X-Ray Diffraction

The X-Ray Diffraction SEF contains a suite of 7 diffractometers and 1 fluorescence spectrometer for analysis of polycrystalline samples, coatings, epitaxial thin films, nanostructured samples, polymers, and single crystals. The assortment of equipment has been selected to provide flexibility so that we can accommodate a wide variety of research.

PRIMARY CONTACT SECONDARY CONTACT LOCATION
Dr. Jordan Cox
Research Specialist
Office:13-4013
Phone: (617) 253-6887
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Charles Settens, Ph.D.
SEF Operations Manager
Office: 13-4013
Phone: (845) 430-2584
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Instrument Lab: 13-4027
Computer Lab: 13-4041



INSTRUMENTS

Panalytical Empyrean Diffractometer

The Panalytical Empyrean diffractometer has been equipped with a Mo X-ray source, focusing mirror and Galipix 3D detector. An alternate Cu X-ray source, Bragg-Brentano HD mirror and PIXcel 1D solid state detector is also available.
The instrument has multiple different stage configurations:• XYZ stage with auto height sensor

• Capillary spinner with alignment camera
• Reflection-transmission spinner stage with 45 position sample changer
• In-operando coin and pouch cell battery holder

There is also an Anton Paar CHC plus+ in-situ heating and relative humidity stage for sample investigations in humid gas, air, inert gas or vacuum. The heating stage can achieve -5 °C to 300 °C in air or inert gas and up to 400 °C in vacuum. Controlled humidity is possible for sample temperatures from 10 °C to 80 °C.

SOP: http://prism.mit.edu/xray/documents/PAN%20EMPYREAN%20SOP.pdf

Contact: Jordan Cox    E-mail: This email address is being protected from spambots. You need JavaScript enabled to view it.     Instrument Location: 13-4027

Panalytical Xpert Multipurpose Diffractometer

Panalytical Xpert diffractometer is equipped with a 1.8kW Cu X-ray source, Eulerian cradle with chi tilt and rotation, and an X’cellerator Scientific position sensitive detector. It  can be used to collect XRPD, GIXD, XRR, and residual stress data. Some texture analysis is also possible. Sample sizes may be as large as 60mm diameter by 3-12mm thick, though a more typical sample size is 10-20mm diameter. Data collection modes can be changed between high-speed high-resolution divergent beam diffraction and parallel beam diffraction. There are several accessories for this instrument, including an X'Celerator position sensitive detector, an Anton Paar HTK1200N furnace for in-situ high temperature measurements (25°C to 1200°C), an Oxford Phenix liquid helium cryostat for in-situ low temperature measurements (25°C to -262.15°C), a diffracted beam monochromator, and a 15-position automatic sample changer.

Info: http://prism.mit.edu/xray/instruments/xpert.html

SOP: http://prism.mit.edu/xray/documents/PAN%20OEC%20SOP.pdf
SOP: http://prism.mit.edu/xray/documents/PAN%20Changing%20Furnace%20and%20OEC%20SOP.pdf
SOP: http://prism.mit.edu/xray/documents/PAN%20Furnace%20SOP.pdf
SOP: http://prism.mit.edu/xray/documents/Using%20Furnace.pdf
SOP: http://prism.mit.edu/xray/documents/PAN%20SOP%20for%20changing%20Sample%20Changer%20and%20OEC.pdf
SOP: http://prism.mit.edu/xray/documents/PAN%20SampleChangerSOP.pdf

Contact: Jordan Cox    E-mail: This email address is being protected from spambots. You need JavaScript enabled to view it.     Instrument Location: 13-4027

Rigaku Smartlab Multipurpose Diffractometer
This diffractometer features a 9kW rotating anode X-ray source, which produces a much higher intensity beam than sealed tube anodes. It is capable of performing most common XRD measurements as well as many uncommon ones, and can rapidly switch between various optical configurations including both Bragg-Brentano and Parallel-Beam geometries. It is suited for XRPD, XRR, GIXD, HRXRD, reciprocal space maps (RSMs), in-plane pole figures, and in-plane grazing incidence XRD scans. Accessories for this instrument include:

  • Incident-beam Ge (022) double bounce monochromator, diffracted-beam graphite monochromator
  • D/teX Ultra linear position sensitive detector furnace, capable of heating to 1400°C in air, inert gases, or vacuum
  • Capillary stage used to hold and spin capillaries of various diameters for data collection in transmission mode
  • 4 inch XY translation stage used as an automatic sample changer
  • In-situ battery cell designed to charge and discharge Li-ion based battery materials in-situ.
  • In-plane arm which allows the point detector to traverse more than a quarter hemisphere around the sample

Info: http://prism.mit.edu/xray/instruments/smartlab.html

SOP: http://prism.mit.edu/xray/documents/SmartLab%20XRPD%20SOP.pdf
SOP: http://prism.mit.edu/xray/documents/SmartLab%20HRXRD%20SOP.pdf

Contact: Jordan Cox    E-mail: This email address is being protected from spambots. You need JavaScript enabled to view it.     Instrument Location: 13-4027

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Bruker D8 High Resolution Diffractometer
Bruker High Resolution diffractometer uses a conventional 1.6kW sealed tube copper anode, and the X-rays are reflected off a parabolic graded multilayer mirror to produce a parallel beam. This instrument features a four-bounce Ge (022) incident beam monochromator. This optic produces highly monochromatic X-rays, eliminating all incident wavelengths except Cu Kα1 (λ =1.540562 Å). The goniometer is a chi-cradle type, with full phi axis rotation and x-y-z translation. Including omega, this gives six positioning axes for the sample (not including the detector axis, 2Theta). Two detectors are mounted on this instrument: a point detector, which offers higher resolution at the cost of speed, and a faster but lower-resolution linear position-sensitive detector. Popular applications include HRXRD, reciprocal space maps (RSM), and XRR.

Info: http://prism.mit.edu/xray/instruments/hrxrd.html

SOP: http://prism.mit.edu/xray/documents/Bruker%20HRXRD%20Triple%20Axis%20SOP.pdf
SOP: http://prism.mit.edu/xray/documents/Bruker%20HRXRD%20RSM%20with%20LynxEye.pdf
SOP: http://prism.mit.edu/xray/documents/Bruker%20HRXRD%20Using%20XRD%20Wizard.pdf
SOP: http://prism.mit.edu/xray/documents/Bruker%20HRXRD%20XRR%20SOP.pdf

Contact: Jordan Cox    E-mail: This email address is being protected from spambots. You need JavaScript enabled to view it.     Instrument Location: 13-4027

Bruker D8 GADDS Multipurpose Diffractometer Cobalt
The Co source Bruker General Area Detector Diffraction System (GADDS) permits collection of diffraction data over a 2theta range -15 to 117 degrees and a chi (tilt) range as large as 30 degrees. The Eulerian ¼ cradle, which permits many unique tilts and rotations of the sample, with a very fast two-dimensional area detector. This configuration makes this instrument ideal for texture and stress measurements, as well as traditional XRPD and limited SCD and GIXD. A selectable collimator, which conditions the X-ray beam to a spot with a size from 0.5mm to 0.05mm diameter, combined with a motorized x-y stage permits micro-diffraction for multiple select areas of a sample or mapping across a sample's surface. Samples can include thin films on wafers or dense pieces up to 6" in diameter (maximum thickness of 3 mm), powders in top-loaded sample holders or in capillaries, dense pieces up to 60mm x 50mm x 15mm (and maybe even larger). In addition, the GADDS system can collect basic WAXS, SAXS, and GISAXS data by configuring the instrument with a collimator-mounted or detector-mounted beam stop and a helium purged flight tube to reduce air scatter.

Info: http://prism.mit.edu/xray/instruments/gadds.html
Info: http://prism.mit.edu/xray/documents/Bruker%20GADDS%20Intro%20to%202D%20Diffraction.pdf

SOP: http://prism.mit.edu/xray/documents/Bruker%20GADDS%20SOP%20Cobalt.pdf
SOP: http://prism.mit.edu/xray/documents/Switching%20Bruker%20GADDS%20System%20to%20SAXS.pdf

Contact: Jordan Cox    E-mail: This email address is being protected from spambots. You need JavaScript enabled to view it.     Instrument Location: 13-4027

Back Reflection Laue Diffractometer
This system uses a two-dimensional multiwire detector to collect back-reflection Laue patterns to determine the orientation of mmscale bulk large single crystals and thin film single crystal substrates.

Info: http://prism.mit.edu/xray/instruments/laue.html

SOP: http://prism.mit.edu/xray/documents/Laue%20SOP.pdf

Contact: Jordan Cox    E-mail: This email address is being protected from spambots. You need JavaScript enabled to view it.     Instrument Location: 13-4027

Bruker Tracer-III SD Portable XRF
This energy dispersive X-ray fluorescence (ED-XRF) unit provides rapid qualitative non-destructive elemental analysis. It features a rhodium X-ray source and a silicon-based detector and is capable of identifying most elements heavier than magnesium in three minutes or less with a spectrum from 1-40 keV. Normally it gives qualitative results, e.g. trace element identification and relative comparisons of similar samples. Quantitative analysis is possible but more difficult, because the user must create a set of calibration standards for each element of interest.

Info: http://prism.mit.edu/xray/instruments/tracer.html

SOP: http://prism.mit.edu/xray/documents/Bruker%20XRF%20SOP.pdf

Contact: Jordan Cox    E-mail: This email address is being protected from spambots. You need JavaScript enabled to view it.      Instrument Location: 13-4027

SAXSLAB Small Angle X-ray Scattering System

The SAXSLAB instrument is setup to perform transmission small or wide angle X-ray scattering on freestanding samples, powders prepared in kapton tape, liquids in disposable or resealable capillaries, gels in sandwich cells with mica windows. Also, there is capability to perform grazing incidence small or wide angle X-ray scattering (GI-SAXS/WAXS) on nanostructured surfaces. The instrument uses a Rigaku 002 microfocus X-ray source with an Osmic  parabolic multilayer optics to focus the beam crossover at the second pinhole. It has two sets of JJ X-ray 4 jaw collimation slits that are tunable from 0.02 to 1 mm and are made of single crystal InP to reduce slit scattering effects. Samples are introduced into a large vacuum chamber that is pumped down to 0.08 mbar. The sample stage has x-y travel and theta tilt for grazing incidence SAXS measurements. The DECTRIS PILATUS 300K detector is on a linear track that has the capability of automatically moving sample to detector distance from from 100 mm to 1500 mm depending on the sizes that are indented to be probed; for WAXS (3-70 Å) and for SAXS (30-2300 Å).

Info: http://prism.mit.edu/xray/instruments/SAXSLAB.html

SOP: http://prism.mit.edu/xray/documents/TransmissionSAXSSOP.pdf
SOP: http://prism.mit.edu/xray/documents/GISAXSSOP.pdf

Contact: Jordan Cox    E-mail: This email address is being protected from spambots. You need JavaScript enabled to view it.     Instrument Location: 13-4027

 

 

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