SEM + EDX

Description of the technique

In Scanning Electron Microscopy a primary electron beam is scanned over the sample surface. Different phenomena such as generation of
secondary electrons (SE), backscattering of the incident electrons (BSE) and emission of X-rays take place. These signals are used by the
corresponding detectors for image formation.
- Secondary electrons are emitted from the uppermost surface of the sample (10 nm). The emission intensity depends on the topography and
the composition of the sample surface.
- Backscattered electrons occur after elastic or quasi-elastic scattering of the primary electrons. The intensity of the BSE signal depends on
the average atomic number of the area illuminated by the impinging beam.
- Inelastic scattering of the incident electrons gives rise to the emission of X-rays with energies characteristic of the atoms in the specimen.
X-ray detectors provide qualitative and quantitative information about the elemental composition.

Instrument

Leica 430i (LEO) equipped SE, BSE and X-ray detectors

SE, BSE modes
Spatial resolution (X, Y) : 5 nm
Magnification : 80 to 300,000
EDX analysis
Spatial resolution (X,Y) : Submicrometer
Detection limits : 0.1 to 100 %
Elemental range : Be to U
Quantitative analysis : Yes

Elemental mapping : Yes

Unique advantages of the technique

Elemental mapping by EDX

Topographical information by SE
Mass density information by BSE
Easy to use
Capability to analyse large samples

SEM Applications
Imaging ANALYSIS:
Biological samples
Ceramics

Composites
Metals
Minerals
Polymers
Semiconductors
Further Materials

EDX MEASUREMENTS:
Linescan measurements
Elemental distribution mapping of elements

SEM Methods

Cutaway of column and chamber

The normal operating vacuum of 10 -4 to 10-6 Torr is reached by a turbomolecular pump which is backed by a rotary pump.

The large working chamber of the SEM allows to observe samples up to 150 mm and 2 kg of weight. The samples are able to be orientated
along 5 axes.

Stage movements and chamber size

An advantage in operating the instrument is its easy manipulation that is completely computer controlled. The PC environment used is
Microsoft Windows. The SEM control application runs within this system.
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Scanning Electron Microscopy

Scanning electron microscopy (SEM) is the best known and most widely-used of the surface analytical techniques.
High resolution images of surface topography, with excellent depth of field are produced using a highly-focused,
scanning (primary) electron beam. The primary electrons enter a surface with an energy of 0.5 - 30 keV, and
generate many low energy secondary electrons. The intensity of these secondary electrons is largely governed by

the surface topography of the sample. An image of the sample surface can thus be constructed by measuring
secondary electron intensity as a function of the position of the scanning primary electron beam. High spatial
resolution is possible because the primary electron beam can be focused to a very small spot (<10 nm). High
sensitivity to topographic features on the outermost surface (<5 nm) is achieved when using a primary electron
beam with an energy of <1 keV.

LEO 440 Scanning Electron Microscope

In addition to low energy secondary electrons,

backscattered electrons and X-rays are also
generated by primary electron bombardment.
The intensity of backscattered electrons can be
correlated to the atomic number of the element
within the sampling volume. Hence, some
qualitative elemental information can be
obtained. The analysis of characteristic X-rays
emitted from the sample gives more
quantitative elemental information. Such Xray analysis can be confined to analytical
volumes as small as 1 cubic micron.

SEM, accompanied by X-ray analysis, is considered a relatively rapid, inexpensive, and basically non-destructive approach to surface analysis. It is often used to survey surface
analytical problems before proceeding to techniques that are more surface-sensitive and more specialized.
Two scanning electron microscopes are available at SSW. There is a LEO440 conventional microscope equipped with a Gresham light element detector and a Quartz Xone energy
dispersive X-ray (EDX) analysis system. The LEO SEM is used for most routine examinations and analysis of a wide variety of materials. The EDX system is capable of detecting
all elements from carbon to uranium, with a detection limit of ~ 0.5 wt% for most elements. Backscattered electron imaging and elemental X-ray mapping provide graphic
presentation of elemental distribution. The Quartz Xone system uses full spectral imaging. This means that all of the X-ray events that occur at each pixel are recorded. This allows
for live and post collection data analysis. Also, standardless quantitative elemental analysis is available.

We also have an Hitachi S-4500 field emission

SEM fully equipped with an EDAXTM EDX
system. The Hitachi S-4500 is used for samples
that require the utmost in spatial resolution and
imaging of the outermost surface. At high
electron beam voltages (>15 kV) a spatial
resolution of <2 nm is possible. This means that
useful images at magnifications of 100 KX or
greater can be obtained. Also, this field
emission SEM has superb low voltage
capability with <5 nm resolution available at 1
kV beam voltages. EDX X-ray intensity
element mapping and quantitative linescans are
available on this instrument.

Hitachi S-4500 Field Emission SEM

This low voltage capability means that many samples that normally require coating to reduce charging problems can be examined without coating. Also, the true outer surface
morphology can be imaged.
For theLEO microscope, samples up to 250 x 250 x 70 mm in size can be examined. For the Hitachi microscope a maximum size of 50 mm diameter (~ 20 mm thick) can be
accommodated. The complete analysis time can vary greatly, depending on the complexity of the analysis required. Typically, a study of a sample surface, including several
micrographs and EDX analysis, would take about one hour.
Some typical examples of the uses of scanning electron microscopy are:

SEM imaging of a corroded copper surface

EDX analysis and mapping of dust from Beijing
Paint crater defect caused by anti-perspirant (EDX and mapping)
Microstructure of sputter deposited silver film
Composition of metallic brakepad
Pinhole in paint caused by cracks in the steel substrate
SEM/EDX and paint defect analysis

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SEM Imaging of a Corroded Copper Surface

Copper is being investigated as a potential container material for long-term underground storage. This sample was exposed to a low pH solution containing dissolved oxygen and
chloride species for a period of 12 months. The main objective of this study was to determine the corrosion behaviour of copper under conditions similar to those expected in
underground storage. Scanning electron micrographs, obtained using a Hitachi S-4500 field emission scanning electron microscope (FESEM), indicate that the extent of general
corrosion was minimum; however, localized corrosion attack, in the form of crystallographic etching, could be seen in these secondary electron micrographs. In addition, the
presence of edge and screw dislocations can also be seen in these micrographs.

Figure 1. SEM image showing the crystalline structure of the etched copper.

Figure 2. SEM image of kink and edge dislocations.

Figure 3. SEM image of a screw dislocation.

Figure 4. SEM image of extensive etching of a variety of screw dislocations.

Figure 5. SEM image of a screw and edge dislocation.

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EDX Analysis and Mapping of Dust from Beijing

Figure 1: Silicon

Figure 2: Aluminum

Figure 4: Iron

Figure 3: Calcium

Figure 5: Potassium

Figure 6: Magnesium

Figure 7: Sodium
Figure 8: Oxygen

Figure 10: Zirconium

Figure 9: Sulphur

X-Ray Intensity Composite Map with EDX Analysis of Different Phases and Possible Phase Identification (See EDX Spectra
Below)

Applications Include:
Materials Evaluation:
- Grain size
- Surface roughness
- Porosity
- Particle size
- Intermetallic distribution

Failure Analysis:
- Root cause failure
determination
- Corrosion failures
- Electrostatic discharge
- Ductile and brittle
fractures
- Fatigue fractures
- Failure mode
identification

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Services : FE-SEM / EDX

What is FE-SEM / EDX?

What is FE-SEM / EDX?

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Field Emission Scanning Electron Microscopy (FESEM) is a high-resolution

imaging technique providing topographical and structural information in plan
view or in cross-section. Often used in conjunction with SEM, Energy
Dispersive X-Ray Spectroscopy (EDX) is used to qualitatively and
quantitatively analyze the elements present in a selected area of the SEM
image. Together FE-SEM and EDX capabilities allow the irradiation by a
focused electron beam, imaging secondary or backscattered electrons and
energy analysis of x-rays.
Typical SEM applications include plan view and cross-sectional imaging for
process development and failure analysis. EDX applications include specific
defect analysis or compositional analysis (for boron and heavier elements).
FE-SEM / EDX at Accurel

Decapsulation/Delid
Emission Microscopy
FIB and Dual-FIB
Quick-Turn Packaging
SEM and FE-SEM / EDX
E-Beam Probing

FE-SEM / EDX:

FE-SEM / EDX at Accurel

Main Applications

Specifications

Table of Figures:

Accurel and Materials Analysis Group offer a wide variety of analytical

services specifically geared towards achieving higher production yields and
long term reliability in the semiconductor industry. Our customers often
request Process Monitoring which can be provided by FE-SEM analysis of
polished IC cross-sections. We have developed a sample preparation
technique whereby it is possible to document an IC fabrication process,
usually with a single polished cross-section (FE-SEM Fig. 1).

Flip Chip FIB

Real Time X-Ray
Turn-Key Failure Analysis
Deprocessing
CIVVA
SAM
TEM

Among the 5 SEM systems in-house, Accurel and Materials Analysis Group
possess two high resolution JEOL JSM-6320F FESEM's equipped with cold
cathode field emission electron guns capable of 1.2 and 2.5 nm microscope
resolution at 15 and 1 kV respectively, a 500 - 650,000x magnification range,
and 50 x 70 mm stage movement (maximum sample size 32 mm). Operation
at low beam energies minimizes damage of electron beam sensitive materials
and charge build-up on insulating specimens. The Philips XL-30 FEG
incorporates a thermally-assisted Schottky source and provides 2 nm
microscope resolution at 30 kV, a 25 - 200,000x magnification range, and 20 x
20 mm stage movement.

FE-SEM Figure 1:
FESEM micrograph of polished IC
cross-section showing stacked via
structure.
(Click for a larger image)

We also can provide specific information about various unique device

structures such as high resistance contacts or vias. We have developed
techniques that allow us to cross-section very specific "problem" structures
with great accuracy.
Non-conductive materials usually require coating with a thin metallic layer to
be imaged in the FE-SEM. Our ion beam coater offers significant
improvement over typical sputter coaters by depositing an amorphous
continuous coating to eliminate decoration effects. (FE-SEM Fig. 6a & 6b)
Accurel and Materials Analysis Group have a super ultra-thin window EDAX
DX4i detector as well as a Noran Voyager EDX which is optimized for light
element detection. EDX capability provides excellent peak separation at low xray energies (FE-SEM Fig. 7). All elements heavier than Be can be analyzed
with a typical detection limit of 0.2 - 1 wt.%. The depth sampled can range
from 0.5 - 3 m depending on the material and the beam energy selected. The
distribution of elements can be displayed as digital x-ray maps (FE-SEM Fig.
8) with a typical lateral resolution of 0.5 m.

FE-SEM Figure 2:
Polished cross-section showing
poor metal step coverage due to
profile of via hole.
(Click for a larger image)

Main Applications

FE-SEM's advanced technology features provide for surface structure

analysis, morphology, backscatter imaging, increased depth of field, and
profiles. FE-SEM's high resolution imaging is often used to analyze materials
with poor electrical conductivity.

FE-SEM Figure 3:
Cross-section showing excessive
epitaxial Si at a contact interface.
(Click for a larger image)

Sample preparation is often required for random and precision cross-sections

of metallographical samples. Typical sample preparation includes cleaves,
cross-sectioning of packages, and frontside and backside lapping.
PROCESS MONITORING

Field oxidation
Formation of gates, contacts, and vias
Local interconnect lines
Metallization step coverage
Planarization techniques such as Spin On Glass (SOG) or Chemical

FE-SEM Figure 4:
Cross-section showing incomplete
etching of a contact hole.
(Click for a larger image)

Mechanical Polish (CMP)

UNIQUE DEVICE STRUCTURES

Anomalies such as poor metal step coverage due to the etched profile of via
holes (FE-SEM Fig. 2), polymer residue at the via interface, or excessive
epitaxial silicon formation at contact interfaces (FE-SEM Fig. 3) are often a
problem. Other anomalies such as incomplete or overetched vias and contact
holes (FE-SEM Fig. 4) can be easily remedied once the extent of the problem
has been documented. Barrier layers such as TiW and TiN which are
commonly used to prevent interdiffusion across interfaces can sometimes fail
(FE-SEM Fig. 5).
FE-SEM Figure 6a shows a zeolite Y powder imaged with traditional DC
magnetron AuPd magnetron sputtered coating. The structure of the coating is
clearly visible as a "cracked" pattern on the grains which could lead to
erroneous conclusions about grain size and texture. FE-SEM Figure 6b shows
the same material coated with a thin layer of tungsten in our ion beam coater.
The coating is now invisible, thereby allowing the true structure of the material
to be imaged.

FE-SEM Figure 5:
Cross-section showing failure of
TiN barrier layer at Al/W interface.
(Click for a larger image)

Specifications

6 Systems
JEOL JSM-6320F (2)
JEOL JSM-6400F (1)
Philips XL-30FEG
JEOL JSM-6100
Advanced Technology
Surface structure analysis
Morphology
Backscatter imaging
Increased depth of field
Profiles
Field Emission (FE-SEM)
High resolution
Analysis of materials with poor electrical conductivity
Increased signal to noise ratio
1.2 nm resolution and 2.5 nm resolution at
15 and 1 kV respectively
EDX Capability
EDAX DX4i detector
Noran Voyager EDX
Elemental analysis

FE-SEM Figure 6a:

Comparison of a) conventional
Au/Pd coating to.
(Click for a larger image)

FE-SEM Figure 6b:

ion beam W coating. ( Courtesy of
Catalytica Advanced
Technologies ).
(Click for a larger image)

Qualitative / Quantitive analysis

X-Ray Maps with lateral resolution of 0.5 m
Detection limit of 0.2 - 1 wt.%
Depth range from 0.5 - 3 m
KLA Stage Navigation
6" Wafer Capability
Defect Analysis
Precision cross-sections
Sample Preparation
Random and precision cross-sections
Cleaves (e.g. photo resist, metal lines)
Cross-sectioning of packages
Metallographical samples
Frontside and backside lapping
Philips XL-40

FE-SEM Figure 7:
EDX spectra showing good
sensitivity and peak separation for
light elements.
(Click for a larger image)

FE-SEM Figure 8:
Color digital x-ray map showing
elemental distribution.
(Click for a larger image)

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