XPS: PHI VersaProbe 1
XPS provides elemental and chemical information about the surface region (first 1- 30 monolayers) of nearly any solid material. XPS is useful for determining the elemental composition on the surface of all non-volatile materials semiquantitatively. It is sensitive to all elements except H and He and also provides some chemical information about the valence state of elements. XPS is sensitive to the top 5 nm of a sample, but it can be used to provide elemental composition as a function of depth by analyzing a sample while removing surface layers by ion etching. XPS is useful for chemically sensitive materials since damage from the x-ray beam is minimal. It is particularly useful for insulating materials such as polymers, oxides, and powders were charging effects limit other surface techniques.
Basic theory of operation: In XPS, soft x-rays (1486 eV for our instrument) illuminate a region of the sample being analyzed, and photolelectrons emanating from it are energy analyzed. From the energies detected, the elements present and sometimes their chemical state (valence) can be determined. Because only atoms near the surface of the sample emit electrons that escape without losing energy, the technique is very surface sensitive.
- Compositional Analysis: Atomic abundance of all elements (except H and He) on insulators, powders, metals, etc.
- Chemical Analysis: Identifies bonds between specific atoms in the surface region. Polymers, oxides, etc. characterized.
- Depth Profiles: Characterizes buried regions as they are exposed by ion etching.
We have a PHI VersaProbe 1 Scanning XPS Microprobe. This system allows for high sensitivity elemental surface composition measurements and high-resolution binding energy chemical shift measurements of solid samples under high vacuum. It uses Al(Kα) radiation (1486 eV) and is equipped with an argon ion sputter gun to clean the sample surface or do depth profile analysis. In addition to argon ion sputtering, the PHI VersaProbe 1 is equipped with a C60 cluster ion sputtering gun for depth profiling of polymer and organic films with minimum ion impact modification to the surface.
- Detection limits (all elements except H and He): ~ 0.01 monolayer, or ~ 0.1% bulk
- Measurement depth: 10 - 50 Å;
- Spot sizes: 10um - 100 um or 1400 um x 300 um with High Power setting.
- Sample size: 0.1 mm to ~5 cm dia. x 5 mm thick
- Spectrometer: Monochromatized Al(Kα) Source; Vacuum ~ 1.2x10E(-7) Pa
Restrictions on samples: Samples must be solid and vacuum compatible. A sample can range in size from 0.1 mm in diameter and very thin to 5cm in diameter and 5mm thick. Powdered and other rough surfaced samples can also be analyzed. Samples are generally mounted using clips or adhesives onto standard fixtures. It is useful to know in advance if the sample is conducting.
In order to become a qualified user on the PHI VeraProbe 1, you need to follow each of these steps in the order as listed here:
- Complete the process to become a lab member of SNSF and follow the instructions to activate a Badger account.
- Complete the SNSF COVID-19 Authorization protocol and receive notification of authorization.
- Join EdX and take the two introductory modules and quizzes under the “X-Ray Photoelectron Spectroscopy” heading.
- Click on this link and navigate to the XPS section, under Surface Characterization & Analysis.
- Send an email to Juliet Jamtgaard to request training.
- Complete the first training session (group session).
- Schedule and pass the second training session (1-on-1).
The PHI VersaProbe 1 is the preferred XPS instrument for users with air-sensitive samples. If your research requires you to use our Vacuum Transfer Vessel (VTV) that can be loaded in a glove box, you will be assigned the VersaProbe 1 instrument.
You will need two training sessions to be a qualified and authorized user on the PHI VersaProbe 1 system and receive swipe card access to the room. The first training session is done in a group, about once a month. The second session is an individual one, which you have to schedule with one of the trainers sometime after your first session. Both sessions will be conducted using web-based instruction and employ social-distancing.
After you receive full qualification, you may request VTV training by contacting Juliet Jamtgaard.
XPS Background Info: There are numerous texts discussing the use of XPS. Some useful examples are:
- Electron Spectroscopy: Theory, Techniques and Applications. C. R. Brundle and A. D. Baker, eds. (a 5 volume series)
- Practical Surface Analysis, D. Briggs and M. P. Seah eds.
- Handbook of XPS, C. D. Wagner (published by Physical Electronics, Inc.)
- Or try http://www.york.ac.uk/org/esca/tech/xps.html.