Problem Solving and Failure Analysis by Auger and ESCA M ... · PDF fileMaterials Science...
Transcript of Problem Solving and Failure Analysis by Auger and ESCA M ... · PDF fileMaterials Science...
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Materials Sci ence & Technolog y1
Problem Solving and Failure Analysis by Auger and ESCA
M. Roth
Empa Duebendorf
Lecture «Advanced Materials and Structures» Institute of Metals Research, Shenyang, October 21-23, 2013
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Materials Sci ence & Technolog y2
Surface Analysis
Problems at surfaces and interfaces Surface Analysis: Methods Auger-Electron-Spectroscopy (AES, SAM) X-ray-Photoelectron-Spectroscopy (XPS, ESCA) Case studies: - Heat-protection coatings on architectural glasses (ESCA) - Damaged pressure sensors (ESCA + SAM) - Surface contamination on HF-reciever coils (SAM) - Adhesion of diamond-like carbon coatings (SAM) - Development of biocompatible coatings (SAM) Conclusions
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Materials Sci ence & Technolog y3
Important Surface Phenomena
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Materials Sci ence & Technolog y4
Surface analysis: methods
Lateral resolution
Info
rmat
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dept
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Materials Sci ence & Technolog y5
Surface analysis: physical processes
Ekin = hν - EB
Auger
ESCA
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Materials Sci ence & Technolog y6
Auger ESCA
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Materials Sci ence & Technolog y7
Scanning Auger Microscope
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Materials Sci ence & Technolog y8
ESCA-Microscope
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Materials Sci ence & Technolog y9
ESCA-analysis method
Imaging ESCA:
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Materials Sci ence & Technolog y10
ESCA-analysis method
C (1s) Photoelectron signal of PET: Determination of different chemical positions of C-atoms
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Materials Sci ence & Technolog y11
Auger - ESCA
Lateral resolution:
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Materials Sci ence & Technolog y
Coatings for heat protection glasses
Object: Glass for buildings Material: SiNa-Oxide Problem: Identification of the heat protection coatings Information: Complex coating system (total thickness: ca. 70 nm) Analysis: ESCA – depth profile analysis
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Materials Sci ence & Technolog y13
Coating on glass: depth profile coating 1
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Materials Sci ence & Technolog y14
Coating on glass: depth profile coating 2
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Materials Sci ence & Technolog y15
Coating on glass: depth profile coating 3
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Materials Sci ence & Technolog y
Coatings for heat protection glasses
3 different coatings
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Materials Sci ence & Technolog y
Coatings for heat protection glasses
Object: Glass for buildings Material: SiNa-Oxide Problem: Identification of the heat protection coatings Analysis: ESCA – depth profile analysis Result: Complex coating system (total thickness: ca. 70 nm) - First layer: Sn-Oxide - Ti-Oxide (In-Oxide) - Ag (3 nm !) - ZnCr-Oxide - Sn-O-N - (ZnCr-Oxide) - SiNa-Oxide (glass) Goal: Reflection of IR-radiation
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Materials Sci ence & Technolog y
Damaged pressure sensors
Object: Pressure sensor Material: SiO2 – substrate material with Ni/Cr – conductors Problem: Zero point drift Analysis: ESCA– and Auger measurements at defective and good sensors
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Materials Sci ence & Technolog y19
Sensor: conductor tracks
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Materials Sci ence & Technolog y20
Sensor: conductor tracks Process: ESCA – sputtering and measure signal for Cr
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Materials Sci ence & Technolog y21
ESCA spectrum of SiO2 - layer
Fluorine !
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Materials Sci ence & Technolog y22
Sensor: conductor tracks Process: ESCA – sputtering and measure signal for Cr
Transfer of specimen to Auger Microscope
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Materials Sci ence & Technolog y23
NiCr-conductor track
Auger analysis:
SEM image
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Materials Sci ence & Technolog y24
Auger-spectrum of NiCr-conductor track
Good sensor
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Materials Sci ence & Technolog y25
Auger-spectrum of NiCr-conductor track
Defective sensor
Sulphur
Phosphorus
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Materials Sci ence & Technolog y
Damaged pressure sensors
Object: Pressure sensor Material: SiO2 – substrate material with Ni/Cr – conductors Problem: Zero point drift Analysis: ESCA– and Auger measurements at defective and good sensors Result: 1) Removal of SiO2–layer: ESCA – sputtering 2) Analysis of SiO2–layer: 1 – 2 % F 3) SEM: higher roughness of defective sensor 4) Auger–analysis: Cl, S, P on conductor NiCr – passive layer is destroyed by corrosion
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Materials Sci ence & Technolog y
Surface contamination
Object: High frequency recieving coil for nuclear magnetic resonance spectroscopy (NMR) Material: Superconductor, coated with 1 µm Cu and 0.2 µm Rhodium Problem: Colouring of the surface (after 2-3 months) Distortion of NMR signal Analysis: AES-depth profile analysis at coloured and good (new) coils
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Materials Sci ence & Technolog y28
Auger depth profile new coil
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Materials Sci ence & Technolog y29
Auger depth profile coloured coil
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Materials Sci ence & Technolog y
Surface contamination
Object: High frequency recieving coil for nuclear magnetic resonance (NMR) spectroscopy Material: Superconductor, coated with 1 µm Cu and 0.2 µm Rhodium Problem: Colouring of the surface (after 2-3 months) Distortion of NMR signal Analysis: AES-depth profile analysis at coloured and good (new) coils Result: 1) New coil: - AES-depth profile: S in Rhodium layer (ca. 15%) 2) Coloured coil: - AES-depth profile: S + Cu in Rhodium Layer ca. 4 % Cl at the surface Formation of Cu2S and CuS compounds, which are instable against Chlorine and humidity
Degradation of the Rhodium Layer
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Materials Sci ence & Technolog y
Thin film technology / adhesion
Object: Dry bearings in machinery components Material: Coatings from amorphous diamondlike carbon Fabrication: Plasma enhanced CVD (at ≤ 200 oC) Properties: - high hardness (4000 – 6000 HV) - high elasticity - low coefficient of friction - ADLC/steel: µ = 0.09; ADLC/ADLC: µ = 0.02 – 0.04 - very high chemical stability - high heat conduction - thermal stability until 250 oC Problem: Adhesion of ADLC on substrate Analysis: AES-depth profile at the interface coating/substrate - detection of trace elements - analysis of precipitates
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Materials Sci ence & Technolog y32
Application of ADLC-coatings
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Materials Sci ence & Technolog y33
Coating: 60 nm ADLC on Si-substrate
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Materials Sci ence & Technolog y34
Adhesion of ADLC
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Materials Sci ence & Technolog y35
Adhesion of ADLC
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Materials Sci ence & Technolog y
Surface analysis for biological applications
Biological reactions on an implant strongly depend on the first atomic layers Characterization of the top surface (nm) with good lateral resolution On metal implants like artificial hip joints the surface consists of an oxide layer Corrosion protection Bioreaction Example: Ti-6Al-7Nb implant alloy Al-rich oxide regions above the α-phase Nb-rich oxide regions above the β-phase Research: Alloy development Surface conditioning (control of oxide layer, thickness, etc.) Coating (diamond-like carbon)
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Materials Sci ence & Technolog y37
SAM: SEM-image
α-phase: dark β-phase: white
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Materials Sci ence & Technolog y38
SAM: O-map
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Materials Sci ence & Technolog y39
SAM: Ti-map
α-phase: Ti-rich
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Materials Sci ence & Technolog y40
SAM: Al-map
α-phase: Al-rich
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Materials Sci ence & Technolog y41
SAM: Nb-map
Nb2O5 distribution on the surface of the TiAlNb-implant (above β-phase)
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Materials Sci ence & Technolog y
Summary 1) Surface analysis: SAM: - depth 0.5-3 nm, lateral 30 nm - SEM-images - element mapping - depth profiles - fracture device in UHV ESCA: - depth 0.5-3 nm, lateral 10 000 nm - chemical information (valence) - depth profiles 2) Failure analysis = problem solving Use first basic (cheaper) methods a) SEM/EDX or microprobe (EPMA), chem. Analysis b) SAM, ESCA (and SIMS, SNMS) 3) Costs: - all methods of analysis are available - automation: control and data acquisition by computer - equipment with high reliability - analysis together with customer