Lecture-9 SIMS & NDT

• SIMS
 Basic Principles
 Instrumentation
 Mass Resolution
 Modes of Analysis
 Applications

• Non-Destructive Analysis (NDA)

or Non-Destructive Testing (NDT)
 Instrumentation
Bombardment of a sample surface with a primary ion beam followed by mass spectrometry
of the emitted secondary ions constitutes secondary ion mass spectrometry (SIMS).
Ion Sources
• Ion sources with electron impact ionization - Duoplasmatron: Ar+, O2+, O-
• Ion sources with surface ionization - Cs+ ion sources
• Ion sources with field emission - Ga+ liquid metal ion sources
Mass Analyzers Vacuum < 10−6 torr
• Magnetic sector analyzer
• Quadrupole mass analyzer
• Time of flight analyzer
Ion Detectors
• Faraday cup
• Dynode electron multiplier
Ion detectors
Mass Analyzers Ip
Is Ion sources

Mass analyzers
SIMS CAMECA 6F
http://www.youtube.com/watch?v=IO-KCjxznLs to~1:50
 Cameca SIMS

Accelerating voltage
Secondary ions have low kinetic
energies from zero to a few
hundred eV.
L1, L2 and L3 - electromagnetic lens

http://www.eaglabs.com/mc/sims-instrumentation.html
 Energy Analyzer and Mass Spectrometer
ESA bends lower energy ions more strongly than higher energy ions. The sputtering
process produces a range of ion energies. An energy slit can be set to intercept the high
energy ions. Sweeping the magnetic field in MA provides the separation of ions
according to mass-to-charge ratios in time sequence.

E Mass Analyzer (MA)

Degree (r) of deflection of

ions by the magnetic filed Magnet Sector
Electrostatic depends on m/q ratio.
Sector V - ion acceleration voltage
r - radius of curvature of an ion
Energy
Focal plane

https://www.youtube.com/watch?v=NuIH9-6Fm6U at~3:40-5:16
https://www.youtube.com/watch?v=EzvQzImBuq8 to~2:06
http://www.youtube.com/watch?v=lxAfw1rftIA at~1:00-4:12
 Basic Equations of Mass Spectrometry
Ion’s kinetic E function of
1 2
mv  zV accelerating voltage (V) and
2 charge (z).

F  mv 2 / R
r Centrifugal force
Applied magnetic field
F  Bzv Lorentz force
Balance as ion goes
2
r  Bzv
mv / R through flight tube
Combine equations to obtain:

m / z  B2 R
r 2 / 2V Fundamental equation of mass spectrometry
Change ‘mass-to-charge’ (m/z) ratio by
m/z = m/e changing V or changing B.
for singly charged ions
NOTE: if B, V, z constant, then:

r m r - radius of circular ion path

 MA

ESA
MA
 Ion Detectors
http://www.eaglabs.com/mc/sims-secondary-ion-detectors.html#next
Faraday Cup
Secondary electron Multiplier
20 dynodes Current gain 107
https://www.youtube.com/watch?v=NuIH9-6Fm6U
A Faraday cup measures the
ion current hitting a metal
cup, and is sometimes used
for high current secondary ion
signals. With an electron
multiplier an impact of a
single ion starts off an
electron cascade, resulting in
a pulse of 108 electrons
which is recorded directly.
Usually it is combined with a
fluorescent screen, and
signals are recorded either
with a CCD-camera or with a
fluorescence detector.
at~5:18-6:50 and to~9:25
M/z
 Time of Flight (TOF) SIMS - Reflectron
http://www.youtube.com/watch?v=ZoAUxsEBUnk TOF-SIMS
http://www.youtube.com/watch?v=KAWu6SmvHjc
TOF SIMS is based on the fact that ions with
the same energy but different masses travel
with different velocities. Basically, ions formed
by a short ionization event are accelerated by
an electrostatic field to a common energy and
travel over a drift path to the detector. The
lighter ones arrive before the heavier ones and
a mass spectrum is recorded. Measuring the
flight time for each ion allows the
determination of its mass.

(TOF) SIMS enables the analysis of an

unlimited mass range with high sensitivity and
quasi-simultaneous detection of all secondary Schematic of time of flight (TOF)
ions collected by the mass spectrometer. spectrometer - reflectron
 Time of Flight (TOF) Spectrometer
TOF operates in a pulse mode.
During a short pulse of E, ions are
accelerated and acquire a constant
kinetic energy:
kinetic energy = mv2/2
but have different m/q and Vs.
Thus they arrive to the detector in
time sequence after travel the same
distance. Time required to travel
distance l from the ion origin to the
detector is:

pulse width

Schematic of TOF spectrometer with a spectrum The light ions with higher Vs arrive
In order to provide higher resolution the pulse to the detector first.
should be as narrow as 1-10 ns. The pulse
repetition frequency is usually in a kHz range.
 SIMS can do trace element analysis WDS ~100ppm
EDS ~1000ppm

Detection limit
is affected by
1 and 2 Static SIMS

3 Dynamic SIMS
 Dynamic Secondary Ion Mass Spectrometry
Dynamic SIMS involves the use of a much higher energy primary beam (larger amp
beam current). It is used to generate sample depth profiles. The higher ion flux eats
away at the surface of the sample, burying the beam steadily deeper into the sample
and generating secondary ions that characterize the composition at varying depths. The
beam typically consists of O2+ or Cs+ ions and has a diameter of less than 10 μm. The
experiment time is typically less than a second. Ion yield changes with time as primary
particles build up on the material effecting the ejection and path of secondary ions.
 Dynamic SIMS – Depth Profiling

Factors affecting
depth resolution

http://www.youtube.com/watch?v=-7gSbaslRCU&feature=related
 Crater Effect

(a)

(a) Ions sputtered from a selected central

area (using a physical aperture or electronic
gating) of the crater are passed into the mass
spectrometer.

(b) (b) The beam is usually swept over a large

area of the sample and signal detected from
The analyzed area is usually required to
the central portion of the sweep. This avoids
be at least a factor of 3  3 smaller than
crater edge effects.
the scanned area.
Sample Rotation Effect
 Gate Oxide Breakdown

http://www.youtube.com/watch?v=IO-KCjxznLs&NR=1&feature=endscreen 2:08-2:40
Dynamic SIMS vs Static SIMS
http://www.youtube.com/watch?v=IO-KCjxznLs at~2:45-3:18
 Mapping Chemical Elements
Some instruments simultaneously produce high mass resolution and high
lateral resolution. However, the SIMS analyst must trade high sensitivity for
high lateral resolution because focusing the primary beam to smaller
diameters also reduces beam intensity. High lateral resolution is required
for mapping chemical elements.

197 AU 34 S

The example (microbeam) images show a pyrite (FeS2) grain from a sample of
gold ore with gold located in the rims of the pyrite grains. The image numerical
scales and associated colors represent different ranges of secondary ion
intensities per pixel.
 Summary
 SIMS can be used to determine the composition of organic and
inorganic solids at the outer 5 nm of a sample.
 To determine the composition of the sample at varying spatial and
depth resolutions depending on the method used. This can generate
spatial or depth profiles of elemental or molecular concentrations.
 These profiles can be used to generate element specific images of
the sample that display the varying concentrations over the area of
the sample.
 To detect impurities or trace elements, especially in semi-
conductors and thin filaments.
 Secondary ion images have resolution on the order of 0.5 to 5 μm.
 Detection limits for trace elements range between 1012 to 1016
atoms/cc.
 Spatial resolution is determined by primary ion beam widths, which
can be as small as 100 nm.
SIMS is the most sensitive elemental and isotopic surface
microanalysis technique (bulk concentrations of impurities
of around 1 part-per-billion). However, very expensive.
http://www.youtube.com/watch?v=QTjZutbLRu0 at~1:38-2:14 advantages and disadvantages of SIMS
 Review Questions for SIMS
• What are matrix effects?
• What is the difference between ion yield
and sputtering yield?
• When are oxygen and cesium ions used as
primary ions?
• What is mass resolution?
• How can depth resolution be improved?
• Applications of SIMS
• Advantages and disadvantages of SIMS
 Non-destructive Analysis (NDA)
Non-destructive Testing (NDT)
https://www.nde-ed.org/index_flash.php

 Introduction to NDT
 Overview of Six Most Common NDT Methods
 Selected Applications
https://www.youtube.com/watch?v=tlE3eK0g6vU NDT very good
 Definition of NDT
The use of noninvasive
techniques to determine
the integrity of a material,
component or structure
or
quantitatively measure
some characteristic of
an object.

i.e. Inspect or measure without doing harm.

 What are Some Uses
of NDT Methods?

• Flaw Detection and Evaluation

• Leak Detection
• Location Determination
• Dimensional Measurements Fluorescent penetrant indication

• Structure and Microstructure Characterization

• Estimation of Mechanical and Physical Properties
• Material Sorting and Chemical Composition
Determination
 Why Nondestructive?
• Test piece too precious to be destroyed
• Test piece to be reused after inspection
• Test piece is in service
• For quality control purpose
• Something you simply cannot do harm
to, e.g. fetus in mother’s uterus
 When are NDE Methods Used?
There are NDE applications at almost any stage
in the production or life cycle of a component.
–To assist in product development
–To screen or sort incoming materials
–To monitor, improve or control
manufacturing processes
–To verify proper processing such as
heat treating
–To verify proper assembly
–To inspect for in-service damage
Six Most Common NDT Methods
Detection of surface flaws
• Visual
• Liquid Penetrant
• Magnetic
Detection of internal flaws
• Ultrasonic
• Eddy Current
• Radiography
1. Visual Inspection
Most basic and common
inspection method.

Tools include
fiberscopes,
borescopes, magnifying
glasses and mirrors.

Portable video inspection

unit with zoom allows
inspection of large tanks
and vessels, railroad tank
cars, sewer lines.
Robotic crawlers permit
observation in hazardous or
tight areas, such as air
ducts, reactors, pipelines.
 https://www.youtube.com/watch?v=xEK-c1pkTUI to~2:26
Low surface wetting
Liquid Penetrant Inspection
• A liquid with high surface wetting characteristics
is applied to the surface of the part and allowed
time to seep into surface breaking defects.
• The excess liquid is removed from the surface
of the part.
• A developer (powder) is applied to pull the
trapped penetrant out the defect and spread it High surface wetting
on the surface where it can be seen.
• Visual inspection is the final step in the
process. The penetrant used is often loaded
with a fluorescent dye and the inspection is
done under UV light to increase test
sensitivity.

https://www.youtube.com/watch?v=tlE3eK0g6vU at~2:48-3:33 https://www.youtube.com/watch?v=bHTRmTQDZzg

 Magnetic Particle Inspection (MPI)
• A NDT method used for defect detection. Fast and relatively
easy to apply and part surface preparation is not as critical as
for some other NDT methods. – MPI one of the most widely
utilized nondestructive testing methods.
• MPI uses magnetic fields and small magnetic particles, such
as iron filings to detect flaws in components. The only
requirement from an inspectability standpoint is that the
component being inspected must be made of a
ferromagnetic material such as iron, nickel, cobalt, or
some of their alloys. Ferromagnetic materials are materials
that can be magnetized to a level that will allow the inspection
to be effective.
• The method is used to inspect a variety of product forms such
as castings, forgings, and weldments. Many different
industries use MPI for determining a component's fitness-
for-use. Some examples of industries that use magnetic
particle inspection are the structural steel, automotive,
petrochemical, power generation, and aerospace industries.
Underwater inspection is another area where magnetic particle
inspection may be used to test such things as offshore
structures and underwater pipelines.
https://www.youtube.com/watch?v=tlE3eK0g6vU at~1:10-2:48 MPI
https://www.nde-ed.org/EducationResources/CommunityCollege/MagParticle/cc_mpi_index.php
 https://www.youtube.com/watch?v=qpgcD5k1494 to~3:03

Magnetic Particle Inspection

The part is magnetized. Finely milled iron particles coated with a
dye pigment are then applied to the specimen. These particles
are attracted to magnetic flux leakage fields and will cluster to
form an indication directly over the discontinuity. This indication
can be visually detected under proper lighting conditions.
Flux leakage

Cracks just below the surface

The magnetic particles form a can also be revealed.
ridge many times wider than
Relative direction between the
the crack itself, thus making the
magnetic field and the defect
otherwise invisible crack visible.
line is important.
https://www.youtube.com/watch?v=dQoB7jpxSe8 MPI testing procedure
 Magnetic particles
• Pulverized iron oxide (Fe3O4) or
carbonyl iron powder can be used
• Colored or even fluorescent
magnetic powder can be used to
increase visibility
• Powder can either be used dry or
suspended in liquid
Examples of visible dry magnetic particle indications

Indication of a crack in a saw blade Indication of cracks in a weldment

Before and after inspection pictures of Indication of cracks running between

cracks emanating from a hole attachment holes in a hinge
Examples of Fluorescent Wet Magnetic
Particle Indications
Magnetic particle wet fluorescent
indication of a cracks in a drive shaft

Magnetic
particle wet
fluorescent
indication of
a crack in a
bearing

Magnetic particle wet fluorescent

indication of a cracks at a
fastener hole
 Advantages of MPI
 One of the most dependable and sensitive
methods for surface defects
 fast, simple and inexpensive
 direct, visible indication on surface
 unaffected by possible deposits, e.g. oil,
grease or other metals chips, in the cracks
 can be used on painted objects
 results readily documented with photo or tape
impression
 Limitations of MPI

 Only good for ferromagnetic materials

 sub-surface defects will not always be
indicated
 relative direction between the magnetic field
and the defect line is important
 objects must be demagnetized before and
after the examination
 the current magnetization may cause burn
scars on the item examined
https://www.youtube.com/watch?v=gqJN8tyosDw to~0:42

Ultrasonic Inspection
(Pulse-Echo)
In ultrasonic testing, high-frequency
sound waves are transmitted into a
material to detect imperfections or to
locate changes in material properties.
The most commonly used
ultrasonic testing technique is
pulse echo, whereby sound is
introduced into a test object
and reflections (echoes) from
internal imperfections or the
part's geometrical surfaces are
returned to a receiver. The
time interval between the
transmission and reception of
pulses give clues to the
internal structure of the
material.
https://www.youtube.com/watch?v=tlE3eK0g6vU at~6:45-8:00 or to 11:35
 Ultrasonic Inspection (Pulse-Echo)
High frequency sound waves are introduced into a material and
they are reflected back from surfaces or flaws.
Reflected sound energy is displayed versus time, and inspector
can visualize a cross section of the specimen showing the depth
of features that reflect sound.
Principle of ultrasonic testing Ultrasonic Probe f
LEFT: A probe sends a sound wave
into a test material. There are two
indications, one from the initial
pulse of the probe, and the second
due to the back wall echo.
RIGHT: A defect creates a third
indication and simultaneously
reduces the amplitude of the back
wall indication. The depth of the
defect is determined by the
ratio D/Ep
Ultrasonic probe is made of piezoelectric Oscilloscope, or flaw detector screen
transducers. https://www.youtube.com/watch?v=UM6XKvXWVFA at~1:18-3:08
http://www.doitpoms.ac.uk/tlplib/piezoelectrics/applications.php
 How It Works?
At a construction site, a technician
tests a pipeline weld for defects
using an ultrasonic instrument.
The scanner, which consists of a
frame with magnetic wheels,
holds the probe in contact with
the pipe by a spring. The wet area
is the ultrasonic couplant
(medium, such as water and oil)
that allows the sound to pass into
the pipe wall.
Spline cracking
Non-destructive testing of a swing
shaft showing spline cracking. Backwall
Spline – any of a series of projections on a
shaft that fit into slots on a corresponding
Lower end Upper end
shaft, enabling both to rotate together.
https://www.youtube.com/watch?v=UM6XKvXWVFA
at~3:08-4:10
 Images obtained by C-Scan
High resolution scan can produce very detailed images. Both images
were produced using a pulse-echo techniques with the transducer
scanned over the head side in an immersion scanning system.

Gray scale image produced using Gray scale image produced using the
the sound reflected from the front sound reflected from the back surface
surface of the coin of the coin (inspected from “heads” side)
Applications of Ultrasonic Inspection
Ultrasonic inspection is often performed on steel and other metals and
alloys, though it can also be used on concrete, wood and composites,
albeit with less resolution. It is used in many industries including steel
and aluminium construction, metallurgy, manufacturing, aerospace,
automotive and other transportation sectors.
Limitations of Ultrasonic Inspection
1. Manual operation requires careful attention by experienced
technicians.
2. Extensive technical knowledge is required for the development of
inspection procedures.
3. Parts that are rough, irregular in shape, very small or thin, or not
homogeneous are difficult to inspect.
4. Surface must be prepared by cleaning and removing loose scale,
paint, etc.
5. Couplants are needed to provide effective transfer of ultrasonic wave
energy between transducers and parts being inspected unless a non-
contact technique is used.
6. Inspected items must be water resistant, when using water based
couplants that do not contain rust inhibitors.
 Eddy Current Testing (ECT)
Electrical currents are generated in a conductive material by an
induced alternating magnetic field. The electrical currents are
called eddy currents because they flow in circles at and just
below the surface of the material. Interruptions in the flow of
eddy currents, caused by imperfections, dimensional changes, or
changes in the material's conductive and permeability properties,
can be detected with the proper equipment.

• Eddy current testing can be used on all electrically

conducting materials with a reasonably smooth surface.
• The test equipment consists of a generator (AC power
supply), a test coil and recording equipment, e.g. a
galvanometer or an oscilloscope
• Used for crack detection, material thickness measurement
(corrosion detection), sorting materials, coating thickness
measurement, metal detection, etc.

https://www.youtube.com/watch?v=tlE3eK0g6vU at~11:36-12:38
 Eddy Current Instruments
Voltmeter
Coil's
Coil magnetic field

Eddy current's
magnetic field
Eddy
currents

Conductive
material
https://www.youtube.com/watch?v=zJ23gmS3KHY to~1:24 what is Eddy current
 https://www.youtube.com/watch?v=9A5fQtOwnzw

Applications of ECT
•Crack Detection
•Material Thickness
Measurements
•Coating Thickness
Measurements
•Conductivity Measurements for
Material Identification
•Heat Damage Detection
•Case Depth Determination
•Heat Treatment Monitoring

Here a small surface probe is scanned

over the part surface in an attempt to
detect a crack.
 Advantages of ECT

• Sensitive to small cracks and other defects

• Detects surface and near surface defects
• Inspection gives immediate results
• Equipment is very portable
• Method can be used for much more than flaw detection
• Minimum part preparation is required
• Test probe does not need to contact the part
• Inspects complex shapes and sizes of conductive materials
 Limitations of ECT
• Only conductive materials can be inspected
• Surface must be accessible to the probe
• Skill and training required is more extensive than other
techniques
• Surface finish and roughness may interfere
• Reference standards needed for setup
• Depth of penetration is limited
• Flaws such as delaminations that lie parallel to the probe coil
winding and probe scan direction are undetectable
 Radiography
Radiography involves the use of penetrating
gamma- or X-radiation to examine material's
and product's defects and internal features. An High Electrical Potential
X-ray machine or radioactive isotope is used
as a source of radiation. Radiation is directed Electrons
through a part and onto film or other media.
+ -
The resulting shadowgraph shows the internal
features and soundness of the part. Material
thickness and density changes are indicated
X-ray Generator or
as lighter or darker areas on the film. Radioactive Source
Creates Radiation

Radiation
Penetrate
the Sample

Exposure Recording Device

https://www.youtube.com/watch?v=VscasN8jgfo Introduction to radiography

 Film Radiography
The part is placed between the
radiation source and a piece of
film. The part will stop some of the
radiation. Thicker and more dense
area will stop more of the radiation.
• The film darkness (density) will
vary with the amount of radiation
reaching the film through the
X-ray film test object.
• Defects, such as voids, cracks,
inclusions, etc., can be detected.

= less exposure

Top view of developed film = more exposure

https://www.youtube.com/watch?v=tlE3eK0g6vU at~3:35-6:45
 Applications of Radiography
• Can be used in any situation when one wishes to view the
interior of an object
• To check for internal faults and construction defects, e.g.
faulty welding
• To ‘see’ through what is inside an object
• To perform measurements of size, e.g. thickness
measurements of pipes

Limitations of Radiography
• There is an upper limit of thickness through which the
radiation can penetrate, e.g. -ray from Co-60 can
penetrate up to 150mm of steel
• The operator must have access to both sides of an object
• Highly skilled operator is required because of the potential
health hazard of the energetic radiations
• Relative expensive equipment
Radiographic Images
 Examples of radiograph

Burn through (icicles) results when too much heat causes

excessive weld metal to penetrate the weld zone. Lumps of
metal sag through the weld creating a thick globular condition
on the back of the weld. On a radiograph, burn through
appears as dark spots surrounded by light globular areas.
For More Information on NDT

The Collaboration for

NDT Education

www.ndt-ed.org

The American Society

for Nondestructive
Testing

www.asnt.org
 Review Questions for NDT
• Applications of NDT
• What are six most common NDT methods?
• Can liquid penetrant inspection be used to detect
internal flaws? Why?
• Why relative direction between the magnetic field
and the defect line is important in magnetic
particle inspection?
• Why are couplants needed for ultrasonic
inspection (UI)? Limitations of UI?
• Advantages and disadvantages of eddy current
testing.
• What is rediography? Limitations of radiography.