determining metals cleanliness using sem-eds

©Gateway Analytical LLC. 2016©Gateway Analytical LLC. 2016

Determining Metal Cleanliness Using SEM-EDS

August 24, 2016

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About Gateway AnalyticalLocated in Gibsonia, Pennsylvania, U.S.A.

Particulate Identification Services

Detailed Report Characterizing and

Identifying particulate

Customer Support to help identity the

source of contaminates.

cGMP-compliant | FDA Registered & Inspected | ISO 17025 & ISO 9001

Standard five day turnaround and available one day turnaround!


About Gateway AnalyticalLocated in Gibsonia, Pennsylvania, USA

Particulate happens, but that shouldn't stop your progress.

Our focus is to remove the hurdles involved with identifying foreign particulate and guide our

customers to fast remediation.


Meet Today’s Presenter

Angela FlowersScientist

Gateway [email protected]

• Angela Flowers currently serves as a Scientist at Gateway Analytical

• Angela’s background centers around the identification, sizing, and characterization of particulate

• She typically uses automated methods of analysis, including CCSEM (computer controlled SEM / EDS) and automated Raman / LIBS technologies

• Since joining Gateway Analytical in 2015, Angela has been key in developing, implementing and incorporating wear debris analysis as a service offering of the laboratory

• She has a Bachelor of Science degree in Forensic Science from Seton Hill University

©Gateway Analytical, LLC 2015. All Rights Reserved. Some Gateway Services may be protected by U.S. issued patents and pending patent applications


How is Cleanliness Analyzed?



• ISO 4406: Cleanliness code (lubricant)• ISO 4407: Contamination counting with optical

microscope• ISO 17853: Wear of implant materials• ISO 16232:Cleanliness of components of fluid

circuits– Automobile OEMs typically use their own version of

this analysis and VDA19

ISO Guidelines



Part1: VocabularyPart2: Method of extraction of contaminants by agitationPart3: Method of extraction of contaminants by pressure rinsingPart4: Method of extraction of contaminants by ultrasonic techniquesPart5: Method of extraction of contaminants on functional test benchPart6: Particle mass determination by gravimetric analysisPart7: Particle sizing and counting by microscopic analysisPart8: Particle nature determination by microscopic analysisPart9: Particle sizing and counting by automatic light extinction particle counterPart10: Expression of results

ISO16232 Guidelines



Cleanliness Codes Guidelines



Analysis Types

• Gravimetric– Provides weight only. No particle size information

• Particle Counters– Provides particle count and size information

• Optical Microscopy– Provides particle count, size and shape information

• SEM/EDS– Provides particle count, size, shape and elemental

composition



Poll Question

• Are you currently using ISO16232 or VDA19 analysis internally?– Yes– No – Not Sure



What is SEM-EDS?



• Scanning Electron Microscopy – Energy Dispersive Spectroscopy

• Morphology and elemental composition of materials

SEM-EDS

5000 µm 200 µm

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Cou

nts

800

600

400

200

0

C

O

Na

AlSi

K Ca Ti

Ti

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• A microscope that uses a beam of electrons instead of a beam of light

• The electrons interact with the sample • Certain signals come off of the sample, and

give us different types of information

SEM-EDS



Principles of an SEMTungsten

Electron Source “Gun Cap”

ElectromagneticOptics

Column

Electron Beam Electron Detector

Image Acquisition



Automated SEM/EDS



• The analysis of a couple of ‘characteristic’ features may not represent the whole

• Find different types of features and the population distribution among the different types of features

• The analyst may have to examine hundreds of fields and thousands of features to find a single interesting or unusual feature

• When the analyst is selecting a sub-set of the observed features, it is easy for an analyst’s expectations to bias the results

Why use Automated SEM/EDS?



What are the sample requirements?• What are the Features of interest?• Background needs to provide good Atomic Number contrast from

features of interest



Analyze EDS

Al2O3 particleRepeat (typically 500 – 10,000 times)

Collect Sample

Individual parts or Assemblies are collected

Prep Sample

Parts are rinsed and particles are collected on a filter patch

Load

Sam

ple

Generate Report

Composition

Match Against Classification Rules

19Confidential



Thresholds

• How to determine what will be considered a feature



Poll Question

• What analysis technique are you currently using at your site.– No analysis technique– Particle Counter– Optical Microscopy– SEM/EDS– Gravimetric



Automated SEM/EDS for Automotive Industry



What is CleanCHK?

• Uses automated SEM/EDS technology to monitor the cleanliness of automotive parts

• Follows current cleanliness standards (VDA-19, ISO16232, OEM standards based on ISO16232)

• Provides the size, shape, and chemistry of each particle. This can be used to locate abrasive or controlled particles



Who Uses CleanCHK?

• Automotive OEMs use CleanCHK to monitor incoming parts from suppliers as well as to monitor assemblies on the production floor

• OEMs create their own standard based on VDA-19 and ISO16232. These standards may be passed onto their suppliers

• First- and second-tier suppliers use CleanCHK to monitor the cleanliness of their parts before they are submitted to the OEMs



Automated SEM/EDS Reporting



ISO16232 Report



Chemistry Report



Automotive-Automated SEM-EDS Data:

Particle Information

50 µm 50 µm 50 µm 50 µm

50 µm 100 µm 50 µm 50 µm

50 µm 50 µm 50 µm 50 µm

100 µm 50 µm 50 µm 50 µm


Contact Us & Follow-up

Get Insights from our Blog:www.gatewayanalytical.com/blog

Contact InformationDavid ExlineVice PresidentGateway [email protected]: 724-443-1900 x106

Angela [email protected]: 724-443-1900 x103

Paige CohenSales Development [email protected]: 724-443-1900 x129

Angus MillerGlobal Marketing [email protected]: 724-443-1900 x132

@GatewayTweets

mailto:[email protected]





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