Auger Electron Spectroscopy (AES) Lab Objective What is Auger electron spectroscopy?

y? What kind of information we can get out of it? Major components and their functions Electron beam-specimen interactions Interaction volume What is magnification, resolution, depth of field and image contrast Auger spectra Auger depth profile Auger line profile Contents Objective The objective of Auger electron spectroscopy lab course is to
familiarize the students with Auger microprobe analyzer, its operation and working principle. Provide hands-on experience to operate the instrument What is Auger Spectroscopy Auger electron spectroscopy provides information about the chemical composition of the outer surfaces of the sample. Electron beam is used to excite the surface of the sample. Relatively low energy Auger electrons are also emitted in addition to x-ray. The
emitted Auger electrons can be collected with the appropriate detector to yield valuable information about the surface of the sample. What information we can get Auger spectrum Identifications of elements present at the surface Auger map Distribution of elements across the surface Depth profile Change in composition with depth into the surface Chemistry Chemical bonding states of the elements Types of Surfaces Processes occurring at
the surface are of great practical importance in corrosion, coatings and semiconductors etc. Surface analysis by John T.Grant Auger Process Incident electron removes the inner shell electron. Outer shell electron fills the empty space. Instead of x-ray emission , an electron from higher shell is ejected. The energy of auger electron is characteristic of the element from which it was emitted. Most auger electrons are absorbed by the lattice, only those at
the surface are able to escape. Surface analysis by John T.Grant Instrument HSA analyzer Electron Gun Ion gun Probe current detector OL aperture Sample loading system EDS detector Two types of analyzers are used 1. Cylindrical mirror analyzer (CMA) 2. Hemispherical sector analyzer (HSA) Analyzers for AES Cylindrical mirror analyzer (CMA) Electron gun is integrated within the spectrometer Electron energy resolution is low No shadowing for
spherical particles HSA consists of pair of concentric hemispherical electrodes b/w which there is a gap for the passage of electrons. There is a series of lenses b/w the sample and the analyzer to retard the energy of ejected electrons. These lenses also maximize the collection angle to ensure higher efficiency. Hemispherical analyzer Excellent electron energy resolution Tilt sample for improved sensitivity Electron/Specimen Interactions When the
electron beam strikes a sample, both photon and electron signals are emitted. Incident Beam Specimen X-rays - composition info Auger electrons - Surface sensitive compositional Backscattered electrons - Atomic number and topographical Cathodoluminescence - Electrical Secondary electrons - Topographical Specimen Current Electrical Electron sample interaction volume Electron Sample interaction volume Interaction volume increases with
increasing acceleration voltage and with decreasing atomic number The incident electrons do not go along a straight line in the specimen, but follow a zig-zag path. Electron Sample interaction volume Energy distribution of emitted electrons Secondary electrons are low energy electrons with energies of 50eV or less Backscattered electrons have higher energies than the SE. they also have wide range of energy distribution Auger electrons
have intermediate energy range Auger electrons Auger emission vs. x-ray emission Vacuum requirements Auger analysis is carried out in a vacuum chamber and the pressure is maintained 10-7 to 10-8 Pa. Ion pumps and Ti sublimation pumps are used for the main chamber Ion pump is also used to evacuate the Field emission electron Gun chamber Turbo molecular pump is used to evacuate the specimen loading chamber The specimen
chamber and gun chamber can be baked to improve vacuum When a Auger microprobe is used, the electronoptical column and sample chamber must always be under vacuum. 1. If the column is in a gas filled environment, electrons will be scattered by gas molecules which would lead to reduction of the beam intensity and stability. 2. Other gas molecules, which could come from the sample or the microscope itself, could form compounds and
condense on the sample. This would lower the contrast and obscure details on the surface. Why vacuum? In thermionic electron gun, electrons are emitted when a solid is heated. There are two types of thermionic guns. Tungsten wire filament Single crystal of LaB6 Thermionic guns Tungsten wire Single crystal of LaB6 With field emission guns we get a smaller spot and higher current densities compared to thermionic guns Vacuum
requirements are tougher for field emission guns Field emission tip Field emission gun In field emission guns (FEG) a strong electric field is used to extract electrons -Single crystal of W, etched to a thin tip Schottky field emission gun ZrO/W emitter is used. Schottky emission takes place when a strong electric field is applied to the heated metal surface. ZrO coating on the tungsten single crystal reduces the work function. Schottky field emission
gun Electromagnetic lens An electromagnetic lens consists of a coil of copper wires inside an iron pole piece. A current through the coils creates a magnetic field in the bore of the pole pieces which is used to converge the electron beam The magnetic field is inhomoneous in such a way that it is weak in the centre of the gap and becomes stronger close to the bore. Electrons close to the centre are less strongly deflected than those passing the lens
far from the axis. Secondary Electrons SE are generated from the collision between the incoming electrons and the loosely bonded outer electrons These are low energy electrons (~10-50 eV) Topographic contrast arises because SE generation depend on the angle of incidence between the beam and sample MoO3 crystals Secondary electron detector A scintillator (fluorescent substance) is coated on the tip of the SE detector and a high voltage
of about 10KV is applied to it. The SE are attracted to this high voltage and then generate light when they hit the scintillator. This light is directed to the photomultiplier tube through a light guide. Then the light is converted to electrons and these electrons are them amplified as an electric signal. Everhart-Thornley Detector (E-T) Back scattered electrons Back Scattered Electrons are produced by elastic interactions of beam electrons with nuclei of
atoms in the specimen and they have high energy and large escape depth. BSE images are a function of atomic number, Z i.e. high average Z appear brighter than those of low average Z. BSE image from flat surface of an Al (Z=13) and Cu (Z=29) alloy Solid state BSE detector A semiconductor detector, has an annular structure and detects more efficiently BSE since their angular distribution goes as cos(). When BSE enter and scatter
inelastically the electron hole pairs are created. The inversely polarized diode moves electrons and holes in opposite directions and produces an output signal. What is Magnification Magnification is the ratio of the length of the scan D on the Cathode Ray Tube (CRT) to the length of the scan d on the specimen. For a CRT screen that is 10 cm square: M= D/d = 10cm/d Increasing M is achieved by decreasing d. M d 100 1mm 1000 100m 10000 10m
100000 1m The smallest distance between two points that can be resolved is called resolution. What is Resolution = 1.22 / E De Broglies equation shows that wavelength of electrons is related to their energy, E. wavelength can be decreased by increasing the energy of electrons, to get higher resolution. is in nm and E is in electron volts What is depth of field D = ( m) AM 4x105W To increase D Decrease aperture size, A Decrease
magnification, M Increase working distance, W It is the range of depth at which an object remains under focus Depth of field What is contrast A high resolution, high intensity signal resulting from a scan will reveal nothing if contrast is absent. Contrast can be defined as (S2-S1)/S2 S2 = signal from feature of interest S1 = background signal S2 > S1 What is astigmatism? Astigmatism is a lens error that occurs when electrons sense a non uniform
magnetic field resulting in different focal planes of perpendicular rays. In practice that means distortion of the image in different directions when defocusing. Astigmatism is caused by not perfectly cylindrical lenses because lenses can not be machined to perfect symmetry. The net effect is a disk of minimum confusion rather than that a well defined point of focus What is charging When high energy electron hit the specimen they are absorbed in
the specimen. If the specimen is non conductive, the electrons stop in the specimen. This phenomenon is called charging. Electric flow in a non conducting specimen If charging occurs the electron probe that scans over the specimen is deflected by the repulsive force from a charged potential, resulting in a positional shift of the electron probe. This causes an image to distort. Charging effects Distortion of image and anomalous contrast due to
charging 1. Coating a very thin layer of highly conduction material (Au, Pt, C) on non conducting material 2. Observation at Low kV 3. Use of low voltage ion gun Without ion irradiation With ion irradiation Charge Neutralization Charge Neutralization A low voltage ion beam can be used to neutralize the electrostatic charge on the sample surface. Most effective on Inorganic insulating materials Isolated conductive features Depth profiling a
mixture of conductive and insulating layers Surface analysis by John T.Grant Charge Neutralization Surface analysis by John T.Grant Depth Profiling Inert gas such as argon is used to sputter the area. The sputter rate can be varied Sample can be rotated during sputtering Auger spectra is collected after each sputtering step www.surfaceanalysis.org, John T.Grant Depth Profile Depth profile of a Silicon oxide layer on Silicon. Oxide layer is
removed during ion sputtering Depth Profiling Auger depth profile of Ga and In nitride films on sapphire Auger line scan Auger line scan over a sputtered Silicon oxide surface Auger map Cr rich boride particle in a Ni base super alloy Auger map Oxidation of grain boundaries in a steel sample http://www.ualberta.ca/ACSES/index.htm Analysis of topographic surfaces www.surfaceanalysis.org, John T.Grant Important parameters 1.Accelerating voltage
(kV): The voltage with which the electrons are accelerated down the column. 2.Probe convergence angle (p): The half angle of the cone of electrons converging on to the specimen. 3.Probe Current (ip): the current that impinges upon the specimen and generates the various imaging signals. 4.Probe diameter or spot size (dp): the diameter of the final beam at the surface of the specimen. Accelerating voltage: Increasing the accelerating voltage will:
decrease lens aberration and result in a small probe diameter Increase the probe current at the specimen Increase beam penetration into specimen and thus obscure surface details. Increases charge buildup in non conductive specimens Increases damage to beam sensitive specimens 30kV 1kV Important parameters Working Distance: Increasing the working distance will: Increase depth of focus Increase probe size and thus decrease
resolution Increase aberrations due to the need for a weaker lens to focus Important parameters Objective aperture size: Decreasing the diameter of the objective aperture will: Decrease lens aberrations and thus increase resolution Decrease the probe current Decrease the convergence angle of the beam and thus increase depth of focus Important parameters Focus and alignment: An important aspect of aligning the microscope is that the
apertures are centered w.r.t. the optical axis of the microscope. If an objective aperture is not centered the image will move when you try to focus it. The way to correct this is to wobble the current to the objective lens and align the aperture to minimize the movement in both X and Y plane. Important parameters Stigmatism correction: A current is applied to a ring of stigmator coils around the objective lens therefore central beam becomes more
circular/symmetrical. Important parameters Auger software interface SEM software interface