The document provides an overview of techniques used to study the surface corrosion layers of copper, including optical microscopy, X-ray diffraction, X-ray photoelectron spectroscopy, Auger electron spectroscopy, X-ray excited optical luminescence, and scanning electron microscopy. The goal is to make copper corrosion layers and apply surface-specific techniques to study and compare the different layers.

1. It’s what’s on the outside that counts, true story!
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Promotor: Pieter-Jan Sabbe & Dr. A. Adriaens Bachelorstudents: Nils De Rybel, Nicky Huys, Maria Gomez Rodriguez

2. Outline
• Why study surfaces?
• Goal of project
• Corrosion layers of copper
• Spectroscopic techniques used
• Conclusion
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3. Goal
• Make copper corrosion layers
• Study surface specific techniques
• Apply surface specific techniques
• Compare the layers
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4. Why study surfaces?
Polymer biodegradation Surface tension control
Catalysis Adsorption, desorption
Sensors
Surface hardening Friction control
Behaviour determined
Applications
by surface
Corrosion
Crystal growth
Controlled release polymers
Optical recording media
Anti-reflection coatings
Magnetic recording media
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5. Corrosion of copper
Name Chemical formula
Cuprite Cu2O
Nantokite CuCl
Atacamite Cu2Cl(OH)3
Paratacamite Cu2Cl(OH)3
Tenorite CuO
Chalcokite Cu2S

6. Optical Microscopy

7. Optical Microscopy
• Cupper coupon:
• Chalcokite

8. Optical Microscopy
• Cuprite.
• Nantokite

9. Optical microscopy
• Atacamite.
• Paratacamite

10. Optical microscope
• Tenorite
• Chalcokite

11. X-ray Diffraction (XRD)

12. X-ray Diffraction (XRD)

13. X-ray Diffraction (XRD)
Paratacamite
Copper
Nantokite

14. X-ray Diffraction (XRD)
Paratacamite
Copper
Nantokite

15. X-ray Diffraction (XRD)
Chalcokite
Copper

16. X-ray Photoelectron Spectroscopy
(XPS)
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17. X-ray Photoelectron
Spectroscopy (XPS)
S-Probe Monochromatized XPS
spectrometer from Surface
Science Instruments (VG)
AlKα x-ray (1486.6 eV)
1x10-9 mbar
Analysis surface : 250 x 1000 μm
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18. Standard spectra
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19. Spectra
300000
Copper peaks
250000
200000
Intensity (CPS)
Tenorite (CuO)
150000 Nantokite (CuCl)
Cuprite (Cu2O)
100000 Chalcocite (Cu2S)
Paratacamite (Cu2Cl(OH)3)
50000
0
900 910 920 930 940 950 960 970 980 990
Binding energy (eV)
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20. Auger Electron Spectroscopy (AES)
Scanning depth is 1-5nm and
lateral resolution ~10nm
Sensitivity is about 1 to 100ppm
Sample conductive
Mutch more specific then XPS
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21. X-ray Excited Optical Luminescence
(XEOL)
• How it works
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22. X-ray Excited Optical Luminescence
(XEOL)
• Source
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23. X-ray Excited Optical Luminescence
(XEOL) Nantokite
Paratacamite(?)
20.00
18.00 Ref. Nantokite (CuCl)
16.00
Nantokite
Paratacamite(?)
14.00
Normalized Intensity
12.00
10.01 Ref. Paratacamite (Cu2Cl(OH)3)
08.01
06.01
04.01
02.01
00.01
889.20 891.00 892.79 894.59 896.38 898.18 899.97 901.77 903.56 905.36 907.15
-2
Energy / keV 10
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24. Scanning Electron Microscopy (SEM)
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25. Scanning Electron Microscopy (SEM)
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26. Scanning Electron Microscopy (SEM)
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27. Scanning Electron Microscopy (SEM)
1 - 30 keV
0.5 - 10 nm
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28. Scanning Electron Microscopy (SEM)
• Secondary electrons
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29. Scanning Electron Microscopy (SEM)
• Backscattered electrons
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30. Scanning Electron Microscopy (SEM)
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