Sem

1. Materials Characterization Lab www.mri.psu.edu/mcl Scanning Electron Microscopy Mark S. Angelone John Cantolina MCL MCL msa3@psu.edu jjc16@psu.edu JUNE 22, 2005

2. Materials Characterization Lab www.mri.psu.edu/mcl Summer Characterization Open Houses Technique Time Date Location Thermal analysis (TGA, DTA, DSC) 9:45 AM June 8 250 MRL Bldg. Transmission Electron Microscopy (TEM/STEM) 9:45 AM June 15 114 MRI Bldg Scanning electron microscopy (SEM) 9:45 AM June 22 541 Deike Bldg. Analytical SEM 11:00 AM June 22 541 Deike Bldg. X-ray Diffraction (XRD) 9:45 AM June 29 250 MRL Bldg. Dielectric Characterization (25 min lecture only) 9:45 AM July 6 250 MRL bldg. High temperature sintering lab (20 min lecture only) 10:15 AM July 6 250 MRL Bldg. Focused Ion Beam (FIB) 9:45 AM July 13 114 MRI Bldg TEM sample preparation 11:00 AM July 13 114 MRI Bldg Orientation imaging microscopy (OIM/EBSD) 9:45 AM July 20 250 MRL Bldg. Chemical analysis (ICP, ICP-MS) 9:45 AM July 27 541 Deike Bldg. Atomic Force Microscopy (AFM) 9:45 AM August 3 114 MRI Bldg Small angle x-ray scattering (SAXS) 9:45 AM August 10 541 Deike Bldg. Particle Characterization 9:45 AM August 17 250 MRL X-ray photoelectron spectroscopy (XPS/ESCA) 9:45 AM August 24 114 MRI Bldg Auger Electron Spectroscopy (AES) 11:00 AM August 24 114 MRI Bldg NOTE LOCATIONS: The MRI Bldg is in the Innovation Park near the Penn Stater Hotel; MRL Bldg. is on Hastings Road. More information: www.mri.psu.edu/mcl

3. Materials Characterization Lab www.mri.psu.edu/mcl Materials Characterization Lab Locations MRI Bldg: XPS/ESCA, FIB SIMS, TEM, HR- TEM, FE-Auger, MRL Bldg: Hosler Bldg: AFM, XRD SEM, XRD, OIM, DTA, SEM,AFM,ESEM, DSC, TGA, FTIR, Penn Stater FE-SEM, EPMA, ICP, Hotel Raman, AFM, Powder, E&ES Bldg: ICP-MS,BET, SAXS dielectric, prep, shop, SEM IC, UV-Vis Route 322 Steidle Bldg: Atherton Street Nanoindenter (322 Business) I-99 Park Ave. 0 0 0 0 0 0 0 Ave. 0 0 0 0 0 Park 0 Beaver 0 0 Stadium 0 0 0 Centre 0 0 Porter Road Community Univ Shortlidg Hospital 0 0 Burrowes Road ersi ty D e Pollock Road Road rive North Hastin Deike Bldg: gs Ro ad College Ave.

4. Materials Characterization Lab www.mri.psu.edu/mcl MCL SERVICES • Facilities/Instruments • User Training • Operators/Analyst for hire • 24/7 • Online bookings • User fees • website/contacts to get started

5. Materials Characterization Lab www.mri.psu.edu/mcl Things To Do Today ― Overview of SEM Techniques ― specific applications from Penn State materials ― discussion of MCL capabilities ― how to get started ― campus resources ― a brief lab tour

6. Materials Characterization Lab www.mri.psu.edu/mcl

8. Materials Characterization Lab www.mri.psu.edu/mcl • MCL SEM CAPABILITY • CSEM • VARIATIONS • MICROANALYSIS Later this morning

9. Materials Characterization Lab www.mri.psu.edu/mcl SEM VARIANTS • IMPROVE RESOLVING POWER •Theoretical Limits ˜ 5 – 7 Å •LaB6 •Field Emitter • EXPAND SAMPLE RANGE •Insulating •Out gassing •WET •Beam sensitive • EXTEND INFORMATION •SE type/BSE type discriminating detectors •XRAY: EDS, WDS •CL •BSED/OIM •Dynamic Experiments (Temp, Humidity, Atmosphere…..)

10. Materials Characterization Lab www.mri.psu.edu/mcl CSEM (Conventional Scanning Electron Microscopy) • W – Hairpin Emitter •M H V •SE via ETD •3-4 nm P-P Resolution •50X – 30,000X Typical •Up to 200mm sample size typical •MHV compatible electrically conducting samples

15. Materials Characterization Lab www.mri.psu.edu/mcl Beam B B + 12 kV B F B PM LG S B SE Specimen B -50 V to + 250 V

16. Materials Characterization Lab www.mri.psu.edu/mcl CSEM (Conventional Scanning Electron Microscopy) • W – Hairpin Emitter •M H V •SE via ETD •3-4 nm P-P Resolution •50X – 30,000X Typical •Up to 200mm sample size typical •MHV compatible electrically conducting samples

17. Materials Characterization Lab www.mri.psu.edu/mcl CSEM (Conventional Scanning Electron Microscopy) • FEI/PHILIPS XL20, XL30 • HITACHI 3500N • HITACHI 3000 • ADDITIONAL INFORMATION: • BSE (H 3500N) • EDS • XL20 Z > 11, spectra only • H3500N Z > 5, spectra, maps, etc • BSED/OIM (H3500N) • USER FEATURES: • Digital Images (All) • Print Images (XL20) • Motorized Stage (H3500N) • APPLICATIONS: • Aggregate microstructures • Semi conductor device structures • Corrosion/weathering • Materials defects

20. Materials Characterization Lab www.mri.psu.edu/mcl CSEM (Conventional Scanning Electron Microscopy) • FEI/PHILIPS XL20, XL30 • HITACHI 3500N • HITACHI 3000 • ADDITIONAL INFORMATION: • BSE (H 3500N) • EDS • XL20 Z > 11, spectra only • H3500N Z > 5, spectra, maps, etc • BSED/OIM (H3500N) • USER FEATURES: • Digital Images (All) • Print Images (XL20) • Motorized Stage (H3500N) • APPLICATIONS: • Aggregate microstructures • Semi conductor device structures • Corrosion/weathering • Materials defects

33. Materials Characterization Lab www.mri.psu.edu/mcl FESEM (Field Emission SEM) • Field Emission Tips • Cold • 80mm motorized stage • Schotky • Thermal • Small samples typical (< 15mm) • UHV • LV-SEM (2-3nm @ 1kV • Beam sensitive samples • Short W.D. SE Detectors • Insulators • Surface contrast • 1nm P-P Resolution • Applications • 500X – 450,000X + • JEOL 6700F •SE only

35. Materials Characterization Lab www.mri.psu.edu/mcl FESEM (Field Emission SEM) • Field Emission Tips • Cold • 80mm motorized stage • Schotky • Thermal • Small samples typical (< 15mm) • UHV • LV-SEM (2-3nm @ 1kV • Beam sensitive samples • Short W.D. SE Detectors • Insulators • Surface contrast • 1nm P-P Resolution • Applications • 500X – 450,000X + • JEOL 6700F •SE only

40. Materials Characterization Lab www.mri.psu.edu/mcl Carbon 1s

45. Materials Characterization Lab www.mri.psu.edu/mcl ESEM (ENVIRONMENTAL SEM) • W-Hairpin • 3-4 nm P-P Same as • 25X – 30,000X Typical CSEM • 100 mm Stage

46. Materials Characterization Lab www.mri.psu.edu/mcl ESEM (ENVIRONMENTAL SEM) • W-Hairpin • USER FEATURES • 3-4 nm P-P Same as • Great GUI • 25X – 30,000X Typical CSEM • Digital Images/Spectra • 100 mm Stage • Image Analysis • IR Chamber View • 3 VAC MODES • Heating (1000°C) • HIGH (CSEM) • LOW (LVSEM) • APPLICATIONS • WET (ESEM) • All CSEM • Insulators • FEI QUANTA 200 • Out Gassing •Wet Mode • Information Sources • Dynamic Heat/Cool/Wet •SE/BSE All modes • EDS Z> 5 spectra, maps, quant • Charge contrast (?)

47. Materials Characterization Lab www.mri.psu.edu/mcl Insulators

52. Materials Characterization Lab www.mri.psu.edu/mcl Out Gassing

55. Materials Characterization Lab www.mri.psu.edu/mcl Wetting

61. Materials Characterization Lab www.mri.psu.edu/mcl Dynamic Heat/Cool/Wet

81. Materials Characterization Lab www.mri.psu.edu/mcl www.mri.psu.edu/mcl Mark Angelone 310 Hosler Bldg 883-9350 msa3@psu.edu

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