Empyrean Technical Specification
Empyrean Technical Specification
Technical specifications
2 3
H
Wide enclosure doors for easy access to all parts of
the diffractometer
I PC-controlled system settings for all measurement
types via the Data Collector control software
5 Detector
Sample stage
2
and holder
The Empyrean system: Integral features (A–H) and configurable options (1–6).
4 5
Basic specifications
The X‐ray generator, tube housing, goniometer, rack mounts, cabinet, Data Collector control software, control electronics
Goniometer
and power supply are integrated into every Empyrean configuration. Basic specifications for the entire system are shown
below. Configurations Vertical goniometer with either theta–theta or theta–2theta (Alpha-1) geometry
Measuring circle diameter 480 mm (radius 240 mm). Can be changed for specific applications
System and supplies Goniometer angular range 360° (without accessories)
Exterior dimensions 1400 mm (w) × 1162 mm (d) × 1947 mm (h). The instrument has transportation wheels, Max. 2θ range –111° < 2θ ≤ 168° (depending on accessories)
and requires an absolute minimum door opening of 867 mm for transportation
Angle positioning Digital optical position sensing (DOPS3) with lifetime positioning accuracy using
Interior accessibility 1360 mm (w) × 1100 mm (h), allowing access to the experimental area by at least four Heidenhain encoders and path tracking technology
people
Max. angular speed 15°/s
Weight 1050 kg (2310 lb)
FWHM for powder diffraction <0.03° 2θ on LaB6 (with 0.01 rad Soller slits)
X‐ray safety Less than 1 µSv per hour, measured at 10 cm distance, determined with a Mo source
(60 kV, 50 mA) (this X-ray safety level determination method assures the absolute Highest achievable resolution ≤0.0028° (≤10″) for Si single crystal (111) reflection (rocking curve with 4 × Ge(440)
safety of all radiation energies up to and including those from an Ag tube at 60 kV) monochromator)
Safety loops Xsafe: Two independent safety loops monitor the conditions under which the shutter 2θ linearity over whole range Equal or better than ±0.01° 2θ
can open. The system cannot operate when the doors and shutters are open Smallest addressable increment 0.0001°
Msafe: A double safety interlock system ensures unrivalled protection of users from Positioning reproducibility 2θ ≤ ±0.0001°
potential trap hazards by moving parts
PreFIX Second-generation universal pre-aligned fast interchangeable modules (PreFIX) for
Cooling water supply 4–6 L/min, pressure up to 8 bar, temperature 15–35°C above the dew point alignment-free interchange of optics, stages and accessories
Compressed air supply House line, compressor, or air bottle; 2–5 bar (0.2–0.5 MPa) Optic PreFIX dismounting/ 2θ < ±0.0015°, user-independent
Power supply Single-phase, 180–253 V, 47–63 Hz mounting peak position
reproducibility
Max. power consumption 4.6 kV·A (basic system)
Stage PreFIX dismounting/ Z < ±2.5 µm, user-independent
Rack mounts (19 inch) Easy access to non-ambient controllers and integrated vacuum system
mounting Z position
reproducibility
PreFIX
module
T-block
Countersunk
Lock pin
U-block
PreFIX
Locking screw
High-speed accuracy (0.0001° addressable increment) PreFIX system for alignment-free optic and PreFIX U-blocks for alignment-free stage exchange Component recognition for all optics
stage exchange
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1 X-ray tubes
All the Empyrean tubes are manufactured with patented Mo LFF 60 55 3.0
CRISP technology to avoid corrosion of both tube parts Mo LFF-HR* 60 55 2.5
and nearby optics such as incident beam mirrors.
Ag LFF 60 55 2.2
Ag LFF-HR* 60 55 1.8
* LFF-HR (Long Fine Focus – High-Resolution): This focus design delivers long-term stability of a high-quality X‐ray beam
at continuous high power. It is an ideal solution for mirrors and monochromators
X-ray generation
X‐ray generator power 4 kW (max. 60 kV, max. 100 mA)
Available anode materials (LFF) Cu, Co, Cr, Fe, Mn, Mo, Ag
Tube housing Pb-free. Patented technology* prevents corrosion in the incident beam path caused by
X‐ray-induced ionization of air
* Corrosion-resistant incident smart beam path (CRISP)
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Selecting the right sample stage and holder is vital To ensure that the X‐rays are probing the correct part Spinner stages
to ensure reliable, accurate results for your samples. of your sample, we offer several sample alignment Reflection–transmission spinner stage Sample changer Sample holders for powders, solids and
Fortunately, with a large choice of sample stages – from strategies, including measuring routines, cameras, laser viscous materials
the popular static and spinner stages to versatile modular gauges and mechanical dial gauges.
360° continuous rotation 3 × 15 positions with 3 additional We offer:
stages and more – you’ll be sure to find something that Finally, if you’re in a high-throughput environment,
Programmable spinning speed, max. monitor positions • Different aperture sizes for large and
comfortably accommodates your sample, and enables then make sure you ask about the options for reducing
120 rpm Supports domed sample holders small illuminated areas
safe, precise handling. turnaround time by automating the analysis of multiple
for air-sensitive samples • Zero-background inserts for small
samples. Programmable phi scan with step size
quantities
0.1° ± 0.1°
• Patented design low-angle holders
Max. holder diameter 44 mm • Holders for transmission (between foils)
Supports domed sample holder • Disposable holders
Static stages • Solid sample holders
Supports coin battery for in-situ
For flat samples, or powders in flat Multipurpose Flow cell • Options for mounting solids in open or
measurement
sample holders spring-loaded holders
• Air-tight sample holders
Included with every Empyrean Manual positioning (using dial gauge For dynamic crystallization and SAXS • Specialized domed sample holders for
Used with rectangular sample holders for Z-adjust) research air-sensitive samples
Max. sample volume φ step size 1° (±1°)
15 mm × 20 mm × 2 mm Tilt range ±3°, step size ±0.3° (±0.3°)
Z range 0–100 mm
Z step size ±15 µm (±15 µm)
Reflection–transmission spinner
Stage Programmable Manual Z Programmable Manual XY Manual phi Sample Axis Range Step size Axis Range Step size
Z XY platform
XY 54 mm 0.01 mm ± 0.01 mm
Range 25 mm 73 mm 54 mm 54 mm 360° Static
Z 12 mm 0.001 mm ± 0.001 mm Z 12 mm 0.001 mm ± 0.001 mm
Step size 0.001 mm 0.001 mm 0.01 mm 0.01 mm 0.01° Static
φ 720° 0.01° ± ≤0.01° φ 720° 0.01° ± ≤0.01°
Reproducibility ±0.001 mm ±0.001 mm ±0.01 mm ±0.01 mm — —
χ 96° (–3° to 93°) 0.01° ± ≤0.01° χ 96° (–3° to 93°) 0.01° ± ≤0.01°
Programmable XY and Z Manual XY and Manual XY and manual Manual Z with sample platform
with large levelling holder programmable Z with Z with sample holder and large holder for solids
for solids sample holder for for solids
solids 5-Axis cradle (with sample holder 80 mm) 3-Axis cradle (with manual XY sample platform)
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Stage accessories
Laser height sensor Alignment camera Dial gauge for height Capillary alignment Stage holder
alignment microscope
Sample alignment Z Sample positioning XY. Sample alignment Z Alignment of PreFIX holder for safe Coin cell holder Electrochemical cell Transmission holder VTEC VTEC-trans
in combination with a Capillary alignment capillaries outside the storage of stages
motorized Z stage cabinet
*
PEEK dome option
DHS 1100 Domed hot stage DCS 500 Domed cooling stage
Non-ambient stages for high temperature Non-ambient stages for low and medium temperatures
HTK 1200N with Z-axis control HTK 16N with Z-axis control XRK 900 reaction chamber with Z-axis TTK 600 with Z-axis control CHC Plus+ with PheniX cryostat with Cryostream Compact
HTK 1200N capillary with Z-axis HTK 2000N with Z-axis control control Z-axis control Z-axis control 800 Plus for capillaries
control HTK 2000N W with Z axis control
Resistance heating, liquid Heating/cooling Two-stage closed-cycle cooler Gas stream cooling/heating
Oven heaterwith spinner or capillary Strip heater w
ith flat plate Oven heaterwith flat plate nitrogen cooling Flat plate Flat plate Capillary
perating temperature:
O perating temperature:*
O perating temperature:
O Flat plate perating temperature:
O perating temperature:
O perating temperature:
O
• HTK 1200N spinner, rigid • HTK 16N • Macor sample holder Operating temperature: • Compressed air cooling • 12–290 K (–261°C to17°C) • 80–500 K(–193°C to
• RT to 1200°C • RT to 1600°C (Pt strip†) • RT to 900°C (air, inert gas, • Dry air cooling • 10 to 80°C (humid gas) 227°C)
Cool-down time:
• RT to 1000°C (helium) • RT to 1500°C (Ta strip‡) vacuum) • –10 to 400°C • –5 to 300°C (dry air, • From RT to 20 K Cool-down time:
• HTK 1200N capillary extension • HTK 2000N • RT to 750°C (10 bar helium) (dry air, nitrogen) nitrogen) (–253°C): 40 min • From RT to 100 K
• RT to 1000°C (quartz capillary) • RT to 2300°C (W strip‡) • Stainless steel sample holder • –20 to 600°C • –5 to 400°C (10 –2 mbar) • From RT to 12 K (–173°C): 20 min
• RT to 700°C • RT to 1600°C (Pt strip†) • RT to 600°C (all atmospheres) (10 –2 mbar) • Liquid nitrogen cooling (–261°C): 60 min Liquid nitrogen consumption:
(borosilicate capillary) • RT to 1500°C (Ta strip‡) • RT to 260°C (with electrical • Liquid nitrogen cooling • –120 to 300°C (nitrogen) tmospheres:
A • 0.6 L/h at 5 L/min gas flow
Atmospheres: Atmospheres: feedthrough) • –150 to 400°C (nitrogen, • –180 to 400°C • Vacuum (≤10 –4mbar) ample holder accessories:
S
• Air, inert gases, nitrogen • Air, helium, nitrogen Atmospheres: dry air) (10 –2 mbar)
ample holder accessories:
S • Capillary spinner
• Vacuum (10 –4 mbar) • Vacuum (≤10 –4 mbar) • Air, inert gas, vacuum (1 mbar), • –190 to 600°C Humid air/nitrogen: • Cr–Cu alloysample in transmission geometry
ccessories for reflection geometry:
A trip compatibility:
S reactive gases* (10 –2 mbar) • 5–95% RH (10–60°C) holders • Glass capillary
• Al2O3 sample cups • Vacuum (for Pt, Ta, W) • Gas pressure from 1 mbar to 10 bar Atmospheres: • 5–70% RH (at 80°C)
• Zero-background insert • Inert gases (for Pt) (relative)† • Air, inert gases, nitrogen Atmospheres:
• Vacuum (≤10 –4 mbar) • Air, inert gases, nitrogen
*
Affected by the chamber atmosphere For reactive gases list, refer to
*
• Pressure (max. 2 bar • Vacuum (10 –2 mbar)
†
Only for short-term operation in air Anton Paar
or vacuum †
High-pressure atmospheres require
relative) ample holder accessories:
S
‡
Only in vacuum (≤2 × 10–4 mbar) hard X‐rays ample holder types:
S • Cu–Nialloy sample
High-vacuum pump required
• Standard reflection holders
sample holder • Zero-background insert
• Transmission geometry
with foil
• Transmission geometry
with capillary
• Coin cell holders
for batteries
HTK 1200N oven chamber HTK 2000N chamber XRK 900 reaction chamber
TTK 600 chamber CHC Plus+ cryo- and PheniX cryostat Cryostream Compact 800 Plus
humidity chamber
Alexander Dziouba
Systems Software Architect, Malvern Panalytical
16 17
Multi-layer mirror for high- Multi-layer mirror for high- Provides a quasi-parallel Provides a focused (on the These work with: These work with: These work with:
quality, high-intensity Kα, quality, high-intensity Kα, high-intensity Kα beam (Kβ detector) high-intensity • Focusing X‐ray mirror • Focusing X‐ray mirror • Focusing X‐ray mirror
and suppression of Kβ and and suppression of Kβ and <0.5% of its original level) Kα beam (Kβ <0.5% of its • Parallel beam X‐ray mirror • Parallel beam X‐ray mirror • Parallel beam X‐ray mirror
white radiation white radiation The PreFIX module housing original level) • Hybrid monochromator • Bragg-BrentanoHD
Produces divergent and The PreFIX module housing contains slots for: The PreFIX module housing
quasi-parallel beams: contains slots for: • Primary equatorial slit contains slots for:
• Primary and secondary • Primary equatorial slit (e.g. 1/2°) • Primary equatorial slit
(entry and exit) (e.g. 1/2°) • Primary beam attenuator (e.g. 1/2°)
programmable beam • Primary beam attenuator or beam mask • Primary beam attenuator
masks with sizes in the or beam mask • Secondary Soller slits or beam mask
range 0.1–14 mm • Secondary Soller slits • Secondary beam • Secondary Soller slits
• Fixed-mode divergence • Secondary beam attenuator, beam mask or • Secondary beam
slit: 1/50° to 1/2° in six attenuator, beam mask or anti-scatter slit attenuator, beam mask or
steps anti-scatter slit Optionally used as a anti-scatter slit
• Programmable divergence Tubes: Mo, Cu and Co diffracted beam optic in Tubes: Cu, Co, Mo, Ag
slits: 0.5–20 mm in 0.5 mm (Dedicated optic for each mirror–mirror geometry (Dedicated optic for each
steps tube type) Tubes: Cu and Co (Dedicated tube type)
• Soller slits: 0.03 rad
optic for each tube type)
Works with matching dCore
for a fully automated and GISAXS kit with focusing mirror Microbeam masks with parallel beam mirror Microbeam collimator with
programmable suite of Bragg-BrentanoHD
configurations
Tubes: Cu and Co (Dedicated
optic for each tube type)
dCore FRS with monochromator and Front of shielding tube Front of shielding tube
miniprop detector with FASS. with PASS
Goniometer showing tube, Bragg-BrentanoHD incident beam optics, 5-axis cradle, and dual arm supporting two sets of
diffracted beam optics (1) Pixcel3D with Soller slits and PASS and (2) Miniprop detector with Soller slits and PPC.
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Supported tubes Ag, Mo, Cu, Co, Fe, Cu, Co, Fe, Mn, Cr Ag, Mo, Cu Ag, Mo, Cu, Co, Ag, Mo, Cu, Co,
Mn, Cr Fe, Mn, Cr Fe, Mn, Cr
Efficiency (Cu Kα) >94% >95% ~100% 84% 93%
Efficiency (Mo Kα) 37% ~100% 36% 99%
Energy resolution <5% (for Cr, Co, Cu Kα) 18% 25% 19% 45%
(for Cu Kα) <3% (for Ag, Mo Kα)
Maximum count Overall† 38.4 × 106 cps Overall 30 × 109 cps Overall 2.4 × 1011 cps 1 × 106 cps 1 × 106 cps
rate Strip† 300 × 103 cps Strip 120 × 106 cps Strip 4.7 × 108 cps
Maximum Overall <0.4 cps Overall <0.5 cps Overall <6.0 cps 2 cps 8 cps
background
Parallel plate collimator 3-bounce 3-axis analyzer Diffracted beam mirror Dffracted beam monochromator
for PIXcel
PDF-2 Features 327,600+ entries. 224,900+ entries have I/Ic values for quantitative analysis by
reference intensity ratio
Five-year license
PDF-4/AXIOM Features 101,900+ selected data entries, including inorganic and organic entries
Cost-effective database, developed for users of benchtop XRD systems
Three-year license term or six-year and nine-year prepaid packages
“It’s exciting to be working at the cutting edge of technology, combining physics
with computer science to provide great tools for materials scientists worldwide.” PDF-4+ Features 460,900+ entries, including 353,300+ entries with atomic coordinates
One-year license serviced by subscription
Gareth Tye PDF-4 Minerals Features 49,900+ entries, including 40,300+ entries with atomic coordinates
Scientific Programmer, Malvern Panalytical
A subset of the PDF-4+ database with all the features and capabilities, targeted to
minerals and related compounds
One-year license serviced by subscription
PDF-4/Organics Features 560,100+ entries and with 156,100+ entries with atomic coordinates
Collection with special focus on materials used in commercial and regulatory fields
One-year license serviced by subscription
26 27
Data analysis
AMASS AMASS is an analytical software package for visualizing and analyzing single and 2-axis scan data to
Product demos
determine relevant thin-film parameters
If you like what you’ve read about Empyrean, but want to
• AMASS Basic offers many peak position-based calculations for rocking curves, and reciprocal
see what it’s like in real life… then look no further!
space maps in order to calculate mismatch, composition, thickness and relaxation
• AMASS HR is an additional option providing simulation and fitting of rocking curves Talk to us about arranging:
• AMASS Reflectivity is an additional option offering analysis of specular reflectivity curves and • A remote demo by video link
reflectivity maps, including calculations and simulation with fitting
• An in-person demo at your local application center
The embedded COM interface allows direct connection with Python, Matlab and Command Prompt
Alternatively, visit our YouTube channel to watch product
Stress Stress Plus is an option for Stress that extends the analysis to shear stress and polycrystalline coatings demos at the click of a mouse!
(thin films).
• Wide choice of pattern treatment and peak position methods.
• Multiple-{hkl} sin²ψ stress analysis.
• Combined Multiple-{hkl} and χ-tilting stress analysis.
• Analysis directly on the grazing incidence XRD data.
ARRANGE A DEMO
• Analysis on combined datasets from multiple measurement files.
• Interactive calculations and complete, automatic analysis.
It is suitable for routine analysis as well as for research.
Stress Plus Stress Plus is an option for Stress that extends the analysis to anisotropic systems (such as in thin
films), and is suitable for routine analysis as well as for research
Texture Texture is an analytical software program for quantitative texture analysis with comprehensive graphics
tools
Texture includes corrections on experimental pole figures and calculation of orientation distribution
Customized systems
functions (ODFs), pole figures and inverse pole figures according to the WIMV method. It reads texture
If you’ve looked through these specs, and are thinking We can adapt the Empyrean to your requirements,
data files from Data Collector (*.XRDML) and PC-Texture
“that’s not quite what I need”, then don’t worry, the including:
EasySAXS EasySAXS is for the analysis of small-angle X‐ray scattering (SAXS) and ultra-small angle X-ray ‘Specials’ team is here to help. • Modified sample holders for unusual samples
scattering (USAXS) data, and offers a full data analysis toolbox, automation options and reporting
• Customized optical modules
Providing analysis on nanoscale structures and dimensions, nanoparticle shapes and specific surface
• Non-ambient stages
areas, EasySAXS data can additionally be exported in a format that is compatible with publicly available
SAXS software packages that give access to extended analysis options • Addition of in-house devices
• Batch automation for improved throughput
We’re continually devising ways of helping our customers
CONTACT US get the best results from their samples. Let’s talk about
how we can help you.
Customer support
Every Empyrean we ship is built to an exacting standard – So wherever you are in the world, a Malvern Panalytical
and that same care and attention extends to our applications scientist or service engineer is never too far
post-sales service too. away, ready to offer:
• Online and telephone support
• Preventative maintenance
• Corrective maintenance
• Remote diagnostics
• Spare parts management
• Training and consultancy
• Performance certification
CONTACT OUR SALES TEAM
• Updates and upgrades
Why choose us? Service & Support
When you make the invisible visible, Malvern Panalytical provides the global training, service
and support you need to continuously drive your
the impossible is possible. analytical processes at the highest level. We help you
Our analytical systems and services help our increase the return on your investment with us, and
of this information and we shall not be liable for errors contained herein or for damages in connection with the use of this material. Malvern Panalytical reserves the right to change the content in this material at any time without notice.
customers to create a better world. Through ensure that as your laboratory and analytical needs
Disclaimer: Although diligent care has been used to ensure that the information in this material is accurate, nothing herein can be construed to imply any representation or warranty as to the accuracy, correctness or completeness
chemical, physical and structural analysis of materials, grow, we are there to support you.
they improve everything from the energies that Our worldwide team of specialists adds value to your
power us and the materials we build with, to the business processes by ensuring applications expertise,
medicines that cure us and the foods we enjoy. rapid response and maximum instrument uptime.
We partner with many of the world’s biggest companies, • Local and remote support
universities and research organizations. They value us
• Full and flexible range of support agreements
not only for the power of our solutions, but also for the
• Compliance and validation support
depth of our expertise, collaboration and integrity.
• Onsite or classroom-based training courses
With over 2200 employees, we serve the world,
• e-Learning training courses and web seminars
and we are part of Spectris plc, the world-
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