Surface Analysis
SAL Facility Overview
The Surface Analysis Lab provides nanoscale measuments of chemical composition and bonding for the top 5-10 nm of solid surfaces through X-ray Photoelectron Spectroscopy. Additionally, the Surface Analysis Lab houses instrumentation for Powder X-ray Diffraction, X-ray Emission Spectroscopy, and X-ray Absorption Fine Structure.
| Instruments | Internal | Federal | External |
|---|---|---|---|
| CD | $8.00 | $13.00 | $120.00 |
| MPXRD | $7.00 | $11.00 | $60.00 |
| XAFS | $40.00 | $64.00 | $260.00 |
| XES | $40.00 | $64.00 | $260.00 |
| XPS | $25.00 | $40.00 | $95.00 |
| Tech Assist | $40.00 | $64.00 | $120.00 |
EHS Prerequisites
- General Laboratory Safety
- Laboratory Hazardous Waste
- Analytical X-ray Equipment
General Training
- SAL Orientation (offered monthly)
- Instrument specific training (offered by request)
Physical Electronics Genesis
- Signal from top 5-10 nm of surface
- 5 µm minimum beam size
- Hot (500°C) / Cold (-100°C) Stage
- Inert sample transfer vessel for samples sensitive to atmosphere
Rigaku Miniflex 600
- Phase identification and quantification
- Graphite monochromator for increased S/N
- 6-position automated sample changer with integrated spinner
easyXAFS easyXES150
- Hard X-ray absorption fine structure spectrometer (4.5-25+ keV)
- Bulk (several µm) measurement
- Lanthanide sensitivity
easyXAFS Brimstone
- Tender X-ray emission spectrometer (2-5 keV)
- ~1 eV energy resolution
- Sensitive for P and S
easyXAFS easyXES150
- Hard X-ray emission spectrometer (4.5-25+ keV)
- Bulk (several µm) measurement
- Lanthanide sensitivity
Complete these training courses at https://www.ehss.vt.edu/train.php
- General Laboratory Safety
- Laboratory Hazardous Waste
- Analytical X-ray Equipment
- Instrumentation is designed to protect the user from incidental X-ray exposure through shielding, distance and interlocks.
- Gloves are provided for SAL users at the sample preparation desk. Additional PPE needs to be brought to the lab by the user.
- Please take any waste or consumed samples with you back to your primary laboratory. The SAL cannot accommodate the variety and scope of materials brought in for testing, and undocumented disposal of chemicals in the SAL hazardous waste bin can lead to mixing of non-compatible waste.
How to fill out an Analytical Services ISR
Supplier: "VT Chemistry Surface Analysis Service Center"
Direct link to FACES Scheduling System
FACES Group: VT_SAL
Contact Nicholas Popczun
nip@vt.edu
540-231-6604
Data analysis Resources
Copy for publication
Experimental Methods
X-ray Photoelectron Spectroscopy. XPS spectra were collected on a PHI Genesis spectrometer using an aluminum anode X-ray source with a photon energy of 1486.6 eV. Survey spectra were collected with a 25 W, 15 kV source producing a 100 µm beam with a scan range of 1100 to 0 eV with a step size of 0.5 eV and pass energy of 280 eV. High resolution spectra were collected with a step size of step size of 0.1 eV and pass energy of 26 eV.
Replace bold and underlined sections with information provided on your XPS report
Acknowledgements
This work was performed in part at the Virginia Tech Surface Analysis Laboratory (RRID:SCR_27504) which is supported by the National Science Foundation under Grant No. CHE-1531834.
If using CasaXPS for data analysis, please cite:
- Fairley, Neal, et al. "Systematic and collaborative approach to problem solving using X-ray photoelectron spectroscopy." Applied Surface Science Advances 5 (2021): 100112.
Data repositories and information
Copy for publication
Experimental Methods
Powder X-ray Diffraction. PXRD spectra were collected on a Rigaku Miniflex 600 spectrometer using an copper anode X-ray source. Diffractograms were collected with a 2 theta range of 3 to 90 at a speed of 15 degrees/min and step size of 1.
Replace the bold and underlined sections with information from the General Measurement settings.
Acknowledgements
This work was performed in part at the Virginia Tech Surface Analysis Laboratory (RRID:SCR_27504)
Sample Preparation Guides
Additional Guides and Manuals *************
Copy for publication
Experimental Methods
X-ray Absorption Fine Structure / X-ray Emission Spectroscopy. XAFS / XES spectra were collected on a (easyXAFS easyXES150 / easyXAFS Brimstone) spectrometer using a tungsten anode X-ray source. Spectra were collected with 70W from on the Fe K edge with 0.25 eV steps for a duration of 2 seconds per point.
Replace the bold and underlined sections with information from the General Measurement settings.
Laboratory Hours
Staffed Hours: 9a - 5p, M-F
24/7 access for trained users
Contact SAL Staff
Nicholas Popczun
SAL Facility Manager
njp@vt.edu
540-231-6604
Emergency Contact
VT Environmental Health & Safety
540-231-5364
www.ehs.vt.edu
Kenny Smith
Facilities Manager
kesmith7@vt.edu
Drew Murphy
Safety Coordinator
drewmurphy23@vt.edu
Lab Address
Hahn Hall South 008
Virginia Tech
900 W. Campus Blvd.
Blacksburg, VA 24061