Bruker QUANTAX EDS User manual

QUANTAX EDS
Energy-dispersive X-ray spectrometer
for electron microscopy
User Manual

Bruker Nano GmbH
Am Studio 2D
12489 Berlin
Tel. [phone]
Fax [phone]
E-mail [e-mail]
Internet www.bruker.com
The reproduction, transmission or use of this document or its contents is not permitted without express
written authority. Offenders will be liable for damages. All rights reserved.
We have checked the contents of this manual for agreement with the hardware and software described.
Since deviations cannot be precluded entirely, we cannot guarantee full agreement. However, the data in
this manual are reviewed regularly and any necessary corrections are included in subsequent editions.
Suggestions for improvement are welcome.
Order no. DOC-M82-EXS066
© 2015 Bruker Nano GmbH, Berlin, Germany.
All trademarks and registered trademarks are the sole property of their respective owners.
Printed in the Federal Republic of Germany.

Contents QUANTAX EDS
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Contents
1Introduction .................................................................................................................................. 5
2Safety Information ....................................................................................................................... 7
2.1 Radiation Safety ........................................................................................................... 9
2.2 Beryllium .................................................................................................................... 10
2.3 Electrical Safety.......................................................................................................... 10
2.4 Electromagnetic Compatibility ................................................................................... 11
3The QUANTAX EDS System ..................................................................................................... 13
3.1 Hardware System Components................................................................................. 15
3.1.1 XFlash®Energy Dispersive X-ray Detectors ................................................. 15
3.1.2 Signal Processing Unit................................................................................... 15
3.1.3 Spectrometry Data Interface and EM Control............................................... 16
3.1.4 Computer Workstations ................................................................................ 17
3.2 ESPRIT 2 Software..................................................................................................... 18
3.3 General Operating Instructions .................................................................................. 19
3.3.1 Detector Maintenance................................................................................... 19
3.3.2 Electronic Units ............................................................................................. 20
3.3.3 Software and Data Handling.......................................................................... 21
4The ESPRIT 2 Software.............................................................................................................. 23
4.1 Start-up and Login ...................................................................................................... 25
4.2 User Administration ................................................................................................... 26
4.3 Workspaces................................................................................................................ 28
4.4 Display Control ........................................................................................................... 29
4.5 Configurator Bar ......................................................................................................... 31
4.5.1 Sample Configuration .................................................................................... 32
4.5.2 Standards Configuration ................................................................................ 32
4.5.3 Microscope Configuration ............................................................................. 33
4.5.4 Scan Configuration ........................................................................................ 34
4.5.5 EDS Configuration ......................................................................................... 36
4.5.6 Additional Configurators ................................................................................ 37
4.5.7 Report............................................................................................................ 38
4.5.8 Project ........................................................................................................... 38
4.6 Loading and Saving Data and Results........................................................................ 39
4.7 System Functions ...................................................................................................... 41
4.7.1 System .......................................................................................................... 41
4.7.2 Appearance.................................................................................................... 43
4.7.3 Spectrometer ................................................................................................ 44
4.7.4 Imaging.......................................................................................................... 45
4.7.5 WDS .............................................................................................................. 47
4.7.6 Microscope.................................................................................................... 47
4.7.7 Stage ............................................................................................................. 47
4.8 The Help System........................................................................................................ 47
5Step-by-Step Guides.................................................................................................................. 49
5.1 Preparatory Steps....................................................................................................... 51
5.2 Energy-Channel Calibration ........................................................................................ 53

User Manual Contents
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5.3 Image Capture ............................................................................................................ 55
5.4 Image Extension......................................................................................................... 57
5.5 Drift Correction ........................................................................................................... 59
5.6 Image Processing ....................................................................................................... 61
5.7 Spectrum Acquisition ................................................................................................. 63
5.8 Using the Spectrum Chart .......................................................................................... 65
5.9 Sample Coating Correction......................................................................................... 68
5.10 System Factor Calibration/ Beam Current Setting......................................................70
5.11 Standards Library........................................................................................................ 73
5.11.1 Maintain Standards Library for Bulk Samples................................................73
5.11.2 Maintain Standards Library for Electron Transparent Samples –
Cliff-Lorimer Factors ......................................................................................76
5.11.3 Maintain Standards Library for Electron Transparent Samples –
Zeta Factors ................................................................................................... 78
5.12 Quantitative EDS Analysis of Bulk Samples...............................................................81
5.12.1 Using the Method Editor ............................................................................... 81
5.12.2 Standardless Quantification ...........................................................................83
5.12.3 Standard-based Quantification with a Temporary Reference........................86
5.12.4 Standard-based Quantification with Standards Library..................................88
5.13 Quantitative EDS of Electron Transparent Samples...................................................90
5.13.1 Standardless Cliff-Lorimer Quantification ......................................................90
5.13.2 Standard-based Cliff-Lorimer Quantification..................................................92
5.13.3 Standard-based Zeta Quantification............................................................... 94
5.14 Object Analysis........................................................................................................... 96
5.15 Line Scan .................................................................................................................... 98
5.16 Quantitative Line Scan (QLine) .................................................................................100
5.17 Map Acquisition........................................................................................................ 102
5.18 Quantitative Mapping (QMap) .................................................................................. 104
5.19 Map Processing........................................................................................................ 106
5.20 Phase Analysis.......................................................................................................... 109
5.21 Creating a Report...................................................................................................... 112
5.22 Managing Projects.................................................................................................... 114
Index................................................................................................................................................ 117

1Introduction
QUANTAX is the ideal all-purpose energy dispersive microanalysis system for industry,
research and education. Different system levels and various options are provided for
scaling and tuning of QUANTAX to a broad range of analysis tasks and application
environments. QUANTAX microanalysis systems are suitable for scanning electron
microscopes, transmission electron microscopes, electron beam microprobes, dual beam
devices, as well as other X-ray spectrometry applications.
All QUANTAX systems provide state-of-the-art qualitative and true standardless
quantitative microanalysis for bulk specimens, polished samples, thin layers, particles,
and rough surfaces. This is accomplished by optimized automatic or interactive spectrum
analysis methods, fundamental parameter approaches (e.g. P/B-ZAF) and the most exact
and comprehensive atomic database available. Different standard-based quantification
packages are optionally available. The unique capability of combining standard-based and
standardless analysis methods (hybrid quantification) completes the range of analytical
possibilities.
An intuitive user interface, the flexible project management package, as well as various
options for quick and comprehensive report generation complement the analysis
toolboxes. The software tools are tailored to meet both the needs of the novice as well as
the experienced user. All QUANTAX systems’ ESPRIT software includes an online help
system and supports remote diagnosis and assistance via the Internet.
This manual provides a general software overview and a practical step-by-step description
of the most common measurement procedures that can be performed with the
QUANTAX EDS system. The integrated assistants and the online help of the ESPRIT
software provide additional support. Details on the individual hardware parts and
additional technical data are contained in separate manuals. The individual device manuals
also contain further references regarding operational safety. Please follow all safety
instructions closely to avoid hazards to personal safety and equipment. In case of
necessary maintenance, reinstallation, severe computer breakdown, hardware changes,
etc. the Bruker customer support or your local supplier have to be contacted for further
assistance and instructions.
According to the modular structure of QUANTAX not all parts of this manual may apply in
detail to a given installation nor should be taken literally in all cases. For instance, where
the general term “electron microscope” (EM) is used, this applies to the whole class of
electron-beam or dual-beam systems; SEM includes also STEM, microprobes, or other
scanning devices.
The ESPRIT software layout may vary according to the modules installed on your system
and therefore may differ slightly from what is shown in the illustrations and figures.

2Safety Information
2.1 Radiation Safety ........................................................................................................... 9
2.2 Beryllium .................................................................................................................... 10
2.3 Electrical Safety.......................................................................................................... 10
2.4 Electromagnetic Compatibility ................................................................................... 11

User Manual 2 Safety Information
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2.1 Radiation Safety QUANTAX EDS
9
Operation of the QUANTAX EDS
microanalysis
system is restricted to trained personnel
familiar
with the system as well as the product
documentation, general safety pre
cautions, and
laboratory rules. A briefing on safety issues is
given
at the time of installation or during user training.
Local, state, or federal regulations have to be taken
into account additionally to the safety instructions
given here. Additional instructions for specific parts
of the QUANTAX system - e.g. the X-ray detectors -
may be contained in the according manuals.
The QUANTAX EDS microanalysis system may only
be used in combination with electron microscopes or
similar devices. Any other use beyond that is
considered non-intended usage. The operator,
not
the manufacturer, assumes sole liability for all
personal injury and material damage arising from
non-intended usage.
2.1 Radiation Safety
Changes to the original detector
installation are strictly prohibited.
Radiation safety may be impaired by
improper installation or de-installation.
The QUANTAX microanalysis system uses
the
X-radiation that is generated by
sample interaction
with electrons from the electron source o
f the
microscope or photons emitted by the optional X-
ray
source. Microscopes
and attachments approved by
the microscope vendors are generally designed
to
shield this type of radiation sufficiently.
The QUANTAX XFlash®
detector is installed
according to th
e applicable radiation safety
regulations. Changes to the original installation and
equipment, including flanges, vacuum sealing,
support, etc. are strictly prohibited.
In case the XFlash®detector has to be uninstalled,
make sure that the original blind flange
of the
electron microscope vendor is used to seal the
sample chamber port. In case the original flange is
not available contact th
e microscope vendor for
support.

User Manual 2 Safety Information
10
2.2 Beryllium
Beryllium is highly toxic!
If a beryllium window is destroyed
despite all caution, absolutely all frag-
ments must be carefully collected and
disposed of according to regulations.
Beryllium safety issues apply only to X-
ray detectors
with beryllium X-
ray entrance windows. Low energy
windows do not contain toxic substances.
Beryllium is toxic
if parts are inhaled or swallowed.
With X-
ray detectors, however, this is only possible
in the rare case of a window breaking. S
pecial care
must be taken with XFlash®detectors, as they
do
not contain enough vacuum to suck in the remains
of
a broken window, as a UHV-Dewar normally does.
In case of an accidental destruction
of a beryllium
window, gather all fragments thoroughly and collect
them using pieces of adhesive tape. The was
te has
to be labeled and disposed of
according to the local
safety hazard regulations. Wear a filter mask
during
cleaning up.
2.3 Electrical Safety
High voltage inside. Do not remove
covers.
All parts have been designed according to the safety
requirements for electrical equipment for
measurement, control and laboratory use, or
the
European Low Voltage Directive, respectively. The
system must be correctly installed and used only for
the purposes it is designed for
. Especially grounding
of the system or system parts - as performed during
installation - must not be changed for any
reason. In
case of any supplements or replacement parts
being
installed
, supply voltage settings must be checked
and adjusted to the local mains voltage.
Certain p
arts of the system may contain dangerous
voltages. No covers need to be removed during
regular operation; maintenance sho
uld only be
carried out by trained and certified personnel.

2.4 Electromagnetic Compatibility QUANTAX EDS
11
2.4 Electromagnetic Compatibility
Due to its physical construction
, the highly sensitive
X-
ray detector may not fully comply with common
standards regarding
electromagnetic immunity of
general electronic equipment.
This is not a
disadvantage under normal circumstances
because
the QUANTAX system
works under the same
conditions as electron microscopes and
the
laboratory environment is
designed to meet the
requirements of these instruments.
Bruker devices fulfill all requirements
regarding
active electromagnetic compatibility (emission rules).

3The QUANTAX EDS System
3.1 Hardware System Components................................................................................. 15
3.2 ESPRIT 2 Software..................................................................................................... 18
3.3 General Operating Instructions .................................................................................. 19

User Manual 3 The QUANTAX EDS System
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3.1 Hardware System Components QUANTAX EDS
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3.1 Hardware System Components
Typical QUANTAX
EDS system parts
XFlash®energy dispersive X-ray
detector (s)
Signal processing unit
Interface and EM control
QUANTAX server computer
Optional client workstations
ESPRIT 2 software package
System components of QUANTAX comprise the X-
ray detector, interface hardware, one or more
computers, and several software modules. All parts
are selected for performance and trouble free
interaction. Exchanging any part of the QUANTAX
system with non-approved items (e.g. user
defined
computers) may impair the functionality.
3.1.1
XFlash®Energy
Dispersive
X-ray Detectors
Fig. 3.1-1 Bruker XFlash
®
detector
Single photon counting. Energy dispersive X-
ray
spectrometers take advantage of the pho
ton nature
of light. In the X-
ray range the energy of a single
photon is just sufficient to produce a measurable
voltage pulse at the output of an ultra-
low noise
preamplifier connected to the semiconductor
detector crystal. The individual pulse heights ar
e a
statistical measure of the corresponding quantum
energy. By digitally recording and counting a great
number of such pulses within a so-called multi-
channel analyzer (MCA), a complete image of the X-
ray spectrum is built up almost simultaneously. This
digital quantum counting technique makes the
energy dispersive spectrometry extremely reliable.
Bruker XFlash

Detector. The Bruker XFlash®
detector is an energy dispersive X-
ray detector that
works according to the principle of the silicon drift
detector (SDD).
It uses a special arrangement of drift
electrodes and active components on the detector
crystal chip to raise the signal strength to a level that
can be measured even at room temperature.
XFlash® detectors are maintenance-
free, durable,
lightweight, completely vibration free, and do no
t
require any consumables.
3.1.2
Signal Processing
Unit
The signal processing unit is the heart
of the
spectrometer electronics. Different auxiliary utilities,
like signal inspectors and count rate meters are
incorporated in the signal processing
unit, as well as
all the necessary supply and operational circuits. The
data interface connects the spec
trometer and the
QUANTAX server.

User Manual 3 The QUANTAX EDS System
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Fig. 3.1-2 Signal processing unit SVE 6
Spectrometry signal processing. Inevitable
electronic noise requires the detector signal to be
averaged over a certain time for the purpose of pulse
height analysis. This averaging or noise filtering is
performed by the so-
called signal shaper. The
necessary time per pulse (filter
time) limits the
maximum acquisition speed of a spectrometer. The
applicable filter
times are determined by the
properties of the detector noise and the required
energy resolution (peak separation).
Pulse throughput.
With optimum signal shaper the
QUANTAX the XFlash®can output 20 000 to 130
000
cps, depending on the type of detector used
(refer to
the detector’s hardware manual for specifications)
.
Faster than o
ptimum shapers can be selected at the
expense of energy resolution, which is acceptable for
ultrahigh-speed applications like element mapping.
The QUANTAX spectrometer electronics is
configured according to the chosen detector and
QUANTAX system level.
3.1.3
Spectrometry Data
Interface and EM
Control
Data interface.
The proprietary Bruker MegaLink
high-
speed data interface transfers the spectrometer
data in real time to the QUANTAX server. The PCI
plug-in board Bruker IO-
Scan can connect up to 4
spectrometers simul
taneously. Bruker MegaLink is a
serial interface protocol featuring full galvanic
isolation for improved noise immunity at connection
length of up to 30 m. For basic spectrometer
functions that do not require real time spectrometry
a standard computer
interface (RS232) can be used
as an alternative.

3.1 Hardware System Components QUANTAX EDS
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Fig.
3.1-3 PCI-plug in IO-Scan
QUANTAX scan system. The PCI plug-in board IO-
Scan also contains the necessary hardware for
controlling the x/y electron beam deflection as well
as two separate digitizers for the image signals of
the electron microscope (EM).
Position tagged
spectrometry data acquisition is provided for
advanced line scan and element mapping. Digital
signal processing supports the server computer in
time critical tasks. Control signals for hardware scan
switching are provided as well.
Switch Box. The opti
onal switch box allows sharing
the external scan interface of the EM between
QUANTAX and third party applications. The switching
is fully automatic.
Microscope data transfer. Microscope dat
a transfer
is based on different networking technologies
according to the type of microscope. For older
brands, serial connections (RS232) are also provided.
3.1.4
Computer
Workstations
Client-server architecture. All QUANTAX
systems
feature client-
server architecture. The server part
controls the spectrometer and microscope hardware
and performs basic data evaluation; the client system
is what is visible
to the user and provides the
graphical user interface (GUI). Client and s
erver can
share one computer or run on different computers.
Multiple client workstations can connect to a
QUANTAX server with network access (LAN).

In some cases client and/or
server application may share
computers with the SEM installation.
Server workstation.
Based on the operating
Windows®
system, the QUANTAX server can be
used as standalone unit or network component. The
connections to the optional client workstations are
accomplished either
via a separate network or via the
intranet of the company or lab. With appropriate
upgrades it is also possible to connect to wide area
networks. The QUANTAX server performs the
measurements and primary spectrum mathematics.
It also provides the public and
private data areas of
the QUANTAX user.

User Manual 3 The QUANTAX EDS System
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3.2 ESPRIT 2
Software
System requirements.
QUANTAX requires
Windows®7
with a service pack level specified at
time of installation. Operating system updates are to
be approved by Bruker Nano. Only
computers
provided or approved by Bruker Nano may be used.
Windows®
administrator rights are required for the
installation of QUANTAX.
Ask your system
administrator for help.
Hardware driver. During the
first startup of the
server PC the driver for the IO-Scan plug-in must
be
installed. The driver is available from the ESPRIT
installation CD, which should always be at hand.

Do not save the license with a
pdf-reader. This procedure destroys
the license.
License file.
A user and system specific license file
is contained on a separate CD. During the ini
tial start
of ESPRIT the user is prompted to provide this CD
for registration.
The license file (Licence.pdf) is stored to the server
computer; after completion the license CD should be
kept in a safe location.
Software options.
Licenses control general access
to the ESPRIT software as well as installed
options.
Selected options or the complete license can be
time-
limited. Updated license files obtained from
Bruker Nano can be read in the System
workspace
(see section 4.7)
. Changes will be enabled after
restarting ESPRIT.
The
license is also provided as hard copy. The
contents can be checked against the file, which can
be opened by any pdf-reader or from the System
/
System workspace by clicking the button.
Hardware key. The system license is bound to a
system specific hardware key coded into the
QUANTAX server hardware. Client workstations can
receive certification from a licensed server via the
network. Standalone PCs (data stations) must be
equipped with an optional USB
dongle replacing the
hardware coded key.

3.3 General Operating Instructions QUANTAX EDS
19
USB Dongle.
The QUANTAX dongle for standalone
systems (systems without access to a QUANTAX
server) fits any USB-
port on the regarding PC. A
software driver for the dongle must be
installed
during system installation; the dong
le must be
present to use the data station.
Install the QUANTAX base system selecting option
Data Station (with dongle)
. Leave the ESPRIT
install CD in the drive and plug in the dongle into a
convenient USB-port. For details
refer to the
separate ESPRIT Installation Manual.
Windows®
will detect the new hardware
automatically and display an installation wizard.
Select the options shown in the images below and
finish the installation. Note that the dongle does not
replace but only enables a valid QUANTAX license.
3.3 General Operating Instructions
3.3.1
Detector Maintenance
The detector is the most sensitive part of the
spectrometer. According to the type of detector at
hand, different operations regulations apply. These
must be followed strictly.

After complete shutdown of the
XFlash®detector, an extended
warmup period and/or energy channel
recalibration (see section 5.2) may be
necessary for high precision
measurements.
XFlash® detectors. Bruker XFlash®
detectors are
maintenance-free. There is no
additional wearout
caused
by permanently powering the detector;
nonetheless detectors for light element analysis may
exhibit slight parameter changes after very long
periods (several weeks) of continuous operation.

For windowless detectors the
standby mode must be enabled
before the microscope chamber is
vented to avoid contamination on the
detector crystal.
Standby. Standby mode for the thermo
electrically
cooled detecto
r can be chosen between work
sessions to prevent unnecessary heating of the
detector housing. From the standby mode, the
detector can be quickly put back into a stable
measuring mode. Standby mode can be entered via
the Detector configuration dialog (see section 4.5.5
)
or by confirming the corresponding option when
terminating a work session.

User Manual 3 The QUANTAX EDS System
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Cooling mode. A mode selecti
on for the detector
cooling is provided for XFlash®detectors. Maximum
cooling will provide the optimum energy resolution.
Thermostat mode
will reduce possible changes due
to varying environment temperature. Though these
changes are normally negligible, thermostat mode
is
the proposed setting with most QUANTAX
applications. Please check the XFlash®
Reference
manual
to decide which of the above options is the
most suitable for your purpose.

A broken detector window
caused by any user interaction
impairs warranty and can result in a
total damage of the X-ray detector.
Additionally, a broken beryllium
window represents a substantial
health risk.
Detector window. The X-ray detectors
are
e
quipped with a beryllium window (detection range
starting from sodium) or a light element window.
Both kinds of windows are extremely thin, fragile,
and contact sensitive. In general, cleaning of the
windows is neither necessary nor permissible. If
the
detector window is contaminated
, contact customer
support or your local supplier for assistance.
3.3.2
Electronic Units
Setup. Unauthorized changes
to the electronic and
electric installation are not permitted. Besides sa
fety
regulations (see section 3.1.2)
also electromagnetic
immunity and noise pick up issues a
re addressed
during installation.
Note that electronic parts may have to be adapted to
the local mains voltages, if this should chan
ge for
whatsoever reason. Also replacement parts have to
be checked for proper settings before being
connected to the mains supply. Details are described
in the according reference manual.

The spectrometers are highly
sensitive measurement devices,
which can be impaired or destroyed
by inappropriate use.
Electrostatic damage.
All electronic components
and computers require the typical operating
precautions for electronic products. Especially, all
usual preventative measure
s against electrostatic
discharge
(ESD) must be carried out. All components
of the QUANTAX system are designed for laboratory
use only.
Cleaning.
Covers of electronic compartments must
never be opened. Only dry cleaning (dusting) of the
outer compartmen
ts is permissible. The detector
window must not be cleaned at all.