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A leading engineering & scientific consulting firm dedicated to helping our clients solve their technical problems.

Sweating the small stuff…Impact of Nanotechnology on Failure Analysis

Eric Guyer, PhD, PE

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What does “Nano” mean?

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“Nano” Is…

micro

One billionth of a meter

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Nano vs. Billion

$1 $1,000 $1,000,000 $1,000,000,000

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What is Nanotechnology?

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Nanotechnology is NOT “Y2K-ish”

Nanotechnology is an emerging technology that has the potential to be used in a broad array of FDA-regulated products, including medical products, foods and cosmetics…

These nanomaterials can have different chemical, physical, or biological properties than their conventionally-scaled counterpart materials used in many products regulated by FDA.

http://www.fda.gov/Food/GuidanceComplianceRegulatoryInformation/GuidanceDocuments/ucm300914.htm

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The Hype…

http://www.howstuffworks.com

https://www.futureayacentre.org/nano-robot-will-fight-tumor-with-cancer/

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The Best We Can Do In 3D

Lucas R. Meza. Proceedings of the National Academy of Sciences Sep 2015, 112 (37) 11502-11507; DOI:10.1073/pnas.1509120112

25 µm

10 µm

50 µm

20 µm20 µm20 µm20 µm

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Unconventional Nanofabrication

Atomic force microscope tip “pen” and solution “ink”

▪ Sub-50-nm patterning resolution

▪ Development of parallel patterning capability

Al2O3 SnO

Su et.al., J. Am. Chem. Soc. (2002)

https://commons.wikimedia.org/wiki/File:ClassicDPN_mech.png

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What “Nano” Can We Do?

1–D: particles

2–D: coatings

3–D: structures

Already in use…

Progress, but still

limited in capabilities

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Why is Nano Important?

We Live in a Material World

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Materials Discovery

▪ Pottery ~20,000 years

▪ Metals ~8,000 years

▪ Bronze age ~5,500 years

▪ Iron age ~3,000 years

▪ Polymers ~150 years

▪ Nanomaterials ~30 years

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IBM: Atomistic Engineering

www.ibm.almaden.com

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1) Properties Change

New Materials…

2) Surface Area

• Optical (e.g. color, transparency)• Mechanical (e.g. hardness, toughness)• Chemical (e.g. reactivity, reaction rates)• Electrical (e.g. resistivity)

• Footprint: more devices in smaller space• Surface area to volume (catalysis, drug

delivery, absorption, diffusion)

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The Color of Money…

Kumar, Nature Protocols (2008)

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“Quantum Dots” – Biomarkers / Cell Targeting

Researchers at the Winship Cancer Institute (part of the Emory-Georgia Tech Center for Cancer Nanotechnology

Excellence) are working to develop clinically viable ways to detect biomarkers that indicate a patient's risk of developing

cancer. They have developed a nanotechnology-based method to detect a number of molecular markers at the same time

("multiplexed") on a single tissue specimen with the use of quantum dot particles as fluorescent stains. In the above

image, the method is used with colon tissue in an effort to identify markers which are predictive of increased risk of

developing colon cancer. Credit: Seema Harichand-Herdt, M.D.; Vaunita Cohen; Ruth O'Regan, M.D.; and Robin

Bostick, M.D.

www.nih.gov

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“It’s NOT In Typical Consumer Products”

Why Do Attorney’s Care?

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00M61SF.000 A0T0 0609 EG01Source: Woodrow Wilson International Center for Scholars; www.nanotechproject.org

Nano-Enabled Consumer Products

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Nano-Enabled Consumer Products

Forster, et al, Nanotechnology in the market: promises and realities, Int. J. Nanotechnol.,2011

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Automobiles…

www.nanowerk.com

http://beaudaniels.com/generic-car-update

Fluid Level Sensors

Engine control

sensors

Shaft torque

sensor

Climate control

sensor, central

locking, mirror

positioning, etc

Tire rubber

and tire

pressure,

temperature

sensors

Battery

components

Antiglare coatings

Suspension

positioning systems

Gyroscopes and

accelerometers for

positioning and air bags

Seat occupancy

Brightness

adjusting

mirrors

On-board

electronics

Steering position

sensor

Shaft torque

sensor

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Coatings – Automobiles

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Smudge Resistant Coatings

https://d3nevzfk7ii3be.cloudfront.net/igi/MFXGOCaMC1OJxWAk.huge

http://www.aculon.com/hydrophobic-coatings.php

Hydrophobic coatings used

in these applications are

generally 2 to 4 nm thick!

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Cosmetics

▪ Large ZnO particles

▪ Block UV light

▪ Scatter visible light

▪ Nano ZnO particles

▪ Block UV light

▪ Cannot scatter visible light

▪ (too small) → transparent

http://www.nano.org.uk/

“Traditional” ZnO

Sunscreen is white

Nanoscale ZnO

Sunscreen is clear

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Silver Nanoparticles – Bacterial Cell Death

Forster, et al, Nanotechnology in the market: promises and realities, Int. J. Nanotechnol.,2011

http://www.nanosilver.eu

http://news.rice.edu/2012/07/11/ions-not-particles-make-silver-toxic-to-bacteria-2/

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Implications on

Failure Analyses

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Expert Testimony

Frye (1923)

▪ Theory and methodology of expert testimony must be generally accepted within scientific community

Daubert (1993)

▪ Scientific expert testimony should be reliable

Kumho (1999)

▪ Daubert scrutiny may apply to all experts, whether scientific or non-scientific

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FRE Rule 702…

1) The expert’s scientific, technical, or other specialized knowledge will help the trier of fact to understand the evidence or to determine a fact in issue;

2) The testimony is based on sufficient facts or data;

3) The testimony is the product of reliable principles and methods; and

4) The expert has reliably applied the principles and methods to the facts of the case

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Daubert Challenges to Experts

http://www.pwc.com

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Daubert Exclusions

http://www.pwc.com

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How Do I Attempt to Avoid a Challenge?

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Applying Daubert

1. Has the theory or technique been scientifically tested?

2. What is its known rate of error?

3. Is it generally accepted by the relevant scientific community?

4. Testimony concerns matters growing naturally and directly out of

research the expert has conducted independent of the litigation?

5. Has it been reviewed by other practitioners?

6. Unjustifiably extrapolate from an accepted premise to an unfounded

conclusion?

7. Adequately accounted for obvious alternative explanations?

8. Expert is being as careful as he would be in his regular professional

work outside paid litigation consulting?

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Basic FA Process

1) Examine the product

2) Collect data

3) Microscopy / non-destructive characterization

4) Develop protocol for destructive characterization (mechanical, chemical, thermal, electrical)

5) Develop hypotheses & test

6) Synthesize info → Conclusion/opinions

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How do I Avoid Challenges?

Testing hypotheses AND analytical techniques

▪ Experts develop joint testing protocol

▪ Standards

▪US standards such as ASTM, ANSI, ASME, etc.

▪ International standards: NACE, ISO, etc.

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ASTM Standards for Nanomaterials

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ASTM Terminology

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How do I Avoid Challenges?

▪ Literature review

▪ Is there (dis)agreement on the “academic” methods?

▪ If so, consider multiple analytical techniques

▪ Statistical analyses

▪ Of the test for rate of error

▪ Of results for significance

▪ Reporting

▪ Methodology section in each report – and provide very specific details re: testing if conducted

▪ Relate it back to basic / fundamental scientific, physical and chemical principles

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Analytical Means Enable

Failure Analysis

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Glass-Metal Feed-Through

Example photographs taken from

internet – following work not

conducted on these devices

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Glass

Platinum pin

Titanium

Titanium

Glass-Metal Feed-Through: In Cross-Section

Glass

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Gla

ss

Glass-Metal Feed-Through: In Cross-Section

Glass

Titanium

Oxide

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375nm

Titanium

Oxide

Porosity in

oxide layer

Interface

porosity

Glass-Metal Feed-Through: In Cross-Section

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Material Composition

O Al

Ca Co

Zr Ba

Zn

Si

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Closing

▪ Nanotechnology is here to stay

▪ Open to challenges without careful planning

▪ Significantly advances general FA capabilities

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Thank you!