Scanning Electron Microscopy (SEM) Lab

Contents
Objective What is SEM? What kind of information we can get out of it? Major components and their functions Electron beam - specimen interactions Interaction volume Magnification, resolution, depth of field and image contrast Energy Dispersive X-ray Spectroscopy (EDS)

Objective
The objective of SEM lab course is to familiarize the students with scanning electron microscope, its operation and working principle. Provide hands-on experience to operate the instrument

What is SEM
In scanning electron microscopy (SEM) an electron beam is focused into a small probe and is rastered across the surface of a specimen. Several interactions with the sample that result in the emission of electrons or photons. These emitted particles can be collected with the appropriate detector to yield valuable information about the material. The most immediate result of observation in the scanning electron microscope is that it displays the shape of the sample.

What information we can get

Topography The surface features of an object and its texture Morphology The shape and size of the particles making up the object Composition The elements and compounds that the object is composed of and their relative amounts

Why we use electrons

Naked eye can resolve two points about 0.1-0.2mm apart Any instrument that images detail finer than 0.1mm can be claimed as a microscope The resolution of light microscope is limited by the wavelength of visible light (green light wavelength = 550nm)
d = 0.61 / sin
is the refractive index of the medium, for air =1 sin = numerical aperture, can be assumed =1

So the resolution of good light microscope is about 300nm Many microstructural features that influence properties of materials can not be resolved in a light microscope Electrons have very small wavelength therefore are ideal to increase resolution For 20kV electrons = 0.06nm Theoretically it can be used to image species as small as 0.03nm

Major components of SEM

Thermionic guns
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

Tungsten wire

Single crystal of LaB6

Thermionic gun

Field emission gun

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

In field emission guns (FEG) a strong electric field is used to extract electrons -Single crystal of W, etched to a thin tip

Field emission 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.

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.

Electromagnetic lens
Electromagnetic lenses are used to demagnify the image of the electron beam exiting the electron gun and to focus the beam on the specimen
Condenser lens It focuses the electron beam to the objective lens Objective lens determines the final spot size of the electron beam, i.e., the resolution of a SEM.

Specimen stage

Electron-Specimen Interactions
When the electron beam strikes a sample, both photon and electron signals are emitted.

Incident Beam
X-rays - composition info

Backscattered electrons - Atomic number and topographical

Cathodoluminescence - Electrical

Secondary electrons - Topographical

Auger electrons - Surface sensitive compositional

Specimen

Specimen Current
Electrical

Electron sample interaction volume

Electron Sample interaction volume

Interaction volume increases with increasing acceleration voltage and with decreasing atomic number

Electron Sample interaction volume

The incident electrons do not go along a straight line in the specimen, but follow a zig-zag path.

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

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

Everhart-Thornley Detector (E-T)
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.

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.

How do we get an image

Electron gun
156 288 electrons! electrons!

Detector

Image

How do we get an image

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 100 1000 10000 100000 d 1mm 100m 10m 1m

What is Resolution
The smallest distance between two points that can be resolved is called resolution.
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

= 1.22 / E

What is depth of field

It is the range of depth at which an object remains under focus

D=

4x105W AM

(m)

To increase D Decrease aperture size, A

Decrease magnification, M Increase working distance, W

Depth of field

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 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

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.

Important parameters
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

30kV

Increases damage to beam sensitive specimens

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.

Why vacuum?
When a SEM is used, the electron-optical 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 detail in the image.

EDS analysis

Characteristic x-rays
Characteristic x-rays are emitted when electron beam removes an inner shell electron from the sample, causing higher energy electron to fill the shell and release energy. These x-rays are used to identify the compositional analysis

Line scans

EDS detectors
The Solid-State EDS Detector

High purity silicon drifted with lithium System must be cooled to Liquid N2 temperatures. Mounted with a fixed geometry relative to specimen and beam

EDS detectors
The Solid-State EDS Detector
Electrostatically or peltier cooled EDS detector No Liquid N2 requirement, dry.

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

Charging effects
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.

Distortion of image and anomalous contrast due to charging

Charge Neutralization
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

SEM control interface

EDS control interface