CLS_X-Ray_Diffractometer_Specs.pdf

MADN-CHM-LS 21 March 2016

MEMORANDUM FOR Directorate of Contracting, United States Military Academy, West Point, NY 10996

SUBJECT: Specification for X-Ray Diffractometer.

This specification describes the minimum capabilities of X-ray diffraction equipment to be provided. The required functionality includes but is not limited to the following;

Phase identification

Crystallographic analysis

Percent Crystallinity

Crystallite Size/Microstrain

Rietveld Analysis

Search/Match with PDF-2

High Temperature diffraction option

Transmission diffraction

SAXS and GSAXS Small Angle X-ray Scatter

Grazing Angle

Some of the aforementioned applications might require optional equipment, but the contractor must offer that equipment at the time the system is delivered.

The system being offered should have the following features/functionality

PHYSICAL

As this is a solicitation for a replacement, it is required that new unit fit in same footprint and not require additional utilities

Dimensions (excluding computer): not to exceed 45”Dx55”Wx80”H in any dimension.

Electrical: 208VAC, 60A

If Chilled water is required, contractor will supply chiller/heat exchanger

Dimensions: not to exceed 36”Dx24”Wx36”H in any dimension

208VAC, 20A

Contractor will provide equipment to condition air, if required.

DEPARTMENT OF THE ARMY

UNITED STATES MILITARY ACADEMY

West Point, New York 10996

REPLY TO

ATTENTION OF

Contractor will remove existing Philips X’Pert x-ray diffractometer.

Contractor will supply all trucking, moving and rigging service required for removal of existing equipment and delivery of new equipment.

RADIATION AND SAFETY ENCLOSURE

A complete floor standing radiation enclosure must be provided which prevents exposure from either the direct or scattered x-ray beam. The enclosure(s) must meet all local, New York State, and federal X-ray radiation safety requirements for all possible anode types including Copper, Silver, Chromium, Manganese, Cobalt.

A key lock must be present to prevent unauthorized use of the system with power settings readily displayed on the front of the physical instrument.

The enclosure must have large front doors for convenient access to the goniometer optics and sample stages. These doors must lock automatically when the x-ray shutter is open.

X-RAY TUBES AND TUBESTAND

The diffractometer must be supplied with an X-ray tube of the long fine focus design (0.4 x 12 mm) with a maximum loading of 1.8 kW. The tubes shall have a copper and shall have ceramic insulation that provides superior focal stability over glass tubes.

The tube must be manufactured by the supplier of the diffractometer (for total system responsibility) and have self-contained water lines for superior temperature control and stability.

Tube design must allow the physical rotation of the X-ray tube body that results in the anode surface being rotated from line projection to point projection as required for utilization of maximum X-ray tube flux in either line or point modes. Change of anode surface projection should be easy to accomplish even by inexperienced users in under 5 minutes without the need for realignment of the tube, optics or goniometer either manually or via computer and not require interruption of water flow to the tube itself during any part of the change.

Separate from the generator, the X-ray tube must include an electronic chip that specifies the maximum generator settings for the specific source material, identifies the tube anode and serial number automatically to the system software, and records use parameters such as hours of use for a tube.

GENERATOR

The system must include an X-ray generator that is capable of 3.0 kW output power and use ultra-sonic frequency solid state technology with remote computer control and tube recognition. It must allow pre-set kV and mA values to be used for different analytical programs and also allow the user to program a standby setting (minimal kV and mA) when the diffractometer is not being used. Automatic control of all important operation parameters must also be included.

The kV setting must be adjustable to 15-60 kV output in 1 kV steps at a stability of less than 0.01% at mains variation of +/- 10%. The mA setting must be adjustable to

5-60 mA output in 1 mA steps at a stability of less than +/- 0.01% at mains variation of +/- 10%.

Generator will have tube recognition and tube lifetime monitoring. The generator will automatically breed new tubes and set limits to power loading (in coordination with recognition port in the x-ray tube).

GONIOMETER

Diffractometer must be a theta/theta goniometers with a minimum radius of 240mm.

The diffractometer must have independent operation of each theta (omega) axis.

The angular range of the goniometer must be 360degrees in omega without accessories) and -111 to 168 degrees for two-theta depending on accessories.

Minimum step size must be 0.0001 degrees in both omega and two-theta.. Slew speed must be at least 15 degrees per second.

Goniometer must employ DC drive motors and high quality (e.g. Heidenhain) encoders direct optical positioning sensing technology, which provides pin point positioning accuracy and zero backlash. The DC motors and optical positioning technology must be under continuous operation to avoid any possibility of angular drift. Encoders on the motor gears are not acceptable.

OPTICS

Incident beam optics. The incident beam optics must incorporate pre-aligned, fast interchange optics modules for the incident x-ray beam, with each module attached to identical incident beam sub frames (individual). The optics mounting frames must be made of hardened tool steel and remounting of optics must be reproducible to < 3 microns. Interchange of each optics assembly must occur in under 2 minutes by persons who have no knowledge or experience in the alignment of x-ray diffraction optics and without the need for realignment of the goniometer or optics modules.

The exchange of the modules must be accomplished by the loosening and tightening of one screw using one tool. These optics modules must in no way interfere with the exchange of the X-ray tube focus from line to point foci and vice versa. The optics modules described below must be included.

o A programmable divergence slit module. This assembly must have a fixed slit mode with software controlled settings of 1/32, 1/16, 1/8, ¼, ½, 1, 2 and 4 degrees and a continuously variable mode with software controlled settings from 0.5 mm to 20 mm sample irradiation in 0.5 mm increments. Each jaw must be under independent control to allow asymmetric illumination and extremely low angle work (less than 0.5 degrees 2 theta). This module must have a slot to allow for the beta filter to be placed on the incident side. This module is to be used with the line focus tube position.

o A graded multi-layer parabolic mirror module to convert the divergent beam into a quasi- monochromatic and quasi-parallel beam of high intensity. The beam dimensions must be 1.2mm X 20mm. The beam divergence must be less than

0.04 degrees. All accessories and optics devices must be included with this mirror for phase analysis and thin film applications using a parallel plate collimator on the diffracted beam. Low angle slits (1/32, 1/16, 1/8 degree) must also be included. This module is to be used with the line focus tube position.

o Small Angle Scatter Slit. Incident fixed slit for incident beam optic such as mirror, hybrid or focusing mirror to limit the size of the incident beam for small angle scattering experiments

Diffracted Beam Optics. The diffracted beam optics must incorporate pre-aligned, fast interchange optics modules for the diffracted beam arm with each module attached to identical diffracted beam sub frames (individual). The optics mounting frames must be made of hardened tool steel and be reproducible to 3 microns.

Interchange of each optics must occur in under 2 minutes by persons who have no knowledge or experience in the alignment of x-ray diffraction optics and without the need for realignment of the goniometer or optics module. The exchange of the modules must be accomplished by the loosening and tightening of one screw using one tool. The optics modules described below must be available.

o Programmable anti-scatter slit module must be included that operates in fixed slit mode with software controlled settings of 1/32, 1/16, 1/8, ¼, ½, 1, 2 and 4 degrees or in continuously variable mode with software controlled settings from 0.5 mm to 20 mm sample irradiation in 0.5 mm increments. Each jaw must be under independent control to allow asymmetric illumination and extremely low angle work (less than 0.5 degrees 2 theta).

o Parallel Plate Collimator, 0.27 Degrees. Typically, the collimator is a set of parallel plates configured to limit the angular divergence of a diffracted x-ray beam to 0.27 degrees. This has the effect of eliminating defocusing effects which occur during asymmetric diffraction experiments. A 0.1 mm slit for reflectivity measurements is included.

o A full solution for sample fluorescence suppression must be available. An electronic adjustment of the detector PHD levels must be able to be set through the software and a diffracted beam monochromator for a fast linear detector must be available as an upgrade.

DETECTOR System must include a pixilated solid state detector with a maximum pixel dimension of 55 micron. The detector must include the following modes operation, 0D where all pixels are added up to give one intensity, 1D where all pixels in one column are added up to form a position-sensitive detector in one direction (static or scanning measurement modes), 2D where all pixels are read out and displayed independently (scanning or static measurement modes) and 3D where all pixels are read out independently and multiple images are combined to reconstruct the voxels of the image (micro computed tomography). Utilization of both 2D and 3D modes may require the purchase of additional hardware accessories for the collimation of the beam or manipulation of the sample via a sample stage. The detector must include a 97% linear count rate per square mm: 13 million photons/second/mm2 background noise: less than

0.5 counts per second for the whole detector and a dynamic range up to 1010. Detector must be maintenance free and not use detector gases. The detector must utilize pre-aligned, fast interchange technique described in the above optics sections.

SAMPLE STAGES. The sample stages must incorporate pre-aligned, fast interchange sample stages. Interchange between sample stages must occur in under 5 minutes without the need for realignment. The following stages must be included:

Reflection / Transmission Sample spinner which utilizes top referencing of the sample holder mounting for accurate positioning for measurements in either reflection or transmission geometry. The mechanism must place the sample holder precisely in the diffraction plane and not be susceptible to “wobble” as the sample spins. Both the phi position and/or the spin rate must be computer software controlled.

Sample holders must include 3 back loading 27mm, 3 back loading 16mm and sample prep station to allow for easy back loading if sample.

o Capillary holders of 1, 0.7 and 0.5 mm will be supplied o Quartz capillaries of three compatible sizes with above holders will be supplied in quantities of at least 25 each.

o Hand tools appropriate with filling and handling capillaries with capillary hold and sample stage will be supplied.

o Sample holder for powder, solids and fibers allowing for 2D SAXS measurements will be supplied.

SAXS, WAXS GSAXS stage. The sample stage for pre-aligned capillary holders must also accepts a powder holder and a holder for solids.. There should also be a clamp holder for solid samples available. The system must have a SAXS/WAXS stage with an adjustable SAXS slit attachment. The stage must be easily exchanged in just minutes using pre-aligned mechanical mounts when other stages or optics are required. These mounts are consistent with the aforementioned mechanical requirements for the optics mounts.

XRD DATA COLLECTION and ANALYTICAL SOFTWARE. All operational, data collection and analytical software capabilities must be available at the time of bid, with demonstration data or output supplied as requested. Operation and execution of the modules shall be fully multi-tasking within the Windows 7 environment, and shall execute their functions in a seamless manner as presented to the user interface. All operational, data collection, and analytical software should be written and supplied by the instrument supplier in order to maximize long term support and enhancement in future versions, and compatibility with potential hardware upgrades to the specific unit that is purchased. The analysis software must be licensed for installation on up to no less than ten (10) computers at USMA and must not utilize license keys or dongles via hardware or network connectivity.

Data Collector Module: Must contain interactive routines to provide the following functionality for all the optics configuration modes of the instruments:

o Data files stored in open architecture yet secure XML file format.

o Both one dimensional and two dimensional scanning are fully supported. One dimensional angle scans include: - coupled theta-2 Theta scans (gonio) - Omega Scans - 2 Theta Scans - Omega/2 Theta Scans – with cradles, also :Z scans - Psi Scans - Phi Scans Non-scanning angles can be set at arbitrary values. Any one dimensional reciprocal space scan between general values can be performed within the Diffraction plane.

o Also with cradles, two dimensional scans built up from a pair of the possible one dimensional scans may be displayed as an iso-intensity contour plot.

o Automatic peak location and centering of a small list of reflections using the available degrees of freedom.

o Mathematical definition of sample alignment using the orientation matrix notation.

o The orientation matrix can be defined from two or more reflections and the orientation matrix can be revised at any time and may be used to refine the lattice parameters of the sample.

o The orientation matrix is used to locate peaks for measurement and provides complete flexibility for the performance of reciprocal space scans. The orientation matrix is used to create maps of reciprocal space that can be used as a graphical interface to data collection or to construct data collection strategies.

o Data collection with real time display of results can be performed in angle or reciprocal space.

o A manual mode operation is provided to give direct control over the positioning and scanning of individual motors. While in manual mode, the current angular position of the motors is displayed on the computer screen.

Automation Software: Included with the Data Collection module shall be a batch scripting program to automate data collection, data analysis and report generation.

Analysis Package: Analysis software must include full Search Match, Rietveld Structural Analysis, Statistical Cluster Analysis and Full Pattern Quantification by Bish and Chipera method. Cluster analysis is performed based on an Agglomerative hierarchy where scans are put into different classes defined by their similarity. The number of clusters is estimated by the KGS test or by the largest relative step on the dissimilarity scale. Also the most representative scan within each cluster must be determined. PCA (Principal Components Analysis) must then be carried out as a separate and independent method to visualize and to judge the quality of the clustering. The correlation matrix of Agglomerative hierarchy is used as input. The cluster analysis module must be capable of performing cluster analysis on an unlimited number of diffraction scans as well as performing fuzzy clustering on solid solutions and or mixtures. Additionally there are cluster validation techniques available like silhouettes or fuzzy clustering. All Software features specified must be integrated into one program. Separate programs and packages are not acceptable.

Crystallographic Analysis Module: A module to assist in indexing, lattice refinement and Rietveld calculations. Tools for a least two analysis tasks shall be included, being: Crystallography (containing 4 indexing methods, the subsequent unit cell refinement, plus a symmetry explorer and the symmetry reduction); Rietveld (powder or neutron data refinement) running either in automatic, semiautomatic or manual mode, including quantitative phase analysis, crystallite size and microstrain determination, and powder pattern simulation. This module must also contain a crystal structure viewer module, and electron density plotting module.

PDF-2 Database. Powder diffraction data administered by International Centre for Diffraction Data.

COMPUTER. Diffractometer will include a computer system the following minimum configuration is to be included:

OptiPlex 3020 Desktop, 3rd Gen Intel Core i3-4130 Processor

8GB Ram, 1600 MHz

USB Keyboard, USB 2-Button Entry Mouse with scroll feature

Dell Professional P2214H 21.5" Monitor With LED

500 GB HDD

8X DVD+/-RW Combo drive

Windows 7 Professional, 64-bit, English, Factory Install

Microsoft Office Professional

RoHS Compliant, Lead Free Chassis and Motherboard

Energy Star 5.2 Category B compliant CPU

WARRANTY: The X-Ray tube, X-ray mirror and goniometer will have a 78 month (minimum), non-pro-rated warranty. All components will have at least a 1 year warranty. Parts, travel and labor are covered.

INSTALLATION. The installation of the diffractometer system will be performed by a factory trained customer support engineer. A pre-installation manual must be provided to assist the purchaser in the planning of the installation. The customer support department must be available to perform a pre-installation inspection to advice of any pre-installation work which may be required. USMA will install the water recirculator unit.

TRAINING. At least two days of on-site training by a qualified application scientist must be included with the systems. Travel and living expenses must be included. This training shall be separate from any operations training by the service/installation engineer at the time of installation. At least four qualified application scientists must be available from vendor’s domestic office to provide this training.

POC is the undersigned at 938-6837 or James.Balz@usma.edu

James G. Balz Supervisory Chemist