhibiting a strong carbohydrate spectrum. First course of investigation pointed to possible sources of cotton fiber contamination
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Absorbance

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Troubleshooting Magnetically Actuated Clutches


Continued investigation revealed distinctly crystalline images
FT-IR spectrum diagnosed as sucrose at this point Diagnoses was met with considerable skepticism as there was no known means for sucrose to be introduced into the product.

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Troubleshooting Magnetically Actuated Clutches


Raman spectroscopy utilized to support FT-IR diagnosis
Raman spectrum is less sensitive to the -OH end groups in carbohydrates and readily identified the material as sucrose
Raman reference spectrum of cellulose

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Raman shift (cm-1)

Raman reference spectrum of sucrose

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Raman shift (cm-1)

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Troubleshooting Magnetically Actuated Clutches


Clear Crystal on Spring (2868) - [Analysis using 532 nm laser]

Crystal on Gray Outer Ring After Removal of Clutch (2868) - [Analysis using 532 nm laser]

Solid crystal (2868) - [Analysis using 785 nm laser]

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Raman shift (cm-1)

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Troubleshooting Magnetically Actuated Clutches


Conclusion: Armed with a confirmed diagnosis, further inquires as to the source of the sucrose with the vendor uncovered that production crews were allowed to drink coffee on the line and that they had a sugar dispenser nearby. Slow crystallization of the sugar caused the failures.

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Analysis of Residual Contaminant


Problem statement: A small residue measuring about 1x4 m was discovered in a cavity formed between various stackup layers during manufacture of a semiconductor device on 6 Silicon wafers. Investigators were asked to determine what the residue was without disturbing the residue or the wafer in any way.

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Analysis of Residual Contaminant


Initially tried FT-IR
Failed to produce results due to the small spot size and interference from specular reflection off of the Si substrate

Raman pursued next


Failed initially with a 532 nm excitation because of overwhelming fluorescence from the sample Switching to a 785 nm laser yielded an excellent spectrum

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Analysis of Residual Contaminant


Conclusion: Searching against a reference library revealed the residue was a polyimide
Residue

Polyimide Reference Spectrum

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Summary
Raman has a lot to offer to the failure analysis lab today
Traditionally Raman systems tended to be rather difficult to use and required lots of maintenance Modern Raman systems such as the Almega XR are part of a new generation designed to be productive tools requiring very little training or maintenance It is likely that they will quickly take their place as one of the primary analysis techniques for failure analysis due to their
Applicability to small particles Insensitivity to substrates Applicability to nondestructive plus analysis

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