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Empyrean Technical Specification

The document describes the technical specifications of the Empyrean X-ray diffractometer. It has integral features like an X-ray generator and safety components. It also has configurable options like X-ray tubes, sample stages, incident and diffracted beam optics, detectors, and software.

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thoanp1990
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0% found this document useful (0 votes)
1K views15 pages

Empyrean Technical Specification

The document describes the technical specifications of the Empyrean X-ray diffractometer. It has integral features like an X-ray generator and safety components. It also has configurable options like X-ray tubes, sample stages, incident and diffracted beam optics, detectors, and software.

Uploaded by

thoanp1990
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd
  • Empyrean Series 3 Overview
  • Basic Specifications
  • X-ray Tubes
  • Sample Stages and Holders
  • Incident Beam Optics
  • Diffracted Beam Optics
  • Detectors
  • Software
  • Additional Resources

Empyrean Series 3

Technical specifications
2 3

Building your Empyrean system

About this document Feature overview Integral features Configurable options


All the following come with every Empyrean system: The following options are configurable, with lots of
This document describes the technical specifications for Using the Empyrean, you can acquire many types of data,
choices under each heading, some of which depend on
all configurations of the Empyrean X‐ray diffractometer and accommodate a wide range of sample types. This
each other:
(XRD), as described in the Empyrean brochures. is because it’s a modular system, with a combination A  ‐ray generator and tube housing for high-stability
X
Before you read this document, you should already of integral features (A–H) and options that can be tubes
know what you need your Empyrean system to do, and individually configured (1–6). 1  ‐ray tubes offering a range of wavelengths for your
X
B  afety locks, warning lights and build quality for full
S
have a rough idea of the functions you’re looking for. radiation safety according to worldwide regulations experiments
This document will help you move to the next stage – a Sample stages and holders to accommodate every
2
High-resolution goniometer with precision-built
C
consultation with an applications specialist to refine your sample shape and size
PreFIX mounting
configuration, and ensure your Empyrean is precisely
D 19” racks for mounting power and controls for up to 3
Incident beam optics suitable for all measurement
tailored to your requirements. 
two non-ambient stages or custom electronics setups
Naturally, some of the detail in this document gets
E On/off switches with generator and goniometer
 4
Diffracted beam optics providing a perfect match for
technical – so don’t be afraid to ask us any questions!
status display the incident beam

F Spacious cabinet with room for sample changers, 5


Detectors to capture every detail

and accessories, gas bottles 6
Software for controlling experiments and conducting
Incident beam optics 3 4 Diffracted beam optics
G
Emergency off button analyses

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

6 Software Ready to start?


1
X-ray tube In consultation with our applications specialists,
you’re now ready to work through the options, and
select the configuration that best matches your
X‐ray generator A requirements. Make sure you talk to them about:

H Wide enclosure • The type of results you need


• The level of data quality you require
C doors • How easy-to-use you need the system to be
High-resolution • Turnaround time
goniometer • The expertise of your team
• Budget
G Emergency off button
B “I love the ease of access into the Empyrean,
Need an Empyrean expert to discuss your ideal
Fully radiation- configuration? in particular when teaching or discussing it
safe enclosure
Contact our team with multiple people. I also love the wide glass
doors that wrap around the side of the cabinet.
It’s an X‐ray lab in its own pristine enclosure”.
Power & control racks D
On/off switches E F Spacious cabinet
Fabio Masiello
Group Product Manager – XRD, Malvern Panalytical

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

Component recognition For all optics

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
6 7

1 X-ray tubes

Our easy-change X‐ray tubes are optimized for the


Tube types
best diffraction performance, and you can choose from
a wide range of X‐ray target materials to give you the Anode Focus Max. voltage (kV) Max. current (mA) Max. power (kW)
wavelength you need for your experiments.
Cu LFF 60 55 2.2
For example:
Cu LFF-HR* 50 55 1.8
• Cu, the most commonly used target material, gives
both a well-resolved and optimum-range diffraction Co LFF-HR* 50 55 1.8
pattern for many materials Co LFF 60 55 1.8
• Ag and Mo generate high-energy X‐rays that can
penetrate solids, and provide access to large Cr LFF 60 55 1.9
scattering vectors. Fe LFF 60 55 1.0
At Malvern Panalytical we have our own tube factory with
our own R&D department and our own recycling facility. Mn LFF 60 55 1.0

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)

Tube voltage 15–60 kV

Tube current 5–60 mA

Line regulation <0.005% for ±10% change in input voltage/current

Available anode materials (LFF) Cu, Co, Cr, Fe, Mn, Mo, Ag

Available anode materials Cu, Co, Mo, Ag


(LFF-HR)

Number of focus window 2, line focus and point focus

Focus size at 6º take off angle 0.04 mm × 12 mm (line focus)


0.4 mm x 1.2 mm (point focus)

Line/point focus rotation Standard feature (with automatic recognition)

Focus window material 300 µm Be

Recommended power settings 0.9–3.0 kW, depending on tube type

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)
8 9

2 Sample stages and holders

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)

All sample types for RT Spinner

Stage for flat samples Multipurpose sample stage Flow cell

Reflection–transmission spinner

Sample changer with A wide range of sample holders are available


three cassettes
10 11

Modular stages Capillary and SAXS sample stages


The modular stages and sample platforms hold samples
Capillary spinner ScatterX78 SAXS/WAXS stage 2D WAXS stage
up to 150 mm in diameter, 100 mm high and with a
maximum weight of 10 kg. They are versatile, with many Supports 1D USAXS, SAXS, Supports 1D and 2D SAXS/ Supports USAXS, 1D and 2D Supports 2D WAXS
configuration options to suit different types of sample WAXS, transmission XRD, WAXS measurements in SAXS/WAXS measurements measurements
and different measurement types. In addition to small and and PDF measurements vacuum in air Gel samples between foils
regular sized samples in the standard holders, large and Spin speed: 5 rev/s
• Alignment-free mounting with pre-aligned sample Bulk samples between
irregularly shaped samples can be supported in a variety
Recommended capillary socket frames
of sample clamps, and accurately positioned either
diameters: 0.3, 0.5, 0.7, • Capillaries (diameters 0.3, 0.5, 0.7, 1.0 mm) PIXCel3D angular range from
manually or automatically.
1.0 mm • Powder samples between foils –22° to +22° 2θ
Accessories for modular stages: • Bulk samples between frames
GaliPIX3D angular range from
• Dial gauge for sample height adjustment. • Temperature-controlled (5 to 70 °C) capillary holder
Programmable XY and Z stages with large levelling holder –30° to +30° 2θ
• Beam knife
• Sample holder for solids
• Holder for wafers with or without adjustable levelling
(up to 100 mm)
• Magnetic ring for magnetic platform
• Magnetic mounting platform
• 12-position sample holder (for <25.4 mm diameter
samples)
• High-throughput stage
• Well plate including holder
Capillary spinner with a ScatterX78 SAXS/WAXS stage 2D WAXS stage for GaliPIX3D
goniometer head

Manual Z stage with multipurpose sample platform

Tilting and rotating cradles


Modular stages 5-Axis cradle (χ, φ, X, Y, Z) 3-Axis cradle (χ, φ, Z)

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°

Maximum sample height: 16 mm Maximum sample height: 64 mm


Maximum sample size: 80 mm (diameter) Maximum sample size: 140 mm (diameter)
Cradle accessories: Cradle accessories:
• Magnetic mounting platform • Magnetic mounting platform
Programmable Z Manual Z Programmable Manual XY Manual phi Sample • Sample holder 80 mm (with or without levelling option) • Sample holder 80 or 140 mm (with or without levelling
XY platform • Sample holder with four positions for 32 mm samples option)
• Sample holder in-plane • Manual XY sample platform
• Sample platform for GISAXS
Modular stage combinations
• Sample platform with holders for reflection and
Programmable XY + Manual XY + Manual XY + Sample platform + transmission
Programmable Z Programmable Z Manual Z Manual/programmable Z
Max. sample height 50 mm 50 mm 100 mm 100 mm

Max. sample size 95 mm × 95 mm 95 mm × 95 mm 95 mm × 95 mm 150 mm diameter

Max. sample mass 2 kg 4 kg 4 kg 10 kg

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)
12 13

High-throughput stage Stages for batteries and electrochemical cells


Axis Range Step size Coin cell holder for CR20xx EL-CELL in-situ Transmission holder for Variable-temperature
type batteries electrochemical test cell thin solid samples electrochemical cell (VTEC)
XY 100 mm 0.01 mm ± 0.01 mm
In-situ studies during charging In-situ studies during In-situ studies during In-situ studies during charging
Z 11 mm 0.001 mm ± 0.001 mm and discharging charging and discharging charging and discharging and discharging
Oscillation Yes Coin cell holder in reflection Electrochemical test cell Thin solid samples, pouch Variable-temperature
geometry for cathode and anode cells, prismatic cells electrochemical cells in
Geometries Reflection and transmission
Enables CR20xx battery materials Transmission geometry reflection (VTEC) and in
Cradle accessories: assembly and loading into a Reflection geometry (hard radiation) transmission (VTEC-trans)
• Magnetic mounting platform standard sized sample holder geometries
Can be mounted on a
• Sample holder 80 or 140 mm (with or without levelling Can be mounted on a modular
Compatible with reflection– modular stage or a 3-axis
option) or multipurpose sample stage
transmission spinner and a cradle
• Selection of standard and made-to-order well-plate
variety of cradles and modular
holders
stages
High-throughput stage

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

Domed stages for low and high temperatures


DHS 1100 Domed hot stage ​ DCS 500 Domed cooling stage
Laser height sensor Alignment camera Dial gauge Alignment microscope Stage holder
Resistance heating​ Resistance heating, liquid nitrogen cooling plate​
Graphite dome* Graphite dome
Operating temperature: Operating temperature:
• RT to 1100°C (air, nitrogen, vacuum) • RT to 500°C (air, inert gas)
Specialist stages • RT to 1000°C (helium) • –180°C to 500°C (vacuum)
Computed tomography GISAXS Customized stages Atmospheres: Atmospheres:
• Air, inert gases, nitrogen​ • Air, inert gases, nitrogen​
3D imaging and absorption of Kit for grazing-incidence small-angle. To suit individual requirements
• Vacuum (<0.6 mbar) • Vacuum (<0.5 mbar)
3D objects X‐ray scattering (for nano-patterned
φ: 0–360°​ φ: 0–360°
surfaces)
χ: 0–85°​ χ: 0–85°​
Works with 3-axis cradle
Transmission: 65% (Cu Kα)​ Transmission: 65% (Cu Kα)​

*
PEEK dome option

DHS 1100 Domed hot stage DCS 500 Domed cooling stage

CT stage GISAXS kit Customized stages


14 15

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 heater​with spinner or capillary Strip heater w
​ ith flat plate Oven heater​with 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 to​17°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 –4​mbar) ​ 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 alloy​sample 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–Ni​alloy 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

“It’s an interesting software challenge to integrate controllers,


chambers, cables and tubes! But it’s rewarding to see all the pieces
come together, because I know that it’s central to the Empyrean’s
dependability, which in turn gives peace of mind to our customers”

Alexander Dziouba
Systems Software Architect, Malvern Panalytical
16 17

3 Incident beam optics


The optimum incident beam optics for your Empyrean depend on the data required and the type of sample.
So whether you want to investigate small sample areas, perform fast routine measurements, study thin films, or deal with
irregularly shaped objects, we have a large supply of incident beam slits, mirrors and accessories to give you the best results.

For basic powder diffraction For specialized methods


Crossed slits Programmable-divergence Fixed-divergence slit (FDS) Johansson monochromator Parallel beam X‐ray lens Monocapillary and focusing Parallel beam hybrid Parallel beam Bartels
slit (PDS) module module for Alpha 1 radiation (multipurpose) lens (microbeam) monochromators monochromators
Crossed slits can be used PDS operates with two A simplified fixed-divergence Part of the Empyrean Works with point focus to Works with point focus to Used with line focus to Used with point or line focus
with line or point focus independently motorized slit (FDS) and fixed anti- Alpha-1 system provide a quasi-parallel beam provide a divergent small provide a parallel beam with to provide an ultra-parallel
to provide a controlled blades, providing a scatter slit (FASS) module Contains a Ge(111) single- The effective beam spot for powder diffraction high resolution and high monochromatic beam
illuminated area symmetrical irradiated is supplied with every crystal monochromator diameter can be adjusted applications intensity Narrowest energy band Kα1
Double-crossed slits provide footprint at all angles Empyrean system. from <0.4 mm to 7 mm by Different capillary lengths Narrow energy band Kα1
It includes: Choice of crystal reflections:
a quasi-parallel beam Two programmable modes: additional cross-slits and spot sizes are available Choice of hybrid
• Slits: 2 × 1/32° (one of Ta), • 4 × Ge(220)
Single-crossed slits provide a • Fixed-divergence slit Used in combination with Monocapillary monochromator • 4 × Ge(220) asymmetrical
mode, to provide 4°, 2°, 1/2°, 1°, 2°
divergent beam diffracted beam parallel plate • 135 mm x 0.1 mm • 2 × Ge(220) • 4 × Ge(440)
1°, 1/2°, 1/4°, 1/8°, 1/16° or • Masks: 5 and 10
A crossed-slit assembly can collimator (PPC) • 135 mm x 0.3 mm • 4 × Ge(220) Optional crossed slits
1/32° • Soller slits: 0.04 rad
be added to the exit-point Tubes: Cu, Co, Cr, Fe, Mn • 165 mm x 0.1 mm Slots for divergence slit,
• Programmable-divergence The optional FDS+FASS Used in combination with
of parallel beam optics, to • 165 mm x 0.3 mm attenuator or mask
slit mode, to provide a conversion kit completes the 3-axis diffracted beam optics
provide a small spot: set and includes: Focusing lens Optional Soller slit holder,
fixed irradiated length Tubes: Cu
• Knob for manual from 0.5–20 mm (in steps • Slits (1/16°, 1/8°, 1/4°, • 50 μm High Intensity crossed slits and SAXS slits
adjustment of 0.5 mm) and 4°) • 50 μm High Resolution
Tubes: Cu, Co (Dedicated
• Slit dimensions 0.0–10 mm • Masks (15 and 20) Tubes: Cu, Co, Cr, Fe, Mn
With slots for: optic for each tube type)
• A beam attenuator or a
beta-filter
• Soller slits
• A beam mask holder
Optional additional anti-
scatter slit holder

X‐ray lens (polycapillary) Monocapillary Hybrid monochromator Bartels monochromator

Crossed slits PDS FDS Johansson monochromator


18 19

Mirror-based multipurpose Accessories for mirror optics


iCore Bragg-Brentano HD
(BBHD) Parallel beam mirror Focusing mirror Incident beam kits for GISAXS Microbeam masks Microbeam collimator

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)

iCore Bragg-BrentanoHD Parallel beam mirror Focusing mirror


20 21

4 Diffracted beam optics For basic powder diffraction


dCore Fixed receiving slit module Fixed anti-scatter slits Programmable anti-scatter
(FRS) (FASS) for 1D and 2D slit (PASS)
detectors
Knowing the optical path of the X‐ray beam towards In addition, if you’re thinking of frequently switching Works with iCore to form Classic fixed receiving slit Large range of pre-aligned Two independent motors
and away from your sample is the key to collecting and between different types of specialist experiment, or you the full MultiCore automated modules anti-scatter attachments are enabling beam offset
understanding a diffraction pattern. need to widen the scope of measurements available in measurement suite available for each detector selection
your batch-process, you may find that a dual arm will Has slots for:
The diffracted beam optics, between the sample and Comprises: • Beam attenuator or beta Slots for: Works in three modes:
detector, must be carefully matched with the incident make life easier.
• Four-mode programmable filter • Beta-filters • Fixed anti-scatter slit
beam optics to ensure that only the cleanest and most anti-scatter slit (PASS): • Fixed receiving slit • Anti-scatter shielding mode, in eight sizes from
relevant signal is detected. We’ll help you to choose • Fixed anti-scatter slit • Soller slits or beam mask tubes 1/32° to 4°
between the numerous options, including programmable mode offers eight sizes holder • Slits • Automatic mode, from
anti-scatter slits, collimators, attenuators, Soller slits, from 1/32° to 4° • Detector mounting plate • Masks 0.5 mm to 20 mm in steps
monochromators, and more. • Automatic mode offers • Soller slits of 0.1 mm
Options:
sizes from 0.5 mm • Fixed anti-scatter slit • Follow mode, matching
to 20 mm in steps of (FASS) the detector active length
0.5 mm • Curved-crystal or flat- (for quasi-parallel beam
• Follow mode (for crystal monochromator applications)
quasi-parallel beam PASS available for any of
applications) matches the 1Der, PIXcel1D or PIXcel3D
the detector active detectors
length
• Open mode stays open
• Two Soller slits:
0.02, 0.04 rad
• Two parallel-plate
collimators: 0.11°, 0.28°

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.
22 23

For specialized methods


Parallel plate collimator PreFIX 3-bounce or Diffracted parallel beam Diffracted beam crystal
5 Detectors
2-bounce 3-axis analyzers (parabolic) mirror (Cu, Co) monochromators
Receiving slit optic for 0D 3-bounce or 2-bounce 3-axis Used in combination with Options:
Whether you’re detecting fast, strong signals or the finest, weakest details, you’ll find what you’re looking for in our range of five
applications using parallel analyzers are used with the a fixed receiving slit or • Flat-crystal
tried-and-tested detectors.
beam geometry as generated incident beam 4-bounce programmable receiving slit monochromators are
from lenses, mirrors or Bartels monochromators Acts as an analyzer for used in parallel beam
double-slit systems and hybrid 2- and 4-bounce applications Detectors
parallel beam applications
Choice of 3 equatorial monochromators that use an incident parallel • Curved crystals are Type 1Der PIXcel1D and GaliPIX3D Proportional Scintillation
acceptance options: 0.09°, Reduces the detector beam mirror or hybrid used in Bragg-Brentano PIXcel3D detector detector
geometry (Medipix 3)
0.18° or 0.27° acceptance angle down to monochromator
12″ for ultra-high-resolution • Monochromator for PIXcel Window size 9 mm × 15 mm 14 mm × 14 mm 30 mm × 24 mm 20 mm × 24 mm 30 mm diameter
Slots for Soller slits and Provides a higher intensity detector with Cu radiation
masks and beta filter measurements of fine than a 3-bounce or
Built-in 0.8 mm detector slit Pixels/strips 1 × 128 256 × 256 502 × 466 — —
structure around strong 2-bounce analyzer
Slot for 0.1 mm collimator slit single-crystal peaks, or fine Factory aligned to diffract a Mode 0D, 1D 0D, 1D (PIXcel1D) 0D‡, 1D, 2D, 3D 0D 0D
for reflectometry scattering signal around specific wavelength 0D, 1D, 2D, 3D
Options: direct beam (PIXcel3D)
• Flat-crystal Slots for slits and masks
monochromator Strip width 70 µm 55 µm 60 µm — —
Slit rotation capability
2D pixel size — 55 µm × 55 µm 60 µm × 52 µm — —
Point spread — 1 pixel 1 pixel — —
function per pixel
Active length 0.07–9 mm 0.055–14 mm 0.06–30.6 mm — —
range
Smallest step size* 0.0021° 2θ 0.0016° 2θ 0.0018° 2θ — —

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

1Der PIXcel3D GaliPIX3D Proportional Scintillation


detector detector
*
 t 240 mm goniometer radius in scanning mode. † Count rate when PHD levels are 25–80%. ‡ Supported by an inclusive dedicated
A
“Working at the frontier of detector technology has always been very exciting and 0D detector

motivating. With the dedicated detector group of Malvern Panalytical we have


celebrated many successes: the introduction of the photon counting solid state strip
detector and hybrid pixel technology. This has led to improvements in measurement 1Der detector energy resolution
speed, data quality and has opened the door to many new applications”
Tube anode material Typical energy resolution (eV) Energy resolution %
Cr 270 < 5%

dr. ir. Roelof de Vries Co 320 < 5%


Group Leader Detector Development Cu 340 < 5%
Mo 390 < 3%
Ag 440 < 3%
24 25

6 Software Data analysis


HighScore HighScore independently performs data treatments and XRD phase identification on any powder
diffraction data
It includes:
Empyrean software has two functions:
• Search-match algorithm using peak and profile data
• The instrument control software provides a single interface from which you can control all experiments and system • Graphics for examining, displaying, and editing diffractograms
settings, as well as export and manipulate XRD data • Referenced Intensity Ratio (RIR) and Direct Derivation Method (DDM) for estimation of quantities
• The data-analysis software provides everything you need to interrogate your results, starting with programs for of identified phases
in-depth analysis of individual results or large sets of results, but also including automation programs to manage • Percent crystallinity via External Standard, Internal Standard or PONKCS method
batch analysis or even batch measurement-and-analysis. Should you wish, we can also interface the software to • Full pattern as well as peak based (Williamson-Hall Plots) size/strain analysis
integrate measurement and analysis routines into a LIMS system and/or a regulated environment • Multivariate Data analysis, like Cluster Analysis, Principal Component Analysis,
Metric Multi-Dimensional Scaling and t-SNE
• Partial least squares quantification of a property directly from raw data
Instrument control and data manipulation • Total scattering data normalization for Pair Distribution Function analysis
• Supports commercial (ICDD, CSD), free (COD) and user-defined reference databases
Data Collector This data acquisition and instrument control software is included with every Empyrean
• Batch feature for automated running of a sequence of actions
system
• Automated launch from a command prompt
Provides measurement strategy determination tools, configuration and measurement
management (manual and automated batch measurements), automatic processing, data HSvu is the free app to view XRDML’s and HPF’s on Android and iOS
conversion and viewing functionality for X‐ray diffraction systems
HighScore Plus HighScore Plus is a powerful option for HighScore, which enables:
The automatic processing (APP) function included can interface with third-party
• Rietveld, Le-bail, HKL-file, Pawley, and profile fit for quantitative phase (and amorphous) analysis
software, therefore enabling data-collection and analysis procedures to be run
• Indexing, unit cell refinement and Space group determination via ExtSym Extinction Analysis
automatically
• Structure solving with charge flipping and (Difference) Fourier maps with 3D Electron density as
Data are saved in XRDML format, readable by many text editors. In combination with well as 3D structure display
APP, data format conversion and archiving can be automated • Inclusive Scripting IDE to create and run script programs with or without user interface
• A large number of supporting functions for data correction, manipulation and simulation of
OmniTrust OmniTrust combines OmniAccess, for flexible configuration, with OmniTrail, an audit trail
diffraction patterns
viewer for routine and regulatory audit trail reviews
• Smart batch feature allows intuitive definition of data processing, and refinement in a linear or non-
OmniTrust enables audit and security functions for Data Collector and Data Viewer, to linear sequence (using a logic tree)
aid technical compliance (to regulations such as 21 CFR part 11) and data integrity • The flexible and powerful tools enable fully automated MS Office reporting and results exporting
PANViewer PANViewer is a software package for visualization, reporting and replaying of 2D
diffractograms and radiographs of computed tomography measurements HighScore Plus provides a fully comprehensive analytical suite for all aspects of crystallography and
crystallographic phase characterization.
PANViewer can also export 2D diffraction data in other file formats common in XRD
Roboriet RoboRiet is dedicated software for the complete automation of Rietveld analysis in a production
Document settings can be stored for future use in PANViewer file format
environment, and offers operator feedback without the possibility to influence the process
XRD2DScan XRD2DScan prepares 2D microdiffraction data for further analysis, by converting 2D
The software reacts to the presence of a scan fulfilling certain conditions, and can run in the
data into 1D data based on predefined areas
background without the risk of influencing the ongoing measurements
The software can also perform mathematical operations on 2D data and provides
various analysis tools
Powder diffraction databases (ICDD)
To complete your phase and structure analysis, we can supply ICDD PDF databases as part of your full configuration

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-
leading precision measurements group. • Sample and application consultancy

Copyright: © 2021 Malvern Panalytical. This publication or any portion thereof may not be copied or transmitted without our express written permission. PN12895
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Worcestershire, WR14 1XZ, 7602 EA Almelo,
United Kingdom The Netherlands

Tel. +44 1684 892456 Tel. +31 546 534 444


Fax. +44 1684 892789 Fax. +31 546 534 598

www.malvernpanalytical.com

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