XPS X-ray Photoelectron Spectroscopy Copyright 2016 University Instrumentation

XPS X-ray Photoelectron Spectroscopy Copyright 2016 University Instrumentation Center UNH-Durham, NH Parsons Hall 23 Academic Way 603 -862 -2790 www. unh. edu/uic Form #1714100 rev. AA 8/1/2016 Created by: John Wilderman

University Instrumentation Center • • Who We Are What We Do Contact Information Emergency Contact Copyright 2016 University Instrumentation Center UNH Form #1714100 rev. AA 8/1/2016

What is XPS? • X-ray Photoelectron Spectroscopy is an analysis technique used for determining elemental composition on surfaces of solid samples. • This technique is both Qualitative and Quantitative. • Detects Elements between Lithium (3) and Lawrencium (103). Copyright 2016 University Instrumentation Center UNH Form #1714100 rev. AA 8/1/2016

How does XPS Work • XPS uses X-rays to dislodge electrons from the shells of the molecules and the resulting photoelectrons are collected, counted, and their kinetic energy measured to determine the elements they were dislodged from. Copyright 2016 University Instrumentation Center UNH Form #1714100 rev. AA 8/1/2016

Photoelectron Pathway Copyright 2016 University Instrumentation Center UNH Form #1714100 rev. AA 8/1/2016

Chamber Section Form #1714100 rev. AA 8/1/2016

XPS Analysis Types • • Surface Composition Surface Contaminates Coating Uniformity (mapping) Depth Profiling (ion etch) Copyright 2016 University Instrumentation Center UNH Form #1714100 rev. AA 8/1/2016

Sample Composition • • • Good Samples Inorganic Compounds Metal Alloys Polymers Glasses Ceramics Carbon Fly ash Inks Wood Paints Copyright 2016 University Instrumentation Center UNH • • Not So Good Samples Brass Soft Polymers Adhesives Epoxies Bad Samples • Liquids • Water based items • Porous Materials Form #1714100 rev. AA 8/1/2016

Vacuum Pressure Units • • Torr PSI Pascals Bars mm. Hg mm. H 2 O in. Hg Copyright 2016 University Instrumentation Center UNH • Absolute vs. Gauge 760 Torr = 14. 7 psi • Rough Vacuum 10 -1 Torr • Medium Vacuum 10 -3 Torr • High Vacuum 10 -6 Torr • Ultra High Vacuum 10 -8 Torr Form #1714100 rev. AA 8/1/2016

Volume Expansion Cleanliness Dust Finger Prints PV=T 1 m. L @ 760 Torr 7. 6 x 108 L @ 10 -9 Torr 1 Mile Wide x 1 Mile Long x 1 Foot Tall Copyright 2016 University Instrumentation Center UNH Form #1714100 rev. AA 8/1/2016

XPS Safety • • • X-rays High Voltage (15 KV) Cooling Water Vacuum System (ion and turbo pump) Sample Loading/Unloading Laser (He Ne) Copyright 2016 University Instrumentation Center UNH Form #1714100 rev. AA 8/1/2016

XPS Hardware Form #1714100 rev. AA 8/1/2016

Hardware Vacuum Pumps Roughing Pump Turbo Pump Ion Pump Copyright 2016 University Instrumentation Center UNH Form #1714100 rev. AA 8/1/2016

Hardware Valves Gate Valve Roughing Valve Vent Valve Fore Line Valve Differential Pumping Valve Turbo Isolation Valve Argon Valve Copyright 2016 University Instrumentation Center UNH Form #1714100 rev. AA 8/1/2016

Hardware Pressure Gauges Ion Gauge TC 1 Roughing TC 2 Turbo Backing Copyright 2016 University Instrumentation Center UNH Form #1714100 rev. AA 8/1/2016

Hardware X-ray Guns Dual Mg Al Gun Mono Al Gun Copyright 2016 University Instrumentation Center UNH Form #1714100 rev. AA 8/1/2016

Hardware Ion Etch Gun Cleaning oxides off sample Depth profiling Copyright 2016 University Instrumentation Center UNH Form #1714100 rev. AA 8/1/2016

Hardware Sample Manipulator X Micrometer Y Micrometer Z Micrometer Copyright 2016 University Instrumentation Center UNH Form #1714100 rev. AA 8/1/2016

Hardware Spot Apertures Slot M 120 Micron 60 Micron 30 Micron Copyright 2016 University Instrumentation Center UNH Form #1714100 rev. AA 8/1/2016

Hardware 0. 350 0. 500 0. 850 1. 000 Iris 30 60 120 Slot M Copyright 2016 University Instrumentation Center UNH Form #1714100 rev. AA 8/1/2016

Photoelectron Pathway Copyright 2016 University Instrumentation Center UNH Form #1714100 rev. AA 8/1/2016

Hardware Laser Z-axis alignment of Sample Copyright 2016 University Instrumentation Center UNH Form #1714100 rev. AA 8/1/2016

Hardware Camera Used for Alignment of sample in all three axis Video monitor Charge balance Laser Power Scan Rotation Copyright 2016 University Instrumentation Center UNH Form #1714100 rev. AA 8/1/2016

Electronics • • • Main Power Ion gage Controller Emission Stabilizer Charge Neutralizer Sample Stage Temp Controller Ion Etch Gun Controller Magnet Power Supply High Voltage Power Supply Ion Pump Controller Copyright 2016 University Instrumentation Center UNH Form #1714100 rev. AA 8/1/2016

Computer System • Sun/UNIX • Graphical Interface • Remotely runs Hardware • Stores Spectra • Off Load • Print Copyright 2016 University Instrumentation Center UNH Form #1714100 rev. AA 8/1/2016

Control Software Copyright 2016 University Instrumentation Center UNH Form #1714100 rev. AA 8/1/2016

Processing Software Copyright 2016 University Instrumentation Center UNH Form #1714100 rev. AA 8/1/2016

Processing Software Copyright 2016 University Instrumentation Center UNH Form #1714100 rev. AA 8/1/2016

Form #1714100 rev. AA 8/1/2016