Micro-XRF EDS can be used in a complementary manner with SEM/EDS to obtain semi-quantitative compositional analysis for identification of alloy types at elemental concentrations above 100 ppm (0.01 wt%). A presentation by Element Materials Technology expert Dan DeMiglio.

1. The Use of Micro-X-ray Fluorescence in an
SEM for Failure Analysis Investigations of
Aerospace Materials
Daniel S. DeMiglio
Senior Metallurgical Engineer, Element Charlotte
June 19, 2012 Aeromat 2012 Conference & Exhibition

2. X-ray Fluorescence (XRF)
June 19, 2012 Aeromat 2012 Conference & Exhibition

3. Electron Beam Sample Interaction
June 19, 2012 Aeromat 2012 Conference & Exhibition

4. X-ray Sample Interaction
Sample
X-ray Spectra Acquisition for microXRF/EDS:
40 micron spot size
35°
35°
10 mm working distance
70° 60 secs acquisition
Sample 50 keV Incident X-ray Beam
(Ag Target 1.0 mA 50 W)
XRF
June 19, 2012 Aeromat 2012 Conference & Exhibition

5. Hitachi S-3700N SEM-IXRF Systems Digital Imaging and EDS Microanalysis
Micro-XRF/EDS Using Fundamental Parameter Software (FP)
June 19, 2012 Aeromat 2012 Conference & Exhibition

6. Hitachi S-3700N VP-SEM Sample Chamber
X-ray Gun
X-ray Detector
SD X-ray Detector: 10 mm2 detector area; 0.3 micron window coated with 30 nm Al film
Micro-Focus Capillary X-ray Gun: 40 micron spot size; 50 keV X-ray beam
June 19, 2012 Aeromat 2012 Conference & Exhibition

7. Copper Alloy
E-Beam
X-Beam
June 19, 2012 Aeromat 2012 Conference & Exhibition

8. Aluminum Alloy
E-Beam
X-Beam
June 19, 2012 Aeromat 2012 Conference & Exhibition

9. Nickel Alloy
E-Beam
X-Beam
June 19, 2012 Aeromat 2012 Conference & Exhibition

10. Weld Analysis (GTAW)
AA 2024-T3
E-Beam Aluminum Alloy X-Beam
June 19, 2012 Aeromat 2012 Conference & Exhibition

11. Metal Shaving
X-Beam
June 19, 2012 Aeromat 2012 Conference & Exhibition

12. Debris Analysis
X-Beam E-Beam
June 19, 2012 Aeromat 2012 Conference & Exhibition

13. Tool Steel Analysis
X-Beam E-Beam
Si V Cr Mn Fe Ni Mo W
(wt%)
X-Beam 0.86 1.72 4.10 0.28 82.05 0.13 4.47 6.38
E-Beam 0.6 1.9 4.0 0.2 76.3 0.2 8.2 8.7
AISI M2 0.20-0. 1.75-2.2 3.75-4.5 0.15-0.4 Bal 0.30 4.50-5.5 5.50-6.7
45 0 0 0 max 0 5
June 19, 2012 Aeromat 2012 Conference & Exhibition

14. Electrical Contact
X-Beam E-Beam
June 19, 2012 Aeromat 2012 Conference & Exhibition

15. Particles Removed from Grease
X-Beam E-Beam
June 19, 2012 Aeromat 2012 Conference & Exhibition

16. Cracked Driver Tool
June 19, 2012 Aeromat 2012 Conference & Exhibition

17. Summary
Micro-XRF EDS can be used in a complementary manner with SEM/EDS to obtain semi-
quantitative compositional analysis for identification of alloy types at elemental
concentrations above 100 ppm (0.01 wt%)
Greater sensitivity at high atomic numbers; low background
Aerospace microanalysis applications include: contamination analysis, wear debris
identification, alloy segregation, weld analysis, nondestructive coating thickness
measurement
For best results Micro-XRF EDS microanalysis must be performed with certified alloy
standards (IXRF Systems - FP EDS microanalysis software)
Small sample sizes (<1 gram) that cannot be otherwise analyzed by bulk chemistry
techniques (OES, ICP, WDS-XRF) are well-suited to Micro-XRF EDS microanalysis
Core particle compositions can be characterized by Micro-XRF EDS
Care must be taken to ignore scattering and artifact X-ray peaks that are not from the
area of interest
June 19, 2012 Aeromat 2012 Conference & Exhibition