Research Grade XRD Specifications.pdf

Minimum Specifications for Research Grade Multi-Application X-ray Diffractometer

The multi-application x-ray diffractometer (XRD) instrument hardware and software must support the following types of analysis:

Powder diffraction (XRPD) using Bragg-Brentano parafocusing geometry and a linear position sensitive detector for faster measurements including Rietveld quantitative analysis

Non-ambient XRPD in gas environments at temperatures up 900°C and pressures up to 100 bar using air, inert gas, hydrogen, oxygen, and carbon dioxide.

Grazing incidence X-ray diffraction (GIXRD) using asymmetric Bragg diffraction measurements Residual stress analysis using iso-inclination, side-inclination, and multi-hkl techniques Texture analysis using pole figure measurements Symmetric and asymmetric high-resolution rocking curve (RC) measurements of epitaxial thin films X-ray reflectometry (XRR) of films ranging in thicknesses from 2 nm to 200 nm multilayers Symmetric and asymmetric reciprocal space maps (RSM) using conventional triple-axis measurements and using faster single-pass mapping with an area detector Diffuse scatter analysis of off-specular reflection (resonant diffuse scattering) and diffuse intensity distribution in reciprocal space around a Bragg reflection Computed tomography (CT) analysis of small specimens and polymers at moderate resolution Microdiffraction analysis with moderate spatial resolution (X-ray spot size >1mm) Spinning capillary geometry XRPD to minimize preferred orientation in minerals, zeolites, and other inorganic materials 2D XRD using a scanning area detector for analysis of grain size and texture using Debye diffraction rings Pair distribution function (PDF) analysis of inorganic materials

X-ray diffractometer (XRD) base system minimum configuration

Minimum XRD instrument specifications:

Cabinet/radiation enclosure:

Cabinet must completely enclose system and prevent exposure to direct and scattered x-ray radiation Must comply with all United States federal x-ray safety requirements Must be able to safely utilize typical radiation x-ray tubes (Cu, Co) as well as hard radiation x-ray tubes (Mo, Ag) No user operations are allowed to require safety interlocks to be overridden Must include a minimum of two 19 inch electronic rack positions for accessory controllers Cabinet must have easy access to install/remove accessories and samples

Goniometer:

A vertical circle Theta-Theta goniometer is required. (The sample stays horizontal for most scanning routines - 2 theta-omega scans). Independent control of 2-theta and omega axes is required as well to allow other scan types (grazing incidence, transmission, etc.)

The goniometer must have optical encoder control, omega and 2-theta step resolution of 0.0001°, at least a ≤-3 to ≥ 160 °2θ scan range, linearity of ±0.01 ° or better, and maximum scan speed of at least ≥60 °/minute

Generator:

The system must have a generator with a minimum power output of 4.0 kW and have all primary operating parameters controlled by the system computer/software. It must also support the use of Mo and Ag x-ray tubes (≥60 kV).

X-ray sources:

Required x-ray sources: Sealed tube sources required. Rotating anode sources are not acceptable due to increased maintenance costs and complexity o Must include a high-resolution Cu x-ray tube providing a stable focus spot for use with x-ray mirrors, and monochromators for general XRPD and thin film analyses o Must include a high-resolution Mo x-ray tube for hard radiation applications including

Transmission through Anton Paar HPC 900 or equivalent high pressure chamber windows

Transmission through a capillary with diameter 0.5 to 1mm containing inorganic samples

Pair distribution function (PDF) analysis to a Qmax of at least 17 A-1 Computed Tomography measurements of inorganic samples and structures

Changing the X-ray tube, breeding the tube and re-aligning the system must be a task that can be accomplished by an adequately trained operator in less than 2 hours.

Breeding times must be specified for various situations (type of source, down-time of source) and breeding protocols available in the instrument software

Must include a chiller with an air-cooled condenser with a cooling capacity appropriate for the base XRD system and all accessories. Must be equipped with manual shut-off valves and all necessary hardware for installation

Optics:

For general ease of use by typical operators, the instrument must include a configuration that allows software selectable, automated changing of modes to enable a variety of analyses without the physical changing of optical components by the operator. This requirement applies to both the incident- and diffracted-beam paths and includes switching between 0D, 1D and 2D measurements. The automated configuration must support the following analyses:

XRPD analysis with Bragg-Brentano parafocusing geometry:

Fixed- or variable-divergence slit measurement Computer control of masks/slits and Soller slits to vary the X-ray beam axial divergence and width

Monochromator (such as curved graphite monochromator or flat mirror) to reduce Cu K-beta, Bremsstrahlung, and W L-alpha radiation

Scanning linear (1D) detector for fast data collection Parallel-Beam geometry for GIXRD, XRR, and residual stress analysis

Computer control of masks/slits and Soller slits to vary the X-ray beam axial divergence and width

Computer controlled switching to diffracted-beam parallel-beam optic and point (0D) detector

Point or pseudo-point focus geometry for microdiffraction, residual stress, and pole figure analysis Computer control of masks/slits and Soller slits to vary the X-ray beam axial divergence and width to <1mm 2D diffraction

Computer control of masks/slits to produce a point or pseudo-point focus X-ray beam with axial width to <1mm

Computer controlled switching of diffracted-beam path to area (2D) detector with full field of view (ie. no Soller slits, large anti-scatter slit, etc.)

High-resolution for rocking curve and reciprocal space map analysis of epitaxial thin films Monochromated K-alpha1 diffraction Resolution (FWHM) of 35 arcseconds or less as measured from Si (111)

Additional optics requirements: The instrument must include optics optimized for hard radiation sources (Mo or Ag x-ray tubes). The incident-beam optic must be a focusing mirror or equivalent that delivers consistent resolution (FWHM) for any capillary diameter from 0.3 to 1 mm when using a linear (1D) scanning detector. The instrument must also include shielding to produce low background noise necessary for PDF analysis. The instrument must include optics for CT analysis of samples up to 25 mm diameter

The instrument should include additional optics for high resolution analysis of epitaxial thin films (rocking curve, reciprocal space map), including

High resolution analysis with ≤22 arcsecond resolution (FHWM of Si (111)) Fast, single-pass RSM measurement using area detector. Example <10 min RSM of (224) film and substrate peaks from NIST2000 SRM with a single scan

Detectors:

The system must include a suite of highly efficient detectors to support all of the various analytical techniques and stage use detailed herein.

Hard radiation detector (Mo, Ag):

The instrument must include a detector for hard radiation with the following capabilities: ≥99% detection efficiency for a Cu anode and hard radiation (Mo or Ag anodes) enabling fast measurements;

Linear (1D) and area (2D) measurements in both static and scanning modes; ≤100 x 100 μm pixel size for adequate resolution; capable of a very small size (<0.015 °2θ when collecting a static 2theta measurement); maximum count rate of ≥1011 cps overall; 99% Linearity of ≥109 cps overall; two level energy discrimination with ≤25% energy resolution; detector coverage of at least 11 deg 2-theta in static linear (1D) mode with the high pressure chamber (HPC 900 or equivalent, as described above) and high temperature sample stage for time-resolved in-situ analyses

Must include all accessories and hardware for mounting the detector and operating the detector, including if required, a separate water chiller and dry air supply

Must include a full set of slits for the detector and all alignment slits needed Must include an anti-scatter slit holder and slits for suppression of scattered x-rays from the windows of non-ambient sample chambers when they are used in conjunction with the detector Must include any necessary hard radiation accessories not included in the base XRD system Must include a focusing mirror for Mo radiation.

Standard detector(s) (Cu, Co radiation):

The instrument must include a single detector or multiple detectors mounted simultaneously capable of supporting the automated multipurpose optics described above, including point (0D), linear (1D) and area (2D) measurement modes. This detector(s) must have the following minimum specifications:

≥99% detection efficiency for Cu radiation; Linear (1D) and area (2D) measurements in both static and scanning modes; ≤100 x 100 μm pixel size for adequate resolution; capable of a very small size (<0.015 °2θ when collecting a static 2theta measurement); maximum count rate of ≥1011 cps overall; 99% Linearity of ≥109 cps overall; two level energy discrimination with ≤25% energy resolution

Must include all accessories and hardware for mounting the detector(s) and operating them Must include a full set of slits for the detector and all alignment slits needed Must include an anti-scatter slit holder and slits for suppression of scattered x-rays from the windows of non-ambient sample chambers when they are used in conjunction with the detector

The instrument must include a detector capable of supporting fast single-pass Reciprocal space mapping (RSM). Example <10 min RSM of (224) film and substrate peaks from NIST2000 SRM with a single scan

Prefer the adaptation of NETL’s current Panalytical X’celerator detector for use with the new system

Sample stages:

Automatic sample changer and spinner:

The instrument must include a sample spinner stage and changer capable of automated exchange of a minimum of 15 samples. A minimum of 15 sample holders for powders must be included. It is preferred that the sample changer is able to utilize the sample holders currently owned or that 6 zero background sample holders be included. The sample spinner stage and changer must accommodate a beam knife to improve low angle background with a linear detector (1D)

General purpose sample stage:

A sample stage capable of holding and positioning monolithic samples must be included. The stage must be capable of accommodating samples up to 10 cm diameter, 10 cm height, and weighing up to 10 kg. It is preferred that the stage is automated and controlled by the system computer.

Eulerian cradle:

The instrument must include a Eulerian cradle that can accommodate samples up to 140 mm diameter, 60 mm thick and 2 kg mass. It must have motorized chi (tilt), phi (rotation), and z (sample height) for residual stress, texture, XRR, RC, and RSM analysis.

High pressure/temperature stage - Anton Parr HPC900 High pressure reaction stage (or better):

Must include a high pressure, high temperature reaction stage for powder samples (temperature, 25 to 900 degrees C, pressure, ambient up to 100 bar with the acknowledgement that the upper temperature limit will be determined by the specific gas used; 900 C in helium or hydrogen and 500 C in air, inert gas, or oxygen; heating rate 1 to 60 C per minute) with controller. Gases to be used include air, nitrogen, helium, carbon dioxide, oxygen, hydrogen.

Must allow basic grazing incidence studies Must include sample holders Installation materials must be included Base XRD system must be capable of providing the required cooling water supply for heating stages

Very high temperature stage - Anton Parr HTK 2000N high temperature stage (or equivalent):

Must include a very high temperature sample stage capable of heating a sample to >1500C in air, inert gas or vacuum and >2000 C in vacuum

Thin film analysis accessories:

Must include a high intensity diffracted beam assembly (rotatable slit holder, two-bounce Ge

(220) asymmetrical monochromator with an acceptance of 0.005 degrees, height slits 1 deg., ¼ deg., 1 mm, width slit 1mm)

Must include high-level software for operation and data analysis (analyzing single and 2-axis scan data; calculations for rocking curves, specular reflectivity, reciprocal space maps to determine mismatch, composition, thickness and relaxation. Sample thin layers including single and textured polycrystalline layers as well as amorphous films

Capillary spinner stage for use with Mo x-rays:

Must include a sample stage with spinner and goniometer head for the mounting of capillary samples within the instrument (Minimum: X and Y movement +/- 3 mm, height adjustment 3 mm, tilt angles X +/- 20 degrees, y +/- 17 degrees)

Must include an initial set of sample capillary tubes Must include a capillary pre-alignment device so that capillary samples can be aligned prior to mounting in instrument

Computed Tomography (CT) Capability:

System must include a sample stage for CT analysis of samples up to 25 mm diameter. The system must also include an appropriate detector and any other necessary components needed to acquire medium resolution scans of organic and inorganic samples in a reasonable time frame

Additionally:

System must include an alignment camera with software with the capability of saving images to the system computer

Must include a dial gauge for sample alignment Must include updating/adapting NETL’s current Anton Parr HTK 1200 hot stage for use with the new system

Computer workstation and components:

Must include a state-of-the-art PC workstation (minimum 64 bit Microsoft Windows 10 pro operating system, 8 GB ram, 2 TB HD)

Must include Microsoft Office Home and Business 2019 or current version Must include necessary network cards for all components/accessories

Software:

The XRD system package must include all software required to operate the XRD system, execute all of the diffraction experiments detailed above as well as analyze the data produced. Required software includes:

XRPD analysis including phase identification and quantification, profile fitting, Rietveld refinement, indexing, line profile analysis (crystallite size and microstrain), charge flipping, PONCKS (for amorphous quantification)

Statistical analysis of diffraction data using cluster analysis and partial least squares refinement

(PLSR)

Calculation of pair distribution function (PDF) from experimental data

Epitaxial thin film analysis, including analysis of epitaxial film mismatch, composition, thickness, and relaxation using rocking curve and RSM data as well as simulation and automatic fitting of rocking curves

XRR analysis of thin films, including analysis of thin film thickness, density, and roughness using XRR and simulation and automatic fitting of reflectivity curves

Software for treatment of 2D diffraction data, including integrating 2D data into equivalent 1D data as needed for XRPD analysis, producing pole figures from 2D data and grain size analysis based on 2D data

Software for residual stress analysis of data collected using side-inclination, iso-inclination, and multi-hkl techniques

Software for texture analysis of pole figures Software for CT reconstruction and analysis Software must be able to read and utilize existing Panalytical XRDML data files

Shipping, installation, training, support and warranty:

Must include insured shipping to NETL, Pittsburgh Must include installation by a factory trained installation engineer(s) Must include a pre-installation site survey to ensure installation location is prepared appropriately Must include a Factory Acceptance Test to verify that the system is meeting factory performance specifications Must include a minimum one-year system warranty covering all components including third party components Must include one preventive maintenance visit within the warranty period Must be able to provide on-site support within 2 business days in response to instrument outage and must provide remote applications support and remote service support free of charge Must include decommissioning, removal and proper disposal of existing x-ray diffractometer system (Panalytical X’pert Pro), cabinet and associated hazardous materials Must include a minimum of 8 hours (can be spread over multiple days) of expert delivered in-depth on-site training for up to four instrument users covering the base XRD system and all accessories and applications (XRPD, RC, RSM, XRR, CT, PDF, Texture, Stress, microdiffraction, and use non-ambient and high-pressure and high-temperature stages). If more than 8 hours is necessary, additional time will be included as required. Travel and lodging will be included.