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X-ray photoelectron spectroscopy: Principle, instrumentation, application

May 18, 2022
Surface characterization technique

Table of Contents

X-ray photoelectron spectroscopy is one of the most widely used surface-sensitive electron emission spectroscopic techniques. Its development is based on the photoelectric effect, which may detect the element existing within a material or covering its surface.

X-ray photoelectron spectroscopy principle

The characteristic binding energies of core electrons in atoms keep them in their orbitals. The characteristics of adjacent atoms, orbital kinds, and atom types all influence the binding energies. The binding energies of electrons emitted from the sample surface are measured by XPS.

The mechanism of photo ionization is utilized to eject electrons from surfaces. For this, the sample surface is irradiated by soft x-ray photons usually 1486 eV from an Al-anode. The photon penetrates the surface to a depth of approximately 1µm. When a photon interacts with a sample atom, the photon’s energy ionizes core electrons, causing them to be ejected from the atoms. Within the bulk of the sample, the mean free path of the ejected electrons is very small due to interaction with the surrounding atoms. But, electrons expelled from atoms in the sample’s top 5nm layer have a high chance of leaving without further interaction.

x-ray photoelectron spectroscopy principle

These electrons will pass into the ultrahigh vacuum(UHV) conditions within the spectrometer to ensure that electrons are not scattered by gas molecules and to limit surface contamination during the analysis. An electron energy analyzer(spectrometer) measures the kinetic energy Ek of the ejected electrons. The original binding energy Eb experienced by an electron in the sample can be calculated from Ek using the simple relationship.

E k = hv-E b – ϕ

where E k = kinetic energy of the ejected electron

E b = binding energy of the electron

hv= incident photon energy

ϕ= work function of spectrometer

The different atoms have different electron shells with different binding energies. Each element has unique binding energy (Eb) which can be used to identify the elemental composition of the sample surface. The number of emitted photoelectrons with various Ek is counted, and an XPS spectrum is generated, which facilitates the identification of all elements in all states except H and He.

X-ray photoelectron spectroscopy instrumentation

The basic five components of the XPS instrument are listed as,

An ultrahigh vacuum chamber(UHV) with the monochromatic soft x-ray source
Lens system
Energy analyzer

Instrumentation of X-ray photoelectron spectroscopy

X-ray source of XPS

Al or Mg-coated anode is struck by electrons from a high voltage around 10-15 kV, AlKα or MgKα radiation lines are produced at energies of 1486.6 eV and 1256.6 eV respectively.

Ultra-High Vacuum(UHV)

10 -9 – 10 -10 torr or high vacuum condition is necessary to reduce the amount of noise in the XPS spectrum and to avoid any extra peaks from contaminations on the sample surface.

Electrons lens

The electron lens collects and slows the ejected photoelectrons from the sample surface before entering the energy analyzer of XPS.

Energy analyzer of XPS

It is the hemispherical sector, which consists of two concentric hemispheres with a voltage applied between them.

A multichannel display detector which is equivalent to a photographic plate allows simultaneous detection of the kinetic energy of the ejected electrons.

Monitors/Recorder

The high-performance computer is used as a recorder/monitor which controls voltage to the lense and analyzer. It also produces an XPS spectrum. The XPS spectra are generated by plotting Ek intensity vs binding energies, by computers automatically.

Application of x-ray photoelectron spectroscopy

XPS can be used for both qualitative as well as quantitative analysis.

Qualitative analysis

Elemental analysis : The electron energy levels of an atom can be divided into two types, core levels, which are bound to the nucleus, and valence levels, which are only weakly bound. The valence levels of an atom are the ones that interact with the valence levels of other atoms to form chemical bonds in molecules and compounds. Their character(valence bond character) and energy are changed by this process, becoming characteristics of the new species formed.

The core-level electrons of an atom have energies that are nearly independent of the chemical species in which the atoms are bound since they are not involved in the bonding process. Thus, the identification of Core level binding energies thus provides unique signatures of the elements. All elements in the periodic table can be identified in this manner, except for H and He which have no core levels.

Quantitative analysis

Quantitative analysis requires the measurement of relative peak intensities and the intensity of the peak depends on the atomic concentration(N) of an element present in the surface film.

Chemical shift (chemical state analysis)

Chemical shift is the difference in binding energy between the same atom in two chemically distinct states in the same molecule or in two separate compounds. It is characteristic of the nature and the number of atoms surrounding the ionized atoms of the sample. It can be used to see what kind of chemical bonding of atoms is on the sample surface.

It concerns the chemical bonding nature, the nature of functional groups, and the oxidation states of atoms.
An important capability of XPS is its ability to distinguish the same element in different chemical states, because of BE of an electron is different due to changes in charge density around that element by oxidation

In-depth analysis

Estimation of the in-depth distribution of elements in thin surface film is called in-depth surface analysis. It is done to know whether the thin film is homogeneous or not.

Advantages of X-ray photoelectron spectroscopy

All samples solid, gaseous, and liquid samples can be analyzed but mostly solid samples are analyzed.
Good quantification
Excellent chemical state determination capabilities
Its applicability to a wide variety of materials from biological materials to metals.
It is a non-destructive technique.

Limitations of X-ray photoelectron spectroscopy

The main disadvantages of x-ray photoelectron spectroscopy are listed below:

Lack of good spatial resolution i.e poor spatial resolution
Only moderate absolute sensitivity
Its inability to detect hydrogen and helium
It is not suitable for trace analysis.

X-ray photoelectron spectroscopy youtube video

C. R. Brundle, C. K. Evans, Jr., S. Wilson and L. E. Fitzpatrick (eds), Encyclopedia of Materials Characterization: Surfaces, Interfaces, Thin Films , Butxetworch-Heinemann, Reed Publishing (USA) Inc., 199

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PDF X-ray Photoelectron Spectroscopy
Sampling Depth. Sampling Depth is defined as the depth from which 95% of all photoelectrons are scattered by the time they reach the surface ( 3λ ) Most λ's are in the range of 1 - 3.5 nm for AlKα radiation. So the sampling depth (3λ) for XPS under these conditions is 3-10 nm. 1 monolayer.
PDF PowerPoint Presentation
A few electrons get out un-scattered and are detected as the photoelectron peaks. (mostly from the upper 10 nm of the material.) Many more get out of the surface but have lost energy so make up the detected scattered background. The vast majority don't get out and are not detected. An example XP spectrum.
PDF X-Ray Photoelectron Spectroscopy (XPS)
Based on Einstein's photoelectric effect. Many materials emit electrons when light shines upon them. Core electrons with kinetic energy Ek are ejected by incident X-rays. EK = hν - Eb - φsp. EK = kinetic energy Eb = binding energy h = Planck's constant ν = frequency of X-rays φsp = spectrometer work function. hν.
PDF Lecture 7 X-ray Photoelectron Spectroscopy (XPS)
Primary assumption for quantitative analysis: ionization probability (photoemission cross section) of a core level is nearly independent of valence state for a given element. intensity number of atoms in detection volume. 2 . ( ) D ( E ) L ( ) J ( x , y ) T ( x , y , , , E ) N - z .
PDF X-ray Photoelectron Spectroscopy (XPS)
XPS in a nut-shell. • X-ray photoelectron spectroscopy (XPS) is a classical method for the semiquantitative analysis of surface composition • It is also referred to as Electron Spectroscopy for Chemical Analysis (ESCA) • It is based on the photoelectric effect, i.e., emission of electron following excitation of core level electrons by ...
PDF Practical guides for x-ray photoelectron spectroscopy: Quantitative XPS
Figure 1(d) shows the best geometry for quantitative XPS in the dipole approximation, having the magic angle between incoming x-rays and the analyzer and also the plane of polarization 45° out of the x-ray/sample/analyzer plane. Note that the cross section through the angular emission has the same shape as in Fig. 1(b).
PDF X-ray Photoelectron Spectroscopy (XPS)
The smallest analytical area is approximetly 10 nm. Limited specific organic information. Sample must be compatible with an ultra-high vacuum (UHV) environment (>10-9 Torr). Sample size cannot exceed 1 in. (25 mm) in any direction. Height should not exceed 1⁄2 in. (12 mm). Detects all elements with an atomic number of 3 (lithium) and above.
PDF X-Ray Photoelectron Spectroscopy (XPS)
Typical geometry of an X-ray gun. Aluminum windows of 10-30 μm thick separate the excitation region from the specimen. a continuous spectrum (Bremsstrahlung) are produced. Peaks 10 eV above the Kα. 1, 2 with intensities of 8 % and 4 % of Kα and a continuous spectrum contribute 1, 2 to the BG.
(PDF) Fundamentals of X-Ray Photoelectron Spectroscopy (XPS)
Presentation PDF Available. Fundamentals of X-Ray Photoelectron Spectroscopy (XPS) ... It is concluded that existing standardization is delivering good practices in the use of XPS and has a high ...
PDF Module-5 Unit-5 XPS Principle and Instrumentation Introduction
4. Then the XPS spectrum is obtained by determining the K.E. and number of electrons escaping from upper 0 to 10 nm of sample under investigation. 5. XPS may be routinely employed to study inorganic compounds including metal alloys, semiconductors, polymers, glasses, ceramics, ion-modified materials, etc. References: 1.
PPT / PDF Presentations
PPT / PDF Presentations; Software Operation; XPS Basics; XPS Training Videos; Vocabulary. ISO 18115-1:2013 XPS Terms; Terms & Phrases for XPS; XPS. The History of XPS; Collections of XPS Spectra; Future for XPS Instrument Sales; XPS Job Openings. Job Openings at XPS Makers;
(PDF) X-RAY PHOTOELECTRON SPECTROSCOPY (XPS) TECHNOLOGY
spectroscopic method is called X-ray photoelectron spectroscopy (XPS).XPS technique. involves hit ting the sample with low energy ( (~1.5 keV) X-rays such that photoelectric. effect is induced. An ...
(PDF) Presentation on X-ray Photoelectron Spectroscopy
PDF | XPS is a elemental characterization technique. I prepared this presentation for a course requirement. | Find, read and cite all the research you need on ResearchGate
Lecture 8 XPS
Lecture 8 XPS - Free download as Powerpoint Presentation (.ppt), PDF File (.pdf), Text File (.txt) or view presentation slides online. xps
X-ray Photoelecctron Spectroscopy (XPS)
Feb 25, 2018 • Download as PPTX, PDF •. 17 likes • 33,974 views. F. faheem maqsood. Metallurgy and Materials Engineering Department, University of Punjab Lahore. Engineering. 1 of 19. Download now. X-ray Photoelecctron Spectroscopy (XPS) - Download as a PDF or view online for free.
Xps (x ray photoelectron spectroscopy)
Jan 25, 2013 •. 42 likes • 25,671 views. Zaahir Salam. X-RAY PHOTO ELECTRON SPECTROSCOPY. Technology. 1 of 23. Download now. Download to read offline. Xps (x ray photoelectron spectroscopy) - Download as a PDF or view online for free.
X-ray photoelectron spectroscopy: Principle, instrumentation
X-ray photoelectron spectroscopy principle. The characteristic binding energies of core electrons in atoms keep them in their orbitals. The characteristics of adjacent atoms, orbital kinds, and atom types all influence the binding energies. The binding energies of electrons emitted from the sample surface are measured by XPS.
Save or convert to PDF or XPS in Office Desktop apps
You can use the Office programs to save or convert your files to PDFs so that you can share them or print them using commercial printers. And you won't need any other software or add-ins. Use PDF format when you want a file that: Looks the same on most computers. Has a smaller file size. Complies with an industry format.
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PPT / PDF Presentations; Software Operation; XPS Basics; XPS Training Videos; Vocabulary. ISO 18115-1:2013 XPS Terms; Terms & Phrases for XPS; XPS. The History of XPS; Collections of XPS Spectra; Future for XPS Instrument Sales; XPS Job Openings. Job Openings at XPS Makers;
Save PowerPoint presentations as PDF files
Select File > Export. Click Create PDF/XPS Document, then click Create PDF/XPS. In the Publish as PDF or XPS dialog box, choose a location to save the file to. If you want it to have a different name, enter it in the File name box. Optionally, if you want to change what the final PDF file is like, do any of the following: At Optimize for ...
XPS to PDF
First, drag and drop up to 20 XPS files to the area that says "Drop Your Files Here". Conversely, you can hit the "UPLOAD FILES" button and navigate to your XPS documents that way. As soon as you upload a file, our system will start the conversion process. You'll be able to see in real-time as the files move from XPS to PDF.