PR 1300909664 -- Minimum Technical Specifications.pdf

PR 1300909664— HIGH RESOLUTION GRAZING INCIDENCE THIN FILM DIFFRACTOMETER Page 1 of 5

MINIMUM TECHNICAL SPECIFICATIONS

HIGH RESOLUTION GRAZING INCIDENCE THIN FILM DIFFRACTOMETER

I. INTRODUCTION

The Naval Research Laboratory has a requirement for a High-Resolution Grazing Incidence Thin Film Diffractometer, Washington, DC. This system will be used to measure the structural properties of materials under controlled temperature conditions and automatically map properties at ambient conditions across standard 4” semiconductor wafers. The system must allow for safe and easy operation for the users and other occupants of the facility.

Used equipment in whole or in part is not acceptable in the purchase of this system.

The primary components of the system include X-ray source, Goniometer, Optics, Sample stages, Non-ambient sample stages, Detectors, Measurement/ Application software.

II. GENERAL REQUIREMENTS

• The system completely houses electronics, generator, and goniometer in one unit.

• The system shall be able to accommodate an internal cooling unit.

• The system must support network/internet based remote operation/maintenance.

• The system must provide a computer based on a Windows 10 operating system for instrument control and data processing.

• The system must provide alignment-free switching of all beam path components including X-ray tube, all optical components, all sample holders (ambient and non-ambient), and all detectors.

• The system must be capable of fully automatic, motorized switching between Bragg-Brentano, parallel beam, and high resolution XRD (monochromator) geometry without the need of touching the instrument.

• The system must have true plug and play functionality by fully automatic, real-time component recognition and configuration as well as conflict detection for all beam path components.

III. PRIMARY COMPONENTS

A. X-RAY SOURCE

X-ray source must be rotating anode-based generator in order to achieve highest intensity.

The rotating anode X-ray generator must fit in the diffractometer cabinet and must be fully integrated into the measurement software.

The rotating anode X-ray generator must have at least 5 kW capability.

The system must support the kV and mA settings that can be continuously adjustable via software.

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The measurement software must support automatic startup for X-ray tubes for maximum lifetime and an automatic burn-in routine for new X-ray tubes.

The rotating anode must deliver a focal spot brightness larger than 5.5 kW/mm2.

Available X-ray tube anodes shall include Cr, Co, Cu and Mo radiation.

The system must provide fully automated, real-time recognition and configuration of all X-ray tubes.

Two Cu anode assemblies must be included.

B. GONIOMETER

The goniometer must be vertical with theta-theta geometry.

The goniometer must be equipped with independent stepper motors and optical encoders on both goniometer circles (Tube- and Detector-side).

The goniometer must have an angular range of 360° (without accessories).

The goniometer must have minimum angular measurement range of -110° < 2theta < 160° (depends on accessories).

The goniometer accuracy is equal or better than +/- 0.007° 2theta over the entire angular range.

•The goniometer must be vertical with theta-theta geometry and must have an additional axis to rotate the detector arm out of the coplanar geometry. This 3-circle goniometer enables application in non-coplanar geometry, e.g. in-plane diffraction experiments.

The position of the axis of the non-coplanar arm shall be controlled by a direct angular encoder which has a resolution better than 0.002°.

The minimum step size of the non-coplanar arm should be equal to or better than 0.001°.

The positioning accuracy of the non-coplanar arm should be equal to or better than +/- 0.003°.

The track of the non-coplanar arm should be equipped with a distance-detection system for the automated determination of the detector position

The accessible angular range of the non-coplanar arm must be -3°< 2Theta(nc) < 150°.

The sample-to-detector distance on the non-coplanar arm must be variable continuously with a possible maximum distance of more than 350 mm.

Angle positioning: Stepper motors with optical encoders for optimum scanning speed and positioning precision

Minimum angular speed: 20°/s

The minimum step size shall be 0.0001°

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The reproducibility shall be +/- 0.0001°

C. OPTICS

One optic module to provide switching between a) motorized slit for powder diffraction, b) mirror (parallel and focused beam) for grazing incidence diffraction or Reflectometry and c) a high-resolution beam path consisting of mirror and 2-bounce channel-cut monochromator must be fully software-controlled. No alignment is required when switching between these beam paths.

Axial and Equatorial soller slits for Bragg Brentano powder diffraction and beam conditioning for in-plane grazing incidence diffraction.

The 4-bounce monochromator must be included in the system and its beam divergence must be less 0.0035 degrees.

Large FOV Equatorial and Axial soller slits (0.1 mm – 1.0 mm) at least 20 mm x 20 mm in size for GID and IP-GID measurements.

The system must provide collimators longer than 70 mm with various diameters (0.1, 0.3, 0.5, 1.0 mm) and these collimators can be mounted at the optical bench with motorized absorber carousel with 4 positions.

Exchange of all optics must be tool-free using a snap-lock mechanism.

The system must offer fully automatic, real-time recognition and configuration as well as conflict detection for all optical components.

D. SAMPLE STAGES

The system stage must be a Centric Eulerian Cradle with motorized X-Y-Z, Chi and Phi drives. This stage must accommodate domed non-ambient stages without losing any translational functionality.

X-Y drives at least 80 mm and Z drives at least 1 mm.

Chi drive: > 90 degrees

Phi drive: Unlimited rotation

Maximum sample height must be at least 30 mm.

The system must provide a 5” vacuum chuck stage that can be enable unlimited rotation of phi.

The system must offer a motorized tilt stage with at least +/- 5 degrees tilt in orthogonal directions which allows sample normal to be aligned for IP-GID measurements.

A small film stage with a single vacuum opening to accommodate very small sample (<5 mm) without contributing to background.

All sample stages can be exchanged without alignment.

System must offer ambient stage that can hold a standard 4” semiconductor wafer

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E. NON-AMBIENT SAMPLE STAGES

The supplier must be able to offer non-ambient chambers. for low- and high-temperature measurements.

Non-ambient sample stages must be fully integrated into the supplier’s measurement software. The following parameters must be controlled by the software: Heating, cooling, humidity, sample rotation, sample height adjustment, as applicable.

All sample stages can be exchanged without alignment.

The system must include a cooling stage for measurement to liquid nitrogen temperatures. This stage must include at least two extra electrical feedthroughs to apply an E-field to the sample. Stage must operate from liquid nitrogen temperature (-180C) to above room temperature (500C) in a high vacuum environment.

The system must include a heating stage for measurements to higher temperatures in a vacuum environment with fully integrated (non-modular) heating filaments from 25C to 1100C with a sample sized at least 10mm x 10mm x 2mm.

F. DETECTORS

The system must offer fully automatic, real-time recognition and configuration of all detectors. Only 1 detector required for all applications for ease of use and efficient reconfiguration.

• The detector must be 0D/1D/2D position-sensitive detector based on hybrid photon counting pixel technology for Cr, Co, Cu, Mo and Ag radiation.

• Active area must be at least 2,500 mm^2 to capture all scattering features in diffraction space.

• Pixel size of the detector must be <100 microns to achieve sufficient resolution.

• The detector operation must be media-free, and does not require water-cooling or pressurized dry-air purge.

• The sample-to-detector distance must be variable continuously with a possible maximum distance of more than 370 mm to optimize angular resolution versus coverage.

• Detector position must be automatically recognized in real-time by the software and the corresponding calibration files must be automatically selected.

• A single detector mount must incorporate the functionality to rotate the detector, tool-free, in order to optimize angular coverage in gamma direction or 2Theta direction, and must recognize the detector orientation in real-time.

• The detector shall provide more than 500,000 pixels.

• The detector must offer a count rate capability higher than 3.5 x 108 ph/s/mm².

• The detector must be able to combine with axial Soller collimators wider than 75 mm in 2Theta direction for high quality, high speed data collection in 1D mode.

The axial Sollers can be mounted tool-free and recognized in real-time.

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G. MEASUREMENT AND APPLICATION SOFTWARE

• The measurement software must have a graphical instrument representation for real-time display of the actual instrument configuration based on component recognition, real-time validation and conflict detection, and measurement planning (definition of instrument parameters such as slit settings, selection of optical components, and selection of diffractometer geometry.

• Software should support variable measurement parameters such as variable counting time, variable step-size, simultaneous variable counting time and variable step-size support.

• Support graphical interpretation of phase, RSM and XRR mapping of a 4” wafer.

• Software should be able to control measurement position across full 4” sample stage.

• Automated data fitting of XRR data via graphical user interface that is integrated with stage position via motion control software.

• Software should support Rietveld/Whole powder pattern fitting analysis.

IV. REQUIRED APPLICATIONS

The diffractometer, with measurement and application software packages, shall be configured for all diffraction-based material research applications including:

Qualitative and quantitative phase analysis and phase identification Ab-initio crystal structural determination and refinement X-ray Reflectometry Grazing Incidence Diffraction In-Plane Gracing incidence Diffraction Gracing Incidence Small Angle X-ray Scattering High-Resolution X-ray Diffraction Reciprocal Space Mapping Microdiffraction Stress and Texture Analysis XRD measurements at non-ambient conditions (variable temperature and humidity)

V. INSTALLATION AND TRAINING

The contractor shall install the system at Naval Research Laboratory (NRL). The vendor must provide a facility work requirement sheet, including electric power, system cooling water and process gas and gas lines with its proposal.

The contractor must provide two (2)-days, on-site training, for two people, after installation.

The contractor shall also provide two (2)-days, off-site training courses, for two people, to explain all applications, within 5 years from installation date.