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X-ray photoelectron spectroscopy (XPS)

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Lecture 18. Chemical: XPS

Apr 05, 2019

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Lecture 18. Chemical: XPS. X-ray Photoelectron Spectroscopy (XPS), also known as Electron Spectroscopy for Chemical Analysis (ESCA) is a widely used technique to investigate the chemical composition of surfaces. XPS is used to measure:

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• aluminum foil
• electron spectroscopy
• pure materials

Presentation Transcript

Lecture 18.Chemical: XPS

X-ray Photoelectron Spectroscopy (XPS), also known as Electron Spectroscopy for Chemical Analysis (ESCA) is a widely used technique to investigate the chemical composition of surfaces.

XPS is used to measure: • elemental composition of the surface (top 1–10 nm usually) • empirical formula of pure materials • elements that contaminate a surface • chemical or electronic state of each element in the surface • uniformity of elemental composition across the top surface (aka, line profiling or mapping) • uniformity of elemental composition as a function of ion beam etching (aka, depth profiling)

Components of an XPS system The main components of a commercially made XPS system include: • A source of X-rays • An ultra-high vacuum (UHV) stainless steel chamber with UHV pumps • An electron collection lens • An electron energy analyzer • Mu-metal magnetic field shielding • An electron detector system • A moderate vacuum sample introduction chamber • Sample mounts • A sample stage • A set of stage manipulators

XPS Energy Scale The XPS instrument measures the kinetic energy of all collected electrons. The electron signal includes contributions from both photoelectron and Auger electron lines.

Quantitative Analysis by XPS For a Homogeneous sample: • I = NsDJLlAT • where: N = atoms/cm3 • s = photoelectric cross-section, cm2 • D = detector efficiency • J = X-ray flux, photon/cm2-sec • L = orbital symmetry factor • l = inelastic electron mean-free path, cm • A = analysis area, cm2 • T = analyzer transmission efficiency

Quantitative Analysis by XPS • N = I/sDJLlAT • Let denominator = elemental sensitivity factor, S • N = I / S • Can describe Relative Concentration of observed elements as a number fraction by: • Cx = Nx / SNi • Cx = Ix/Sx / S Ii/Si • The values of S are based on empirical data.

X-ray Photoelectron Spectrometer

XPS Spectrum • The XPS peaks are sharp. • In a XPS graph it is possible to see Auger electron peaks. • The Auger peaks are usually wider peaks in a XPS spectrum. • Aluminum foil is used as an example on the next slide.

XPS Spectrum

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X-Ray Photoelectron Spectroscopy (XPS) - PowerPoint PPT Presentation

X-Ray Photoelectron Spectroscopy (XPS)

X-ray photoelectron spectroscopy (xps) david echevarr a torres university of texas at el paso college of science chemistry department outline xps background xps ... – powerpoint ppt presentation.

• David Echevarría Torres
• University of Texas at El Paso
• College of Science
• Chemistry Department
• XPS Background
• XPS Instrument
• How Does XPS Technology Work?
• Auger Electron
• Cylindrical Mirror Analyzer (CMA)
• KE versus BE
• Spectrum Background
• Identification of XPS Peaks
• X-rays vs. e- Beam
• XPS Technology
• XPS technique is based on Einsteins idea about the photoelectric effect, developed around 1905
• The concept of photons was used to describe the ejection of electrons from a surface when photons were impinged upon it
• During the mid 1960s Dr. Siegbahn and his research group developed the XPS technique.
• In 1981, Dr. Siegbahn was awarded the Nobel Prize in Physics for the development of the XPS technique
• Irradiate the sample surface, hitting the core electrons (e-) of the atoms.
• The X-Rays penetrate the sample to a depth on the order of a micrometer.
• Useful e- signal is obtained only from a depth of around 10 to 100 Å on the surface.
• The X-Ray source produces photons with certain energies
• MgK? photon with an energy of 1253.6 eV
• AlK? photon with an energy of 1486.6 eV
• Normally, the sample will be radiated with photons of a single energy (MgK? or AlK?). This is known as a monoenergetic X-Ray beam.
• An electron near the Fermi level is far from the nucleus, moving in different directions all over the place, and will not carry information about any single atom.
• Fermi level is the highest energy level occupied by an electron in a neutral solid at absolute 0 temperature.
• Electron binding energy (BE) is calculated with respect to the Fermi level.
• The core e-s are local close to the nucleus and have binding energies characteristic of their particular element.
• The core e-s have a higher probability of matching the energies of AlK? and MgK?.
• XPS is also known as ESCA (Electron Spectroscopy for Chemical Analysis).
• The technique is widely used because it is very simple to use and the data is easily analyzed.
• XPS works by irradiating atoms of a surface of any solid material with X-Ray photons, causing the ejection of electrons.
• The XPS is controlled by using a computer system.
• The computer system will control the X-Ray type and prepare the instrument for analysis.
• The instrument uses different pump systems to reach the goal of an Ultra High Vacuum (UHV) environment.
• The Ultra High Vacuum environment will prevent contamination of the surface and aid an accurate analysis of the sample.
• The sample will be introduced through a chamber that is in contact with the outside environment
• It will be closed and pumped to low vacuum.
• After the first chamber is at low vacuum the sample will be introduced into the second chamber in which a UHV environment exists.
• A monoenergetic x-ray beam emits photoelectrons from the from the surface of the sample.
• The X-Rays either of two energies
• Al Ka (1486.6eV)
• Mg Ka (1253.6 eV)
• The x-ray photons The penetration about a micrometer of the sample
• The XPS spectrum contains information only about the top 10 - 100 ? of the sample.
• Ultrahigh vacuum environment to eliminate excessive surface contamination.
• Cylindrical Mirror Analyzer (CMA) measures the KE of emitted e-s.
• The spectrum plotted by the computer from the analyzer signal.
• The binding energies can be determined from the peak positions and the elements present in the sample identified.
• Contamination of surface
• XPS is a surface sensitive technique.
• Contaminates will produce an XPS signal and lead to incorrect analysis of the surface of composition.
• The pressure of the vacuum system is lt 10-9 Torr
• Removing contamination
• To remove the contamination the sample surface is bombarded with argon ions (Ar 3KeV).
• heat and oxygen can be used to remove hydrocarbons
• The XPS technique could cause damage to the surface, but it is negligible.
• The X-Rays will penetrate to the core e- of the atoms in the sample.
• Some e-s are going to be released without any problem giving the Kinetic Energies (KE) characteristic of their elements.
• Other e-s will come from inner layers and collide with other e-s of upper layers
• These e- will be lower in lower energy.
• They will contribute to the noise signal of the spectrum.
• The CMA not only can detect electrons from the irradiation of X-Rays, it can also detect electrons from irradiation by the e- gun.
• The e- gun it is located inside the CMA while the X-Ray source is located on top of the instrument.
• The only electrons normally used in a spectrum from irradiation by the e- gun are known as Auger e-s. Auger electrons are also produced by X-ray irradiation.
• When the core electron leaves a vacancy an electron of higher energy will move down to occupy the vacancy while releasing energy by
• Auger electrons
• Each Auger electron carries a characteristic energy that can be measured.
• The X-Ray source can irradiate and remove the e- from the core level causing the e- to leave the atom
• A higher level e- will occupy the vacancy.
• The energy released is given to a third higher level e-.
• This is the Auger electron that leaves the atom.
• The axial e- gun can irradiate and remove the core e- by collision. Once the core vacancy is created, the Auger electron process occurs the same way.
• The electrons ejected will pass through a device called a CMA.
• The CMA has two concentric metal cylinders at different voltages.
• One of the metal cylinders will have a positive voltage and the other will have a 0 voltage. This will create an electric field between the two cylinders.
• The voltages on the CMA for XPS and Auger e-s are different.
• When the e-s pass through the metal cylinders, they will collide with one of the cylinders or they will just pass through.
• If the e-s velocity is too high it will collide with the outer cylinder
• If is going too slow then will collide with the inner cylinder.
• Only the e- with the right velocity will go through the cylinders to reach the detector.
• With a change in cylinder voltage the acceptable kinetic energy will change and then you can count how many e-s have that KE to reach the detector.
• The equation will calculate the energy needed to get an e- out from the surface of the solid.
• Knowing KE, hv and Ø the BE can be calculated.
• The X-Ray will hit the e-s in the bulk (inner e- layers) of the sample
• e- will collide with other e- from top layers, decreasing its energy to contribute to the noise, at lower kinetic energy than the peak .
• The background noise increases with BE because the SUM of all noise is taken from the beginning of the analysis.
• The XPS peaks are sharp.
• In a XPS graph it is possible to see Auger electron peaks.
• The Auger peaks are usually wider peaks in a XPS spectrum.
• Aluminum foil is used as an example on the next slide.
• The plot has characteristic peaks for each element found in the surface of the sample.
• There are tables with the KE and BE already assigned to each element.
• After the spectrum is plotted you can look for the designated value of the peak energy from the graph and find the element present on the surface.
• Hit all sample area simultaneously permitting data acquisition that will give an idea of the average composition of the whole surface.
• Electron Beam
• It can be focused on a particular area of the sample to determine the composition of selected areas of the sample surface.
• Consider as non-destructive
• because it produces soft x-rays to induce photoelectron emission from the sample surface
• Provide information about surface layers or thin film structures
• Applications in the industry
• Polymer surface
• Semiconductors
• Dielectric materials
• Electronics packaging
• Magnetic media
• Thin film coatings
• Dr.William Durrer for explanations on XPS technique, Department of Physics at UTEP.
• www.uksaf.com
• www.casaxps.com
• www.nwsl.net
• XPS instrument from the Physics Department.
• Elizabeth Gardner, Ph.D.
• from the Department of Chemistry at the University of Texas at El Paso
• William Durrer, Ph.D.
• from the Department of Physics at the University of Texas at El Paso
• Roberto De La Torre Roche
• Lynn Marie Santiago

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Remember: Less is more.

A strong presentation is so much more than information pasted onto a series of slides with fancy backgrounds. Whether you’re pitching an idea, reporting market research, or sharing something else, a great presentation can give you a competitive advantage, and be a powerful tool when aiming to persuade, educate, or inspire others. Here are some unique elements that make a presentation stand out.

• Fonts: Sans Serif fonts such as Helvetica or Arial are preferred for their clean lines, which make them easy to digest at various sizes and distances. Limit the number of font styles to two: one for headings and another for body text, to avoid visual confusion or distractions.
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• Pictures: Pictures can communicate complex ideas quickly and memorably but choosing the right images is key. Images or pictures should be big (perhaps 20-25% of the page), bold, and have a clear purpose that complements the slide’s text.
• Layout: Don’t overcrowd your slides with too much information. When in doubt, adhere to the principle of simplicity, and aim for a clean and uncluttered layout with plenty of white space around text and images. Think phrases and bullets, not sentences.

As an intern or early career professional, chances are that you’ll be tasked with making or giving a presentation in the near future. Whether you’re pitching an idea, reporting market research, or sharing something else, a great presentation can give you a competitive advantage, and be a powerful tool when aiming to persuade, educate, or inspire others.

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Select  Add-ins from the ribbon,   then select  More Add-ins .

Select the My Add-ins tab   to view your existing add-ins.

Select  Manage My Add-ins .

Under the Payment and Billing section, choose Cancel Subscription .

Select  OK ,   then Continue .

Once you've cancelled your subscription, you should see a message that says "You have cancelled your app subscription" in the comments field of your add-in list.

Manage an add-in's access to your devices

Note:  The information in this section only applies to Excel on the web, Outlook on the web, PowerPoint on the web, and Word on the web running in Chromium-based browsers, such as Microsoft Edge and Google Chrome.

When an installed add-in requires access to your devices, such as your camera or microphone, you will be shown a dialog with the option to allow, allow once, or deny permission.

If you select  Allow , the add-in will have access to the requested devices. The permission you grant persists until you uninstall the add-in or until you clear the cache of the browser where the add-in is running.

If you select  Allow Once , the add-in will have access to the requested devices until it's relaunched in the browser.

If you select  Deny , the add-in won't be able to access the requested devices. This persists until you uninstall the add-in or until you clear the cache of the browser where the add-in is running.

If you want to change an add-in's access to your devices after selecting  Allow  or  Deny , you must first uninstall the add-in or clear your browser cache.

Add or load a PowerPoint add-in

Add or remove add-ins in Excel

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Evidence Review of the Adverse Effects of COVID-19 Vaccination and Intramuscular Vaccine Administration

Vaccines are a public health success story, as they have prevented or lessened the effects of many infectious diseases. To address concerns around potential vaccine injuries, the Health Resources and Services Administration (HRSA) administers the Vaccine Injury Compensation Program (VICP) and the Countermeasures Injury Compensation Program (CICP), which provide compensation to those who assert that they were injured by routine vaccines or medical countermeasures, respectively. The National Academies of Sciences, Engineering, and Medicine have contributed to the scientific basis for VICP compensation decisions for decades.

HRSA asked the National Academies to convene an expert committee to review the epidemiological, clinical, and biological evidence about the relationship between COVID-19 vaccines and specific adverse events, as well as intramuscular administration of vaccines and shoulder injuries. This report outlines the committee findings and conclusions.

Read Full Description

• Digital Resource: Evidence Review of the Adverse Effects of COVID-19 Vaccination
• Digital Resource: Evidence Review of Shoulder Injuries from Intramuscular Administration of Vaccines
• Press Release

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• India - Mauritius tax treaty update

Protocol to amend double taxation avoidance agreement (DTAA) that includes a principal purpose test rule

Protocol to amend double taxation avoidance agreement (DTAA) that includes a PPT

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India and Mauritius have signed a protocol to amend their double taxation avoidance agreement (DTAA) that includes a principal purpose test  (PPT) rule to align with global efforts against treaty abuse, particularly under the BEPS Action 6 framework.

The application of the PPT may also extend to pre-April 2017 investments that were otherwise grandfathered, unless clarified. With the change, the benefits of the tax treaty can be denied by the tax authorities if one of the principal purposes of the transaction/arrangement is to obtain a tax benefit.

Historically, Mauritius was a preferred jurisdiction for engaging in investments in India due to the non-taxability of capital gains until 2016 when the countries signed a revised tax agreement, giving India the right to tax capital gains in India on transactions in shares acquired through the island nation on and after 1 April 2017.

The protocol takes effect upon both countries notifying each the other the completion of the procedures required by law to bring it into force.  

For more information, contact any member of the KPMG Sovereign Wealth and Pension Funds Tax team, including:

Anjani Sharma | [email protected]

The KPMG name and logo are trademarks used under license by the independent member firms of the KPMG global organization. KPMG International Limited is a private English company limited by guarantee and does not provide services to clients. No member firm has any authority to obligate or bind KPMG International or any other member firm vis-à-vis third parties, nor does KPMG International have any such authority to obligate or bind any member firm. The information contained herein is of a general nature and is not intended to address the circumstances of any particular individual or entity. Although we endeavor to provide accurate and timely information, there can be no guarantee that such information is accurate as of the date it is received or that it will continue to be accurate in the future. No one should act on such information without appropriate professional advice after a thorough examination of the particular situation. For more information, contact KPMG's Federal Tax Legislative and Regulatory Services Group at: + 1 202 533 3712, 1801 K Street NW, Washington, DC 20006.