Equipment
The X-ray center houses numerous instruments for material characterization by X-ray diffraction methods of a wide variety of samples. We also provide space and utensils to prepare samples yourself.
Below is an overview of some of the equipment at the X-ray Center as well as the sample preparation room.
Our devices:
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© Klaus Ranger
Characteristics
- Geometry: ¼ Euler cradle
- Anode: Cu and Mo microfocus X-ray sources
- Monochromatization: multilayer mirrors
- Beam sizes: ∅ 0.2 mm (Cu); 0.2 mm (Mo).
- Distance sample-detector (SD): 40-140 mm.
- Sample movement: ¼ Euler cradle
- Sample adjustment: video adjustment system
- Detector: Dectris Eiger CdTe 1M
Non-ambient
- Oxford Cryostream 800 (90 - 400 K)
- Stoe Heatstream (400 - 1000 K)
Applications
- Structure elucidation of weakly scattering crystals
- Structure elucidation of complex structures (modulated, twinned)
- Diffuse scattering
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© Klaus Ranger
Characteristics
- Geometry: Θ/Θ- diffractometer; parallel beam
- Anode: Cu microfocus X-ray source
- Monochromatization: Montel mirror
- Beam sizes: 2x2 mm², ∅1, 0.5, 0.3, 0.08 mm
- distance anode-sample (AS): 100 - 300 mm
- Distance sample-detector (SD): 100 - 300 mm
- Sample movement: ¼ Euler cradle; xyz stage (load capacity 2 kg).
- Sample adjustment: video adjustment system with laser
- Detector: Vantec 2000 (angular range 2θ= 32°, ψ= 63° with SD= 220 mm)
Non-ambient
- Load frame (planned)
Applications
- Qualitative/quantitative phase analyses (e.g. corrosion products, residual austenite analyses)
- Stress analysis (bulk and thin film samples)
- Texture analysis (bulk and thin film samples)
- Microdiffraction (up to beam sizes > 80 μm)
- "Reciprocal space mapping" thin films
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© Klaus Ranger
Characteristics
- Geometry: Θ/Θ - diffractometer; Bragg-Brentano
- Anode: Cu - X-ray source
- Monochromatization: a) Ni filter; b) secondary monochromator graphite
- Beam sizes: variable beam apertures (primary/secondary automatic)
- distance anode-sample (AS): 240 mm
- distance sample-detector (SD): 240 mm
- Sample movement: spinner without sample environment
- Sample changer for 15 samples
- Detector: a) X'Celerator semiconductor detector (2.1°); b) alternatively proportional counter (0D) with graphite monochromator
no option for non-ambient measurements
Applications
- Qualitative/quantitative phase analyses under ambient conditions (e.g. routine measurements for synthesis control)
- Reflectance measurements/transmittance measurements
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© Klaus Ranger
Characteristics
- Geometry: Θ/Θ- diffractometer; Bragg-Brentano
- Anode: Cu -X-ray source
- Monochromatization: a) Ni filter; b) secondary monochromator graphite
- Beam sizes: variable beam apertures (primary/secondary automatic)
- distance anode-sample (AS): 240 mm
- distance sample-detector (SD): 240 mm
- Sample movement: spinner without sample environment; fixed for sample environment
- Detector: a) X' Celerator semiconductor detector (2.1°); b) Scintillation detector (0D)
Non-ambient
- Closed-cycle cryostat (11K > T < 310 K)
- Anton Paar HTK 1200 N (T < 1200°C); air, nitrogen atmosphere
- Anton Paar XRK 900 reaction chamber (P < 10bar; T < 900°C); gas atmospheres (Ar, H2, CO, CO2, mixtures)
- Anton Paar TTK450 chamber (100K > T < 470K)
Applications
- Qualitative/quantitative phase analysis of crystalline fractions
- Amorphous phase fractions
- Crystallite sizes
- Residual austenite analysis
under non-ambient conditions:
- Reflection measurements/transmission measurements
- Capillary measurements
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© Klaus Ranger
Characteristics
- Geometry: Θ/Θ - diffractometer; Bragg-Brentano (focusing mirror; Cu(Kα1,2)), parallel beam geometry (mirror; Cu(Kα1,2)), channel-cut monochromator (CuKα1), GID; capillary/reflectance and transmission geometry
- Anode: Cu/Mo/Ag - X-ray source
- Monochromatization: a) filter (Cu, Mo, Ag); b) mirror (parallel geometry; focusing for Cu anode)
- Beam sizes: variable beam apertures (primary/secondary automatic)
- distance anode-sample (AS): 240 mm
- Distance sample-detector (SD): 240 mm
- Sample movement: spinner without sample environment; fixed for sample environment
- Tilting stage for stress and texture measurements
- Setup for GID measurements on thin films
- Reflectometer attachment
- Detector: a) PIXCel 3D semiconductor detector; b) scintillation detector (0D) for Ag radiation
Non-ambient
- Currently not foreseen
Applications
- Qualitative/quantitative phase analysis of crystalline components
- Amorphous phase fractions, crystallite sizes, etc.
- Stress/texture measurements
- Reflectometry measurements
- GID measurements on thin films
- Measurements for PD analysis
under ambient conditions:
- Capillary/reflection and transmission geometry
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© Klaus Ranger
Characteristics
- Geometry: 4-circle with kappa geometry
- Anode: Mo X-ray source
- Monochromatization: graphite
- beam size: variable collimators, 0.4-0.8 mm
- distance sample-detector (SD): 36-180 mm
- 2D CCD detector
Non-ambient
- Cooling up to 90 K and heating up to 450 K in dry nitrogen atmosphere
Applications
- Structure elucidation (organics, organometallics and inorganics).
- Determination of absolute configuration (elements ≥ S)
- Structure function relationships (e.g., nonlinear optical materials)
- Crystallographically challenging problems: stacking fault orders, twins, modulation
- Phase transitions (e.g., magnetic or ferroelectric transitions)
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© Klaus Ranger
Characteristics
X-ray tube SST-mAX
- Anode: Rh standard
Goniometer
- Type: θ/2θ decoupled with Direct Optical Position Sensing (DOPS)
- Angular accuracy: 0.0025° θ and 2θ
Optical path
- Primary collimators: 3 max.: 100, 150, 300, 550, 700 or 4000 μm
Primary beamfilters 4 max.: One may be used as beam stop
Crystals: 8 max.: LiF420, LiF220, LiF200, Ge111 (flat/curved), PE002 (flat/curved), InSb (flat/curved),TlAP coated, PX1, PX4, PX5, PX6, PX7, PX10 - Detectors: Flow, scintillation, sealed Xe in tandem with flow counter as duplex counter (optional), Hi-Per Scint (optional)
Counting electronics
- Type: Dual multi channel analyser with digital signal processor
Sample handling
- Types: Solid, fused beads, filters, pressed/loose powders and liquids
- Handling: All samples are fitted in sample holders during measurement. Liquids and loose powders in disposable (P2) liquid cells, which are fitted in liquid sample holders
- Dimensions: 51.5 mm Ø x 40 mm height, maximum
- Weight: Max. 400 g including sample holder
- Sample changer: X-Y changer with priority position for 1 sample (detected) and 2 empty holders with capacity for 8 trays for 8 sample holders and 1 tray for 4 sample holders.
Optional: High-capacity changer up to 209 uncupped samples of 32 mm or 140 uncupped samples of 40 mm diameter - Changer trays: for: 8 sample holders, 8 flex positions, 8 steel rings (Ø 51.5 mm), 21 samples (Ø 25 mm), 12 samples (Ø 32 mm), 10 samples (Ø 41 mm), or 4 sample holders (SPC/monitor tray)
- Loading: Air lock with programmable pumping time, one or two position turret mechanism, sample-surface down, direct loading of unmounted samples in holder in loading position
- Spinner: 0.5 rev/s
Applications
Wavelength dispersive X-ray fluorescence spectrometer for quantitative elemental analysis except Hydrogen, Lithium and Beryllium in solid state materials.
Overview
The Atomika 8030C spectrometer utilizes Total Reflection X-ray Fluorescence (TXRF) for qualitative and quantitative chemical analysis of liquid samples. Quantification is achieved by adding an internal standard of known concentration.
Sample Preparation & Measurement
- Samples are pipetted onto quartz reflectors.
- Automatic loading from sample magazines enables high-throughput analysis.
Excitation & Detection
- Excitation Sources:
- Mo-Kα, W-Lα, W-Lβ
- Bremsstrahlung (32 and 35 keV) from a 2.5kW Mo-W X-ray tube
- Monochromation: Achieved with a double multilayer monochromator.
- Detection: Fluorescence signals are captured using a Si(Li) detector.
Enhanced Sensitivity
- Helium atmosphere reduces scattering, enabling detection of Na, Mg, and Al.
- High-energy bremsstrahlung photons allow measurement of high-Z elements via K-lines.
- Detection limits reach the ppb – or pg range.
Overview & Design
- Developed for macro-XRF scanning of areas up to A4 size (197mm × 310mm).
- Designed for portable and flexible analysis of cultural heritage and technical samples.
- Mounted on a breadboard for transportability outside the lab.
X-ray Source & Excitation System
- End-window 4W air-cooled X-ray tube (AMPTEK Mini-X).
- Rh or Ag anode, easily exchangeable.
- Controlled via USB to PC for automated operation.
Detection & Imaging System
- Peltier-cooled SDD detector (KETEK 150 mm²) for fluorescence detection.
- Standard 45°-45° geometry between source, sample, and detector.
- Integrated CCD camera provides a top-down view of the sample surface.
- Two lasers for beamspot localization:
- Automated height adjustment ensures precise alignment of the X-ray beamspot.
- Corrects for curvature of the sample surface.
- Additional laser prevents collisions with samples, using low-cost components.
- Detection limit for Cu (500 ng sample, 40 kV, 100 µA, 100 s auf Kapton-Folie, extrapolated to 1000 s): 1,1 ng with a Sensitivity of: 0,305 cps/ng
Scanning & Motion Control
- X-Y stage with stepper motors for automated scanning.
- Software-controlled operation (developed in-house).
- Collimators (1, 2, or 3 mm) enable adjustable spatial resolution.
Applications & Performance
- Suitable for cultural heritage analysis and technical sample evaluation.
Overview & Objectives
- Confocal micro-XRF (μXRF) enables 3D spatial analysis of major, minor, and trace elements.
- Traditional polychromatic excitation causes quantification challenges, higher background noise, and scattered bremsstrahlung.
- The new setup aims to:
- Improve quantification accuracy.
- Enhance peak-to-background ratios.
- Maintain high spatial resolution.
- Offer flexibility for different excitation energies and portability to other sources.
X-ray Source & Beam Configuration
- Water-cooled fine-focus X-ray diffraction tube , 2 kW molybdenum tube
- Produces a quasi-parallel, monochromatic beam for improved signal quality.
- Current setup:
Confocal Setup & Detection System
- Two polycapillary half-lenses:
- One on the source side.
- One on the detector side, where a 50 mm² silicon drift detector (SDD) is mounted.
- Focal spot size: ∼15 μm for Mo-Kα.
- Flexible design:
- The second polycapillary can be replaced with a custom collimator for non-confocal μXRF measurements.
Performance & Detection Limits
- Detection limits established using NIST standard reference materials (SRMs) 621 and 1412.
- Selected element detection limits:
- Non-confocal mode: As detection limit of 1 μg/g.
- Confocal mode: As detection limit of 20 μg/g.
- Demonstrated performance on technical and biological samples.
Key Advantages
- Improved quantification due to monochromatic excitation.
- Lower background noise and reduced bremsstrahlung scatter.
- High spatial resolution (∼15 μm focus).
- Flexible system for different excitation energies.
- Portable design for easy transport to other X-ray sources.
Overview & Purpose
- Most micro-XRF spectrometers operate in air, limiting the analysis of low-Z elements (Z ≤ 14).
- This custom-designed spectrometer extends the analytical range down to Z ≥ 6 (carbon and above).
- Vacuum operation eliminates absorption of exciting and fluorescent radiation.
- Automated sample mapping controlled by custom software developed at the Atominstitut.
X-ray Source & Beam Focusing
- Air-cooled, low-power X-ray tube (50W) with molybdenum anode and a 125 µm thin exit window.
- Optional beam filter to reduce spectral background.
- Polycapillary X-ray optics focuses the beam onto the sample, achieving a 31 µm FWHM focal spot for Mo-Kα radiation.
Detection & Sample Positioning
- Si(Li) detector with ultra-thin window for detecting low-energy X-rays.
- High-resolution CCD camera & optical microscope for precise measurement positioning.
- Motorized XYZ sample stage for automated positioning and scanning.
3D Elemental Imaging via Confocal Geometry
- Recently adapted for confocal geometry by adding a second polycapillary X-ray optics in front of the detector.
- Enables 3D elemental imaging of light elements in the laboratory.
- Fig. 9: Shows the new spectrometer setup.
- Fig. 10: Displays the result of a 3D measurement of a test structure.
Key Advantages
- Enhanced excitation & detection conditions for light element analysis.
- Wide energy range excitation using Mo L-lines and K-lines.
- Improved low-energy X-ray detection due to the ultra-thin detector window.
- Vacuum operation eliminates air absorption of X-ray signals.
- Automated scanning with dedicated software.
- Tab. 1 shows the achieved detection limits
X-Ray tube
- Tube: Panalytical long fine focus with chromium anode (PW2278/20)
- Operation: Typically at 30kV and 30mA
- Power: 1.9kW, Max Voltage: 60kV
- Window: 300 µm beryllium
- Mounting: Directly on optical table, shielded with aluminum casing in vacuum chamber.
Monochromator
- Source: Repurposed from older ATOMIC TXRF system
- Bragg Angle for CrKα: 1.412° (determined by scanning in another spectrometer)
Detector & Cooling System
- Detector: Amptek Fast SDD with CMOS preamplifier
- Crystal Area: 70 mm², collimated to 50 mm²
- Window: Ultrathin Si₂N₃ with 43.9% transmission for carbon K-line fluorescence
- Energy Resolution: 122-129 eV FWHM at 5.9 kV
- Cooling: Maintained at 220 K (-53°C)
- Cooling System: Copper plating with Adaptive ET-063-10-13 Peltier element
- Temperature Control: STC-1000 switch to prevent condensation
- Electron Trap: Copper collimator with two permanent magnets to reduce noise from Auger electrons (effective area: 38.48 mm²).
Miscellaneous
- Alignment Aid: CCD camera inside the vacuum chamber for beam and sample positioning, with video feed to PC for easy alignment monitoring.
- Vacuum Pump: Hanning electric pump to maintain a pressure of 0.6-0.7 mbar in the chamber.
- Detection limits: LLD(C)= 4 ng
Vacuum Chamber & Setup
- Entire system enclosed in a vacuum chamber (300 × 300 × 340 mm³)
- Reduces primary X-ray scattering in air and minimizes absorption of low-energy fluorescence X-rays
- Silicon (Si) fluorescence at 1.7 keV is used for normalization in quantification and dose determination
X-ray Source & Beam Conditioning
- 3kW Mo-anode X-ray tube with a 0.04 × 12 mm² focal spot (long fine focus)
- Monochromatized primary beam (17.44 keV, Mo-Kα) using a multilayer monochromator
- Beam intensity monitoring via an ionization chamber
Detector & Data Processing
- Silicon drift detector (SDD, Vortex, Radiant) with 50 mm² active area
- Energy resolution: 140 eV at 5.9 keV (Mn-Kα) with 12 µs shaping time
- Maximum count rate: 100 kcps
Sample Stage & Movements
- 3 linear translation stages (25 mm travel range each)
- 1 rotation stage for angle scans (±0.28 rad, min. increment 1.35 µrad)
- Stage tilts around the beam axis to align the sample parallel to the beam
Measurement Parameters
- X-ray source: 3kW Mo-tube LFF (operated at 50 kV / 40 mA and 50 kV / 55 mA)
- Monochromator: Multilayer
- Detector: Vortex 50 mm² SDD with integrated electronics
- Measurement time: Variable (20 – 120 seconds per point)
- Angular resolution: Variable (23 - 115 µrad)
Measurement conditions: Performed in air and vacuum (<1 mbar)
A sketch of the prototype spectrometer is shown in Figure 1.
Overview
The Epsilon 5 from PANalytical is a commercial Energy Dispersive X-ray Fluorescence (EDXRF) spectrometer. It features:
- Water-cooled X-ray tube with a Tungsten-Scandium anode
- Liquid nitrogen-cooled Germanium detector
Excitation & Elemental Detection
- generator: Up to 100 kV, 24 mA, 600 W
- Wide element range: From magnesium (Mg) to uranium (U)
- Secondary target excitation:
- Fluorescent targets: Use characteristic radiation of the target element to excite the sample.
- Barkla targets: Use scattered tube radiation; polarization in a 3D optical path reduces spectral background compared to a 2D setup.
Sample Handling & Measurement Conditions
- Vacuum conditions for all measurements
- Automatic sample changer
- Compatible with pressed pellets and glass beads (up to 50 mm diameter)
Software & Data Analysis
- Spectrum peak search and match routine
- Quantification options:
- Standard-based analysis
- AutoQuantify software
- Various matrix correction models for improved accuracy
- Detection limits:
- µg/g (ppm) range
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© Klaus Ranger
Charakteristika
Röntgenröhre SST-mAX
- Anode: Rh-Standard
Goniometer
- Typ: θ/2θ entkoppelt mit direkter optischer Positionserfassung (DOPS)
- Winkelgenauigkeit: 0,0025° θ und 2θ
Optischer Pfad
- Primäre Kollimatoren: 3 max.: 100, 150, 300, 550, 700 oder 4000 μm
- Primäre Strahlfilter: max. 4: einer kann als Strahlblende verwendet werden
- Kristalle: max. 8: LiF420, LiF220, LiF200, Ge111 (flach/gekrümmt), PE002 (flach/gekrümmt), InSb (flach/gekrümmt), TlAP beschichtet, PX1, PX4, PX5, PX6, PX7, PX10
- Detektoren: Durchfluss, Szintillation, versiegeltes Xe im Tandem mit Durchflusszähler als Duplexzähler (optional), Hi-Per Scint (optional)
Zählerelektronik
- Typ: Doppelter Mehrkanal-Analysator mit digitalem Signalprozessor
Handhabung von Proben
- Arten: Feststoffe, Schmelzperlen, Filter, gepresste/lose Pulver und Flüssigkeiten
- Handhabung: Alle Proben werden während der Messung in Probenhalter eingesetzt. Flüssigkeiten und lose Pulver in Einweg-Flüssigkeitsküvetten (P2), die in Flüssigkeitsprobenhalter eingesetzt werden
- Abmessungen: 51,5 mm Ø x 40 mm Höhe, maximal
- Gewicht: Max. 400 g einschließlich Probenhalter
- Probenwechsler: X-Y-Wechsler mit Prioritätsposition für 1 Probe (erkannt) und 2 leere Halter mit Kapazität für 8 Tabletts für 8 Probenhalter und 1 Tablett für 4 Probenhalter.
- Optional: Hochkapazitätswechsler für bis zu 209 unkupierte Proben von 32 mm oder 140 unkupierte Proben von 40 mm Durchmesser
- Wechslertabletts: für: 8 Probenhalter, 8 Flexpositionen, 8 Stahlringe (Ø 51,5 mm), 21 Proben (Ø 25 mm), 12 Proben (Ø 32 mm), 10 Proben (Ø 41 mm) oder 4 Probenhalter (SPC/Überwachungstray)
- Beladen: Luftschleuse mit programmierbarer Pumpzeit, ein- oder zweistufiger Revolvermechanismus, Probenfläche nach unten, direktes Laden von unmontierten Proben in Halter in Ladeposition
- Drehvorrichtung: 0,5 Umdrehungen pro Sekunde
Anwendungen
Wellenlängendispersives Röntgenfluoreszenzspektrometer für die quantitative Analyse aller Elemente, ausgenommen Wasserstoff, Lithium und Beryllium in festen Proben.
Sample preparation:
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© Klaus Ranger