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Micro X-ray Fluorescence for Thin-film Thickness & Composition

ATLAS SEMI microEDXRF Metrology Tool

IXRF Systems’ ATLAS SEMI is the very latest micro spot energy dispersive X-ray fluorescence (micro XRF) imaging spectrometer for semiconductor metrology. Designed to image and analyze (edge-to-edge) wafers up to 300 mm diameter, ATLAS leads the industry in virtually every major specification category from the largest chamber and the highest detector active area, to the longest mapping travel and smallest X-ray micro-spot.

Hardware specifications are only half of the ATLAS Advantage™. ATLAS’ Iridium Ultra software platform, developed with SEM-EDS elemental mapping and analytical functionality, is unsurpassed in it’s ability to provide elemental and phase mapping, line scans, critical dimensions (CD) as well as qualitative and quantitative elemental analyses of multi-layer thin film stacks. The functional, flexible, and feature-rich software suite guarantees unprecedented productivity. ATLAS SEMI is the micro XRF metrology tool that leads with innovation.

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Micro X-ray fluorescence (µXRF, µEDXRF, micro-XRF, microEDXRF) spectroscopy is an elemental analysis technique that relies on the same principles as X-ray fluorescence (XRF) spectrometry. The difference is that micro x-ray fluorescence (microEDXRF) spectrometry has a spatial resolution with a diameter many orders of magnitude smaller than conventional XRF, WDXRF or EDXRF spectrometers. Practically, microEDXRF spectrometers with high-precision scanning XYZ-stages — like the ATLAS series — function as a type of XRF hyperspectral imaging microscope, where each pixel (in a map or image) contains information from 4 – 40 keV in the electromagnetic spectrum.

Modern polycapillary focusing X-ray optics are able to create small focal spots of just a few micrometers in diameter. By using such X-ray optics, the IXRF Systems’ ATLAS series of imaging spectrometers provide a tiny focal spot (down to 5 μm, depending on desired configuration) that is much more intense and allows for enhanced trace element analysis and the creation of hyperspectral images of a sample. Micro X-ray fluorescence (μEDXRF) spectometry is commonly employed in many applications, such as: botany, cement, forensics, small feature evaluations, elemental mapping, mineralogy, metals & alloys, electronics, multi-layered coating analysis, micro-contamination detection, film and plating thickness, biology and environment.*

Biggest chamber

ATLAS SEMI micro-XRF imaging spectrometer features the industry’s most voluminous sample chamber, allowing for automation of more samples, larger area mapping capabilities, and wider variability of sample types that can be analyzed. Sample chamber size: 940 x 660 x 355 mm (37 x 26 x 14 inches).

The 5 micron advantage

ATLAS SEMI micro-XRF mapping spectrometer is the FAB-LAB tool of choice for sample characterization using micro-X-ray spot energy dispersive X-ray fluorescence (microEDXRF) spectrometry for metrology information on composition (phase) and elemental distribution of multi-layer thin film stacks. With the smallest X-ray spot in the industry at 5 microns, ATLAS SEMI is optimized for analysis speed without compromising accuracy. The instrument can measure a wide range of sample types, whether small or large, even or irregularly shaped. Equipped with a large high-speed stage, it supports 2D analysis of virtually any kind of sample: small to 12 inch wafers, lead frames, circuit boards, bump bond pads, magnetic media, sputtering targets, etc. Its extra large vacuum chamber delivers superior light element (low-Z) sensitivity.

When it comes to micro-X-ray microscopic imaging (mapping), smaller is always better. Above is a TEM grid. The image on the left was captured using the ATLAS SEMI's 5 micron X-ray spot. The inferior image on the right was taken with a 10 micron X-ray spot.

ATLAS X w/ 5 µm round spot

Conventional w/ 25 µm oval spot

Superior geometry

Perpendicular ATLAS SEMI geometry allows for circular X-ray excitation down to 5 microns for highest spatial resolution.
Smallest spot means it is easier to find a flat aspect of a feature to measure.
Competitor’s inferior angled geometry only allows smallest spot to be 25 microns due to the ellipse.

Unmatched speed

Mix and match up to 4 Silicon Drift Detectors (SDD)
- For the largest possible solid angle collection efficiency
Up to 600 mm² active area
- Available resolutions: ≤130-145 eV resolution
Highest count rate with the smallest spot for fast high-res images

Overview automation

Overview video camera mode:

Automated spectral spot analysis
Automated X-Ray mapping
Automated linescans
Large chamber view for large samples

Spot automation

Video microscope mode:

10 -200X magnification with auto zoom
Auto spectral spot analysis
Automated X-ray mapping
Automated linescans

Intuitive software

Beginner users will find the software simple to navigate in a comprehensive manner. As they advance, more powerful tools are easily accessible with no additional cost. They are all included and not added on as options:

Custom report generation
Phase analysis
Particle analysis
Morphology
And ASTM testing methods

Sample types and conditions

Air, vacuum or helium atmosphere
Vacuum ready in under one minute
Measure: patterned wafers (multi-layer thin films), circuit boards, lead frames, bond pads, magnetic media, sputtering targets … and we can measure liquids, particles and powders too.

Micro X-ray excitation

50 kV / 50 W / 1 mA Rh target (others available) X-ray tube
Polycapillary focusing optic
Filter wheel with up to 7 filters (plus open position) before the focusing optic
Available primary X-ray spot sizes: 5 , 10, 20 or 40 μm
Optional second X-ray tube, with a choice of anodes, is available with spot sizes of 200, 500 or 1000 μm

X-ray detection

Mix and match up to 4 Silicon Drift Detectors (SDD)
- For increased precision and/or reduced acquisition times
50 mm² to 150 mm² active area
- Highest resolution to highest counting rate
Available resolutions: ≤130-145 eV resolution
Peltier cooling

Largest precision stage

Motorized XY, Z optional
- Mapping travel: 400(X) x 300(Y) mm
Speeds up to 300mm/s
- Map acquisitions at ≤ 1ms/pixel
Accuracy < 1µm
Custom adapters available

Chamber and geometry

Chamber size: 950 x 650 x 365 mm (37 x 26 x 14 inches)
Top-down perpendicular geometry from tube to sample
Mapping area: 400 x 300 mm under automatic control
Sample view: 3 sample positioning and analysis cameras
- Samples may be positioned manually with the door open

Iridium Ultra^™ for Windows^® 10

Energy dispersive X-ray fluorescence (micro-XRF) spectroscopic software
- Fundamental Parameters (FP) for solids, liquids, powders and particles
- Thin film FP for up to 8 layers including an infinite base or substrate
- Automatic treatment for sum/escape peaks and full deconvolution
- Up to 8 acquisition conditions per analysis
Hyperspectral EDXRF mapping and imaging, up to 4096 x 4096 pixels
- Every pixel is a full EDXRF spectrum
- Principal component analysis (PCA) for phase mapping
Materials classification database

Acquisition and quantitation

One-click acquisition and automatic peak identification
Customizable identification, labeling, processing, and quantification
Scrolling periodic chart
Drag and drop overlay
Automatic overlap correction, sum/escape peak removal, background correction, and linear/non-linear deconvolution
Fundamental Parameters (FP) and Quantitative Match
Material classification database

Imaging and analysis

Multi-Point automated analysis directly from image
Morphological processing for rapid feature size measurements
Image stitching and montage
Segmentation and feature segregation
Particle analysis package
- Including border removal, sorting and exclusion
- Classification by composition

Mapping and linescans

Simultaneous acquisition of 35 elements
Stored spectral data for every pixel
Live spectrum display during acquisition
Single or multiple map acquisition from image
- Overview or spot camera
Map stitching and montage
Extract spectra from map: point, area, freehand
Create linescan from map
Mouse-over view intensities and concentrations
Phase Analysis
Multi-compositional map display
- Of element and compound ranges
Overlay linescans on image

Specialty and automation

Multilayer thin film and coatings analysis up to 8 layers
Serpentine continuous mapping (dual directional mapping)
ASTM E2926-13 Glass Analysis
Track, store, and recall all stage locations and images

Imaging / mapping flow

Create multiple X-ray maps on any region on the sample
Define map parameters directly from video image
Combine pixels to create analysis regions
- Regions are summed to create a composite spectrum
Automatically identify elemental peaks
Apply analytical quantification method
Analytical results are displayed as a graphic

Top menu navigation

Beginner users find the software simple to navigate
Advanced users find that powerful tools are easily accessible
All software features are included standard
Upgrades are free for life, so you are always up to date
Custom report generation for completeness
Exhaustive toolset comes from scanning electron microscopy

Spectral display features

One click operation for acquisition, automatic peak identification, and quantification
Collection of x-ray spectra into 25 individual windows
Point and click cursor displays energy, counts, and possible elements present
Customizable automatic element identification and labeling of peaks
Scrolling markers from element chart on spectra
Complete annotation tools for spectra; customize text, lines, and more

Alignment laser / operation

Comprehensive software design
Laser alignment focusing
- As shown in the video image
Large high magnification video viewing
Easy to operate joystick
Sub-micron X-Y-Z stage
Alignment laser visible on concrete sample

Automatic phase analysis

Phase analysis by Principle Component Analysis (PCA)
PCA is used in exploratory data analysis, an approach to analyzing data sets to summarize their main characteristics
PCA can be done on intensity or concentration based maps
Phases are defined and percent (%) of field of view of each phase is defined
In a PCA map, phases are marked by a defined color

Imaging composition

User defined compositions define the image
Maps can be defined by intensities or concentrations
Maps can be elements, compounds, components, materials, etc.
Example top series starts with a composite grey scale of a sample
- Key: red is high Si areas and purple is high Ge
Inset image show a more complicated composition analysis map

Click Image to Enlarge

Line profile analysis (linescan)

Relative elemental concentration or intensity along a line
Multiple charts display the “tiled” form of the data
- Relative change of each element is viewed separately
Linescans may also be displayed “stacked” for comparison
- Inset example shows an overlay of a long 300 mm linescan
Larger image is a 5 micron scan at ppm levels

Morphology

Surface morphology is a evaluation of the shape of a surface
Particles, features, inclusions are elementally identified
- And automatically counted/measured by feature type
Additional data on each feature may be easily collected
As shown, an extensive set of image features is available

ATLAS SEMI features

Largest sample chamber in the industry
Spot size down to 5 microns with anti-halo optic
SDD detectors w/ active area up to 150 mm²
Edge-to-edge mapping of 300 mm wafers
50 kV / 50 W polycapillary optic micro X-ray source
Multi-point/multi-area automation & mapping
Air, vacuum, helium for solids, liquids, and powders
Iridium Ultra software running on Windows™ 10 OS
Available clean-room ready stainless steel enclosure

Specifications

Elemental range:

Sodium (Na) through uranium (U)

Sample types:

Solids, liquids, particles, powders and thin films

Sample chamber size:

940 x 660 x 355 mm (37 x 26 x 14 inches)

Analysis atmosphere:

Air, vacuum or He_(g) purge

Primary X-ray source:

50 W max power, 50 kV @ 1 mA

Optional secondary X-ray source:

4-12 W max power, 40-60 kV @ 0.4-1 mA

X-ray source optics:

Polycapillary or aperture collimation

X-ray source anode:

Rhodium (others optionally available)

X-ray source spot size (primary):

5 μm standard (optional: 10, 20 or 40 μm)

X-ray source filters:

Up to 7 plus an open position

Primary X-ray source geometry:

Top-down beam (perpendicular to sample stage)

Detector(s):

2 standard, optionally up to a maximum of 4

Detector types:

Silicon drift detector (SDD) standard (PIN-diode is optionally available)

Detector active area:

50 to 150 mm², up to 600 mm² w/ 4 detectors

Sample stage type:

Motorized X,Y and Z (optional)

Sample stage travel:

600(W) x 300(D) x 210(H) mm

Mapping travel:

300(X) x 400(Y) mm

Mapping scan speed:

1-3 ms/pixel

Stage XY speed:

Up to 300 mm/s

Sample view:

3 cameras for sample positioning and analysis

Operating system:

SFF PC w/ Microsoft® Windows™ 10 OS

Analysis and control software:

Iridium Ultra: provides complete control of parameters, filters, cameras, optical microscopes, sample illumination and positioning, and measurement media

Quality and safety:

CE marked, RoHS, radiation < 0.5 μSv/h

Dimensions:

1690(L) x 787(W) x 1630(H) mm (67 x 31 x 64 inches)

Power:

100-240 V, 1 phase, 50/60 Hz

Bump bond metrology

UBM/RDL: rapid thickness & composition monitoring non-destructively in seconds (i.e., no need to cross section)
Multi stack analysis in one shot
CuNiPd / CuNiAu / CuNiZn
Non-destructive high throughput, down to seconds per bump bond analysis
Direct multi-element detection by XRF spectroscopy
Robust FP software for thickness/composition determination

Circuit board inspection

Fast X-ray mapping for electronics’ inspections
A complete X-ray Spectrum for each pixel in the map
Measure thin gold and palladium coatings on PCBs
Measure coating thickness of Cu, Ni, etc.
Measure solder composition
RoHS / WEEE compliance

Lead frame imaging

Measurements on very small flat components and structures such as conducting paths, contacts or lead frames
Measurements of typical multi-coating systems on lead frames,e.g., AuAg/Pd/Ni/CuFe or Au/Pd/Ni/CuFe in the nanometer range
Determination of the phosphorous content in NiP coatings
Measurements of functional coatings in the electronics and semiconductor industries
Determination of complex multi-coating systems

Wafer metrology

Sn/Ag Bump/Pillar measurements
Light elements
Metal film stack composition such as CIGS
Cu CMP control at BEOL
Multi-stack structures
Sputtering targets
Thermal barrier coating
Thickness and composition control

Sputtering Targets

With mapping, micro-spot energy dispersive X-ray fluorescence (microEDXRF) spectroscopy, it is possible to rapidly scan sputtering targets for inclusions or other undersirable artifacts.
microEDXRF mapping of sputtering targets for inclusions and second phase materials can be used to create “exclusion areas” files.
Knowledge of exact locations of inclusions greatly improves wafer yields.

RoHS / WEEE

With stage mapping, large samples can be quickly mapped for identification of prohibited materials
It is not necessary y to know what elements are present before collecting a map
Elements can be added as the spectrum grows and peaks become evident
ATLAS X offers the largest sample chamber in the industry

CIGS solar cells

Analysis of thin film photovoltaic cells is commonly performed with Micro-XRF
With ATLAS, it is possible to measure structures under vacuum for superior results
For in-line control during the production process as well as for final testing
Quantification for layer thicknesses are in very good agreement with WDXRF results

Reference documents

- - “Company Index: A Guide to Companies.” Microscopy Today 21, no. S1 (March 2013): 50–55. https://doi.org/10.1017/S1551929513000357.
  - Do, Christina, Farida Abubakari, Amelia Corzo Remigio, Gillian K. Brown, Lachlan W. Casey, Valérie Burtet-Sarramegna, Vidiro Gei, Peter D. Erskine, and Antony van der Ent. “A Preliminary Survey of Nickel, Manganese and Zinc (Hyper)Accumulation in the Flora of Papua New Guinea from Herbarium X-Ray Fluorescence Scanning.” Chemoecology 30, no. 1 (February 1, 2020): 1–13. https://doi.org/10.1007/s00049-019-00293-1.
  - Ent, Antony van der, Peter M. Kopittke, David J. Paterson, Lachlan W. Casey, and Philip Nti Nkrumah. “Distribution of Aluminium in Hydrated Leaves of Tea ( Camellia Sinensis ) Using Synchrotron- and Laboratory-Based X-Ray Fluorescence Microscopy.” Metallomics 12, no. 7 (2020): 1062–69. https://doi.org/10.1039/C9MT00300B.
  - Harvey, Maggie-Anne, Erskine, Peter D., Harris, Hugh H., Brown, Gillian K., Pilon-Smits, Elizabeth A. H., Casey, Lachlan W., Echevarria, Guillaume and van der Ent, Antony (2020). Distribution and chemical form of selenium in Neptunia amplexicaulis from Central Queensland, Australia. Metallomics 12 (4) 514-527. https://doi.org/10.1039/c9mt00244h.
  - Van der Ent, Antony, Casey, Lachlan W., Blamey, F. Pax C. and Kopittke, Peter M. (2020). Time-resolved laboratory µ-XRF reveals silicon distribution in relation to manganese toxicity in soybean and sunflower. Annals of Botany. https://doi.org/10.1093/aob/mcaa081.
  - Huang, Xitong, Yong Li, Ke Chen, Haiyan Chen, Fei Wang, Xiaomin Han, Beihai Zhou, Huilun Chen, and Rongfang Yuan. “NOM Mitigates the Phytotoxicity of AgNPs by Regulating Rice Physiology, Root Cell Wall Components and Root Morphology.” Environmental Pollution 260 (May 2020): 113942. https://doi.org/10.1016/j.envpol.2020.113942.
  - Jones, Michael W. M., Peter M. Kopittke, Lachlan Casey, Juliane Reinhardt, F. Pax C. Blamey, and Antony van der Ent. “Assessing Radiation Dose Limits for X-Ray Fluorescence Microscopy Analysis of Plant Specimens.” Annals of Botany 125, no. 4 (March 29, 2020): 599–610. https://doi.org/10.1093/aob/mcz195.
  - Le Pape, Y. “Neutron-Irradiation-Induced Damage Assessment in Concrete Using Combined Phase Characterization and Nonlinear Fast Fourier Transform Simulation.” In Proceedings of the 10th International Conference on Fracture Mechanics of Concrete and Concrete Structures. IA-FraMCoS, 2019. https://doi.org/10.21012/FC10.232765.
  - Li, Y., Y. Le Pape, E. Tajuelo Rodriguez, C.E. Torrence, J.D. Arregui Mena, T.M. Rosseel, and M. Sircar. “Microstructural Characterization and Assessment of Mechanical Properties of Concrete Based on Combined Elemental Analysis Techniques and Fast-Fourier Transform-Based Simulations.” Construction and Building Materials 257 (October 2020): 119500. https://doi.org/10.1016/j.conbuildmat.2020.119500.
  - Pearson, Charlotte, Matthew Salzer, Lukas Wacker, Peter Brewer, Adam Sookdeo, and Peter Kuniholm. “Securing Timelines in the Ancient Mediterranean Using Multiproxy Annual Tree-Ring Data.” Proceedings of the National Academy of Sciences 117, no. 15 (April 14, 2020): 8410–15. https://doi.org/10.1073/pnas.1917445117.
  - Ye, Hui, Changzhi Wu, Matthew J. Brzozowski, Tao Yang, Xiangping Zha, Shugao Zhao, Bingfei Gao, and Weiqiang Li. “Calibrating Equilibrium Fe Isotope Fractionation Factors between Magnetite, Garnet, Amphibole, and Biotite.” Geochimica et Cosmochimica Acta 271 (February 2020): 78–95. https://doi.org/10.1016/j.gca.2019.12.014.
  - Zhang, Mingyuan, Jianxiang Wang, and Li-Hua Shao. “Ultrahigh Flexoelectricity of 3D Interconnected Porous PDMS.” ArXiv:2009.03847 [Physics], September 27, 2020. http://arxiv.org/abs/2009.03847.
  - Ziejewska, Celina, Joanna Marczyk, Aneta Szewczyk-Nykiel, Marek Nykiel, and Marek Hebda. “Influence of Size and Volume Share of WC Particles on the Properties of Sintered Metal Matrix Composites.” Advanced Powder Technology 30, no. 4 (April 1, 2019): 835–42. https://doi.org/10.1016/j.apt.2019.01.013.

Search terms

XRF
X-ray fluorescence
X-ray fluorescence spectroscopy
X-ray fluorescence spectrometry
energy dispersive X-ray fluorescence
energy dispersive X-ray fluorescence spectroscopy
energy dispersive X-ray fluorescence spectrometry
micro X-ray fluorescence
micro X-ray fluorescence spectroscopy
micro X-ray fluorescence spectrometry
micro energy dispersive X-ray fluorescence
micro energy dispersive X-ray fluorescence spectroscopy
micro energy dispersive X-ray fluorescence spectrometry
μXRF
mXRF
μEDXRF
mEDXRF
microXRF
microEDXRF
micro-XRF
m-XRF
micro-EDXRF
m-EDXRF
small spot XRF
small-spot XRF
small spot EDXRF
small-spot EDXRF
ASTM E-2926-13
XRF map
XRF mapping
XRF linescan

EDS & XRFfor Electron Microscopy

micro-XRF µXRF / µEDXRF

Training Courses / Education

Micro X-ray Fluorescence for Thin-film Thickness & Composition

ATLAS SEMI microEDXRF Metrology Tool

Biggest chamber

The 5 micron advantage

Superior geometry

Unmatched speed

Overview automation

Spot automation

Intuitive software

Sample types and conditions

Micro X-ray excitation

X-ray detection

Largest precision stage

Chamber and geometry

Iridium Ultra™ for Windows® 10

Acquisition and quantitation

Imaging and analysis

Mapping and linescans

Specialty and automation

Imaging / mapping flow

Top menu navigation

Spectral display features

Alignment laser / operation

Automatic phase analysis

Imaging composition

Line profile analysis (linescan)

Morphology

ATLAS SEMI features

Specifications

Specifications

Bump bond metrology

Circuit board inspection

Lead frame imaging

Wafer metrology

Sputtering Targets

RoHS / WEEE

CIGS solar cells

Reference documents

Search terms

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EDS & XRFfor Electron Microscopy

micro-XRF µXRF / µEDXRF

Training Courses / Education

EDS & XRF
for Electron Microscopy

micro-XRF
µXRF / µEDXRF

Training
Courses / Education

Iridium Ultra^™ for Windows^® 10

EDS & XRF
for Electron Microscopy

micro-XRF
µXRF / µEDXRF

Training
Courses / Education