MICRO-XRF ON SEM

QUANTAX Micro-XRF
Trace element sensitivity with minimal sample preparation

Innovation with Integrity

Micro-X-ray Fluorescence Analysis
Micro-XRF on SEM, also known as SEM-XRF, empowers the scanning electron microscope
with a range of new analytical capabilities, using the same EDS detector already installed on
the SEM. ​Micro-XRF offers several novel analytical possibilities for elemental analysis in a
SEM, including:

ƒ Non-destructive analysis of valuable, del- ƒ Trace element sensitivity down to con-

icate or irreplaceable samples. In addition, centrations of 10 ppm or less (matrix and
the photon X-ray source does not heat the element dependent).
sample, nor generate any electrical charging
that may impact the analytical quality. ƒ Large area elemental distribution maps
over the centimeter scale whilst measuring
ƒ High spatial resolution analysis at the at the micrometer level is possible in com-
micrometer scale, allowing for the detailed bination with the optional Rapid Stage.
analysis of small or large areas or features
within a sample, even with complex or ƒ Detection of high energy X-ray lines up
heterogeneous elemental distributions, to 40 keV with the 50 kV excitation source,
thanks to the precise spatial localization of allowing for the evaluation of elemental
elements of interest. X-ray lines not normally considered when
using a SEM.
ƒ Detection of a wide range of elements
from carbon (Z = 6) to uranium (Z = 92), ƒ Determination of the thickness of multi-
thus making it applicable to a wide variety layered structures is possible due to the
of samples and applications. greater information depth of X-ray exci-
tation.
ƒ Minimal sample preparation required,
i.e., no coating or polishing, thus saving ƒ Micro-XRF on SEM is a versatile analyti-
time and effort. This allows for rapid cal technique that can be used in a wide
analysis, making it efficient for high- variety of application fields, such as geol-
throughput or routine sample analysis. ogy, archaeology, environmental science,
materials science, forensics, pharmaceuti-
ƒ Fast analysis times, typically from a few cals, and more. The data collected can be
minutes to several hours, depending on qualitative or quantitative from point, line,
the sample and analysis requirements. or map (distribution) analysis.
Micro-XRF on SEM is suitable for time-sen-
sitive applications, or the quick screening of
samples or the analysis of larger samples.

ƒ Accurate and precise quantitative

analysis of the elemental composition of
a sample, which can be standardless or
standard-based.
Full Range EDS Elemental Analysis – Figure 1
Expand Your SEM Capabilities Schematic of a dual photon
beam and electron beam
Micro-XRF on SEM converts the standard source setup with a single
SEM to a dual-beam source system (e-beam EDS detector. The optional
+ photon beam) that can be operated either Rapid Stage sits on top of
independently or simultaneously to benefit from the normal SEM stage to
the advantages of both excitation methods. enhance data acquisition
whilst mapping.
Using photon excitation on a specimen results
in a similar interaction as that seen via elec-
tron excitation, causing the specimen to emit
characteristic X-ray fluorescence radiation.
This X-ray information is captured by a stand-
ard energy dispersive spectrometer (EDS)
and can be utilized and processed as normal.
Qualitative and quantitative data on a sam-
ple’s elemental composition, including major,
minor and trace elements, can be collected
with high sensitivity and spatial resolution at
the micrometer scale.

Micro-XRF analysis does not require any The SEM, as the primary imaging instru-
sample preparation, specifically that may ment, provides high-resolution images of the
alter the sample or even destroys it, making it sample surface. In addition to EDS analysis,
suitable for the analysis of valuable or delicate the fully integrated XTrace 2 micro X-ray
samples in various applications. source enables X-ray fluorescence analysis of
the same sample without sample transfer or Figure 2
Photons (X-rays) generated by a microfocus additional sample preparation. Analysis of Rare Earth
X-ray tube are focused via a polycapillary Elements in a high index
X-ray optic onto the sample surface. The optic Utilizing a micro-XRF on a SEM will maximize glass. Major elements such
spot size can range from 10 µm to 35 µm. the full range of an EDS detector’s analytical as La, Ti, Nb, Gd, Zr, Si,
Upon installation, this focused X-ray beam is possibilities, including spectral information up and Zn as well as the minor
aligned with the electron beam at a nominal to 40 keV as well as major, minor and trace element Y were detected
SEM working distance (WD) maximized for element concentrations and their distribution in the energy range from
EDS analysis. This allows the user to seam- within the sample. 0 to 20 keV.
lessly switch between the two excitation
sources to take advantage of both, or to use
them simultaneously to qualitatively examine Y
trace and light elements at the same time.

Ti La Gd
XTrace 2 - Innovative X-ray source for micro-XRF analysis Increased performance and usability
on SEM
ƒ High tube power generates X-rays at high
XTrace 2 is the second-generation X-ray source for the QUANTAX energies of 50 kV and beam currents of
micro-XRF system. It enables fast micro-XRF spectral acquisition with 1000 µA for a high-count rate allowing
high-resolution data. Advanced features, such as the FlexiSpot mode, accurate elemental data to be collected
the Aperture Management System, and the motorized wheel for the quickly and efficiently.
selection of various filters facilitate the collection of robust data from ƒ Automatically switch between six primary
even the most challenging samples. filters for enhanced background reduction
and precise acquisition of low-count peaks.
ƒ Scan topographic samples with high resolu-
tion XRF signal intensity using an Aperture
Management System (AMS) that keeps the
image in focus across variable focal depths.
ƒ Analyze inhomogeneous and/or irregular
shaped samples using the FlexiSpot mode,
allowing spectral measurements using a
small or a large spot size.
ƒ Extended X-ray tube lifetime with the auto-
matic tube warm-up procedure.
ƒ Optimized safety and user functionality
with the motorized linear stage incorporat-
ing automatic source retraction, including
measure, park, and user specified positions
ƒ Software capability for saving and cor-
relating photon beam and e-beam mea-
surements (control the analysis, select
filters, and move the linear stage using the
XTrace 2 is designed for use with the Bruker XFlash® EDS detector intuitive ESPRIT software).
series for optimum qualitative and quantitative data analysis and hence
requires no additional X-ray detector. It can be adapted to a variety of
inclined SEM ports. Aperture Management System (AMS)
The optional Rapid Stage, which can be temporarily mounted on the
SEM stage, enables fast elemental X-ray mapping over large areas. XTrace 2 is equipped with a patented Aper-
This analytical setup allows the investigation of very large specimens ture Management System (AMS) to retain
up to 50 mm on a micrometer scale even in a SEM. measurement resolution over a certain depth
range, allowing the examination and visualiza-
Full integration into the ESPRIT software makes QUANTAX micro- tion of topographical samples.
XRF an intuitive system for comprehensive SEM EDS and micro-XRF
analysis.

AMS
The AMS feature allows
scanning of samples with
topography in the SEM
by increasing the focal
depth. The surface of
this pyrite crystal shows
a total intensity X-ray
map collected without
AMS (left) and with AMS
(500 µm, right). Mapping
with AMS can even resolve
the sample structures at a
depth of 2.1 mm.
Any analysis that deviates from the micro- Motorized wheel with six primary
XRF focal plane (nominal working distance) filters and two AMS apertures
will result in a larger spot size. The AMS
keeps the optic in focus at varying working The new XTrace 2 has space for nine different
distances by increasing the depth of field. options within the wheel, located between
This means that any reduction in resolution the X-ray tube and polycapillary optic, allow-
due to deviations in the working distance is ing further background reduction for each
minimized, facilitating the high-resolution individual X-ray energy region.
elemental mapping of topographical samples
and their 3D features. Motorized wheel
Position 0 is left blank for
normal unfiltered X-ray
FlexiSpot mode analysis. Positions 1 to 6
are reserved for several
FlexiSpot allows measurements at different primary filters, whilst-
spot sizes, ranging from 35 µm (standard positions 7 and 8 are for
optic spot size) to 500 µm and even beyond. AMS apertures. Switching
Large spot sizes are used for overall analysis, between positions is auto-
while small spot sizes are used for the ana- matic via software control.
lysis of specific features. Measuring at larger SEM safety features
spot sizes allows more accurate quantifica-
tion of inhomogeneous and irregular shaped ƒ Auto source insertion and retraction
samples as well as samples with uneven mode. The polycapillary optic of the X-ray
surfaces. A large spot area provides a more source can be automatically inserted and
representative excitation of the whole sample retracted using XTrace 2’s motorized linear
composition in just one measurement. stage. The source can also be retracted
when the SEM sample chamber is vented
FlexiSpot works by retracting the X-ray for sample change.
source, allowing the X-ray optic to be defo- ƒ SEM air-lock integration. The status
cused out of the nominal focal plane. Each information of the SEM air-lock chamber
individual spot size is selected in the ESPRIT (open/closed) can be integrated into the Auto source insertion and
software via an automated process. Multiple XTrace 2’s security circuit for optimal X-ray retraction
individual spot sizes can also be defined. safety purposes. This feature is designed Top: X-ray optic in meas-
for the integration of various SEM air-lock urement position, bottom:
chambers (from different SEM vendors). X-ray optic in parking
position.

FlexiSpot
The ability to change the spot size from the X-ray optic
spot (10 µm or 35 µm) and larger spot sizes is important
for selecting the most appropriate analytical volume for
sample representativity.
Applications
Micro-XRF on SEM has a wide range of applications across various fields.

Materials science Archaeology and art conservation

The elemental composition and distribution in Cultural heritage objects, such as paintings,
a wide range of materials, including metals, sculptures, ceramics and metal artifacts, can
alloys, polymers, ceramics, composites, be studied using micro-XRF on SEM. It pro-
coatings, and thin films can be determined vides valuable information about the elemen-
using micro-XRF on SEM. It is used for quality tal composition of pigments, dyes, glazes,
control, failure analysis, characterization of and corrosion products, which can help in
surface treatments, and investigation of ele- identifying materials, studying artistic tech-
mental segregation and diffusion in materials. niques, and assessing degradation processes.

Analysis of Rare Earth Elements (REEs) Analysis of coins

Rare earth elements have a range of X-ray Micro-XRF obtains surface information but Elemental distribution
energies, typically the L series are commonly also to detect sample information from analysis of coins
used in standard EDS for identifying those underneath the sample surface which makes Analysis of a Roman coin
REE´s which often overlap with the base it possible to investigate also historic coins highlighting the effects of
metals (e.g., Cr, Mn, etc.). Micro-XRF is capa- to determine their origin or to understand the burial and oxidation on the
ble not only to detect the L series, but also aging process and avoid areas where surface surface of the coin that will
the higher energy K lines (e.g., Ce at 34.7 keV) ageing has occurred. impact any quantification
that have no peak overlaps, which makes the of the alloy composition.
user confident of element identification and
thus support the deconvolution process of
the lower energy lines.

Environmental science

The analysis of soil, sediment, water, and plant

Smithsonian REE phosphate samples is possible using micro-XRF on SEM.
standards It can determine the presence and distribution
All rare earth elements can be of trace elements, heavy metals, and contami-
clearly identified in a single nants in environmental samples, aiding in envi-
map using SEM-XRF analysis ronmental monitoring, pollution assessment,
with automated deconvolution. and remediation studies.
Pharmaceuticals and cosmetics Forensics
industries
Forensic science benefits from micro-XRF on
The application of micro-XRF in SEM in the SEM over a wide range of applications includ-
pharmaceutical and cosmetics industries ing the analysis of trace evidence, gun shot
includes the analysis of raw materials, pack- residues, paint chips and fibers. It can provide
aging materials and the quality assurance of information about the elemental composition
finished products. It can determine the ele- of these samples, aiding in forensic investiga-
mental composition of drugs, cosmetics, and tions and criminalistics.
packaging materials, aiding in quality control,
compliance with regulations, and product
development. Electronics and semiconductor
industries

Geology and mineralogy Micro-XRF on SEM is a valuable tool in the

electronics and semiconductor industries for
The elemental composition of rocks, minerals, the analysis of electronic components, circuit
ores, and soils can be determined and ana- boards, and semiconductor materials. It can
lyzed using micro-XRF on SEM. It can provide determine the elemental composition of solder
information about mineralogical composition, joints, coatings, and contaminants, aiding in
elemental zoning, and trace element distribu- quality control, failure analysis, and process
tion, which can be useful for mineral explo- optimization.
ration, resource assessment, and geological
research. Fast elemental mapping with AMS over
large area of electronics components on a
Analysis of exploration mineral grains Printed Circuit Board (PCB)
The composition of mineral grains can be High-speed micro-XRF on SEM can be used
easily determined with micro-XRF without for the elemental analysis of electronic com-
any sample preparation. These grain frag- ponents, such as this PCB, at trace element
ments were simply mounted on a carbon sensitivity without any sample preparation
stub without any carbon coating and quickly required. In addition, the new AMS keeps
scanned to identify what these minerals the various PCB components in focus, thus
are, in this case eclogitic garnet and clinopy- making it easy to interpret the results, even
roxenes from South Africa. though the sample has a high topography.

Analysis of a PCB board

Element distribution map All the relevant compo-
of various mineral grains nents of a PCB board
SEM-XRF analysis of un- can be clearly identified
polished garnet and clino- via SEM-XRF analysis,
pyroxene grains confirming despite the sample being
that they are derived from three-dimensional. Image
a mantle eclogite, possibly depth-of-field is main-
associated with diamonds. tained thanks to the unique
Aperture Management
System (AMS).
 Technical Data

Sample types Solids and particles

Excitation High brilliance, air cooled micro spot X-ray tube with polycapillary
X-ray optics, Be side window
- target material Rh, optional Ag on request
- tube parameters max. 50 kV, 1000 μA (50 W)
- standard spot size < 35 μm for Mo Ka (17.5 keV)
- primary filters software-controlled motorized wheel with six primary
X-ray beam filters

Detection XFlash® silicon drift detector*

Instrument control No additional PC required, QUANTAX EDS PC can

be used (recommended)*, instrument control unit
connected via Ethernet

Instrument software Bruker ESPRIT software,

optional XMethod software package for thin film thickness analysis (layered samples)

Order No. DOC-B82-EXS010 Rev. 2. ©2023 Bruker Nano GmbH, Am Studio 2D, 12489 Berlin, Germany.
Instrument control functions Complete control of tube parameters and filters

Spectra evaluation XRF peak identification, artifact and background correction, peak area calculation, standardless
quantification, combined XRF and EDS quantification, thin film thickness analysis

Distribution analysis HyperMap capability (hyperspectral database)

All configurations and specifications are subject to change without notice.

Result presentation Quantification results, statistical evaluation, element distribution (line scan, mapping)

Power supply 100 - 240 VAC (1P), 50/60 Hz

Dimension and weight XTrace 2 X-ray source: 428 mm x 297 mm x 179 mm, 14 kg
XTrace 2 electronics: 489 mm x 500 mm x 196 mm, 15 kg

Quality and safety XTrace 2 complies with the following safety regulation standards:
- IEC 61010-1 (3.1) Europe, U.S., Canada
- IEC 61010-1 (3.0) Japan
- IEC 61010-1 (2.0) Australia, Korea

*XTrace 2 requires a pre-installed QUANTAX energy-dispersive X-ray spectrometer (EDS), consisting of XFlash® silicon
drift detector, SVE signal processing unit and system PC.

Bruker Nano Analytics

Headquarters Berlin · Germany
info.bna@bruker.com

www.bruker.com/quantax-micro-xrf