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Our Laboratory Facilities

Introduction

The X-ray diffraction laboratory now includes three analytical instruments that provide a diverse array of diffraction capabilities. These instruments include:

  • Rigaku SmartLab
    (installed March, 2012) multi-purpose diffractometer for general powder diffraction, thin-film (both reflectivity and high-resolution rocking curve analysis), low-volume powder analysis, analysis of samples in capillaries, transmission and reflection SAXS, and advanced non-ambient (including elevated pressure and temperature) analytical capabilities.
  • Rigaku D/max Rapid II
    (installed March, 2012) Micro-diffraction instrument for obtaining diffraction information from very small areas on a variety of intact sample types (including polished thin sections, rock chips, small amounts of powders, etc.) utilizing a very large 2D image-plate detector.
  • Scintag Pad V
    our original (first installed in 1985) diffractometer/goniometer with Scintillation detector for general powder diffraction work.

Details about all systems will be found in the "XRD Resources" section of this page below (or you can click on the system names to go to that section)..


Rigaku SmartLab (on left) and Rigaku D/max Rapid II instruments in the X-Ray Diffraction Laboratory (photo taken March, 2012)


The laboratory is open to all University personnel who are interested in obtaining diffraction data for their samples. The laboratory can be used for powder samples (rock, clay minerals, experimentally created powders or other materials), engineered thin films, and a variety of other materials. User requirements for lab use are on another page. We do not currently have the capability to do single-crystal work in our laboratory.

Before use of the laboratory is permitted, all users must demonstrate familiarity with basic radiation safety procedures, be trained in the use of the equipment, and make arrangements to pay for their use of the laboratory. Please read Requirements for Users of the X-ray Diffraction Laboratory for details of how to be certified for laboratory use.

Only qualified persons (faculty, staff, students) affiliated with the University of New Mexico are permitted to use the laboratory. Laboratory personnel can do work for outside users (i.e., other Universities, government agencies and private corporations) on a contract basis; if you are in this group and are interested in having XRD work done, please contact the Lab Manager, Eric Peterson, by Email (ejpete@unm.edu).

Credit for Use of the XRD Laboratory in Published Papers


We ask that all users of the laboratory give credit for their use of the laboratory in published papers if they present or refer to data acquired in the lab. Suggested wording for that credit is given below for each of our three laboratory instruments. The wording (particularly for the SmartLab system) will require modification based on actual operating conditions and optics used for analysis. Please allow the lab manager to review the XRD citations in your papers before they are submitted for publication to assure that XRD systems and parameters are described accurately.

Rigaku SmartLab system:

Samples were analyzed by X-ray diffraction (XRD) in the XRD Laboratory in the Department of Earth and Planetary Sciences at the University of New Mexico, using a Rigaku SmartLab diffractometer system with the SmartLab Guidance system control software for system automation and data collection. Cu-K-alpha radiation (40 kV, 40 mA) was used with a (see detector options below) detector. Data analysis was completed using (see software options below) using the ICDD (International Canter for Diffraction Data) PDF4+ database (rev. 2011) for phase identification and quantification.

SmartLab Detector Options:
1. D/teX Ultra High Speed Silicon Strip Linear (1D) Detector
2. Scintillation Detector + Detector-side Graphite Monochromator

SmartLab Analytical Software Options:
1a. Rigaku PDXL2 Comprehensive analytical software package including quantitative and whole-pattern fitting / Rietveld quantitative and structural options and/or
1b. Materials Data (MDI) Jade 2010 analytical software package with quantitative and whole-pattern fitting options (both for powder and general diffraction analysis)
2. Rigaku GlobalFit Rocking Curve and Reflectivity analysis software (for thin-film analysis)
3. Rigaku NanoSolver SAXS analysis software (for small angle X-ray scattering analysis)

Rigaku D/max Rapid II system:

Samples were analyzed by X-ray diffraction (XRD) in the XRD Laboratory in the Department of Earth and Planetary Sciences at the University of New Mexico, using a Rigaku D/max Rapid II microdiffraction system with the Rapid XRD control software for system automation and data collection, and Rigaku's 2DP 2-dimensional data processing software. Co-K-alpha radiation (40 kV, 40 mA) was used with the large 465 x 256mm 2-dimensional image plate detector for collection of high resolution diffraction data. Data analysis was completed using (see software options below) using the ICDD (International Canter for Diffraction Data) PDF4+ database (rev. 2011) for phase identification and quantification.

Rapid II Analytical Software Options:
1a. Rigaku PDXL2 Comprehensive analytical software package including quantitative and whole-pattern fitting / Rietveld quantitative and structural options and/or
1b. Materials Data (MDI) Jade 2010 analytical software package with quantitative and whole-pattern fitting options (both for powder and general diffraction analysis)

Scintag Pad V system:


Samples were analyzed by X-ray diffraction (XRD) in the XRD Laboratory in the Department of Earth and Planetary Sciences at the University of New Mexico, using a Scintag Pad V diffractometer with DataScan 4 software (from MDI, Inc.) for system automation and data collection. Cu-K-alpha radiation (40 kV, 35 mA) was used with a Bicron Scintillation detector (with a pyrolitic graphite curved crystal monochromator). Data were analyzed with Jade Software (from MDI, Inc.) using the ICDD (International Center for Diffraction Data) PDF4+ database (rev. 2011) for pattern processing and phase identification.


Data Analysis Software (available to users of all Instruments)

Current Analytical Options in our Laboratory: Each instrument has a dedicated Windows workstation computer attached for instrument control and data analysis. The Scintag control computer uses Windows XP and DataScan 4 software for system control, but does not include any data analysis software. The Rigaku SmartLab and D/maX Rapid II systems use Windows 7 and include control and data collection software specific to those systems in addition to the complete suite of data analysis software described below. The D/maX Rapid II system also includes software (Rigaku's 2DP) that can convert 2D data collected by the instrument into a conventional 2-theta vs. intensity diffraction pattern. Both major analytical software packages can read and process data from all three instruments.

All of our anaytical workstations include the following software for use in analysis of data collected on any of our instruments:

  • Jade 2010 (Release 2.1.6, March 2013) - full-featured analysis of XRD data processing including phase identification, quantitative analysis (including Rietveld refinement) and more from Materials Data, Inc. The lab has been jsing Jade since the mid-1990s for data analysis using the fixed-seat version up until 2012 when we upgraded to a 3-seat license for Jade 2010. The server-based licensing allows for more flexible data processing, and the 2010 version adds full quatitative capabilities lacking in the earlier versions.
  • Rigaku PDXL2 (Ver. 2.0.3) - full-featured analysis of XRD data processing including phase identification, quantitative analysis (including Rietveld refinement) and more from Rigaku. The software follows the "flowchart" process similar to the SmartLab Guidance software to help the analyst through the process of peak identification, search-match and confirmation of phases identified, advanced data processing (including stress-strain and crystallite size broading and multi-phase quantification), and crystal (Rietveld-type) refinements of identified phases.
  • ICDD PDF4+, Release 2012 (from the (Intl. Center for Diffraction Data) is indexed and integrated for search-match and quantification with both Jade 2010 and PDXL2 and available on all analytical workstations.
  • ICSD (Inorganic Crystal Structure Database) FindIT, Release 2013-1 (from NIST and FIZ Karlsruhe) is indexed for search-match and quantification on Jade 2010, and linked for refinements on PDXL2.
  • Rigaku 3D Explore (Ver. 2.5) - used for collection, processing and analysis of 3D data on the Rigaku SmartLab including Pole Figures and Reciprocal Space Maps
  • Rigaku NANO Solver (Ver. 3.6) - used for collection collection, processing and analysis of small angle X-ray scattering (SAXS) data on the Rigaku SmartLab
  • Rigaku GlobalFit (Ver. 1.3.3) - used for analysis and modeling of rocking curve data for thin-films to include analysis of layer and substrate thicknesses of single and multiple layer films

All of our analytical systems are located in the XRD lab rooms B-25 and B-27 of Northrop Hall but some can be remotely accessed for convenience in data analysis. If you are interested in availing yourself of this capability, please contact Eric Peterson (ejpete@unm.edu) who can assist in getting you set up to do that.


Pair of analytical workstations in Room B-27, adjacent to room B-25 where the instruments are installed. Rigaku's PDXL2 is running on the left system, MDI's Jade 2010 on the right system. (photo taken July, 2013)


Summaries of XRD Resources Available in the Lab

Rigaku SmartLab System

The Rigaku SmartLab system is a general purpose XRD research instrument equipped with a large variety of interchangeable components that provide a high level of flexibility in analysis of different types of materials. The system is unique in that it will perform optics and sample alignments in a short period of time (usually 10-20 minutes or less) after change of major components and any time it is requested by the system operator, insuring that the system is always optimally aligned prior to data collection.

Effective May, 2013 the SmartLab system is available to users who have completed a radiation safety training session and hands-on instrument training from a qualified lab manager. The details about what is required before users can use the SmartLab may be found on our "Lab Use" page (linked here). The current Operations Manual (i.e., "Cookbook") for the Rigaku SmartLab may be downloaded as an Acrobat PDF by clicking here.

Listed below are the full array of available components. Some components (mostly detectors and sources indicated below by @) require qualified system administrators to be exchanged, but many (including stages and most optics and indicated below by #) can be changed any trained and qualified users as needed.

X-Ray Sources:

The X-ray source is a long-fine focus standard X-ray tube operated at optimal kV and mA. The "default" source for most analyses is Cu, typically operated at 40 kV and 40 mA; these may be adjusted somewhat (35-45 kV, 30-40 mA) as required for particular experiments. If required for specialized analytical needs, upon formal request lab to the administrator, a Co or Mo (@) source can be installed.

X-Ray Optics:

The SmartLab is equipped with Rigaku's Cross-Beam optics unit that (when used with the Scintillation Detector + monochromator option) enables virtually instantaneous change from standard divergent beam (Bragg-Brentano) optics to parallel beam optics.

A Ge(220) 2-bounce incident beam Monochromator and high-resolution parallel plate collimator are available for high-resolution rocking curve and reflectivity work with thin films

Stages (and associated attachments):

  • Integrated, automatically controlled high-precision Z-stage for automatic vertical alignment adjustments with all other stages
  • Standard stage with single-sample holder for bulk and powder sample holders (#)
  • Chi-Phi-Z Eulerian cradle stage enabling tilt and rotation of samples for precise 3D positioning (#)
  • Capillary attachment with rotation capacity and precise X-Y-Z positioning (#)
  • 100mm XY stage allows precise X-Y-Z positioning in a 100 x 100 mm X-Y range (#)
  • ASC-10 10-position automatic sample changer enables precise Z positioning and computer controlled spinning for programmable data collection on up to 10 samples (#)
  • Small Angle X-ray Scattering (SAXS) attachment with scattered-beam vacuum path attachment for transmission SAXS measurements (#)
  • Anton Paar XRK900S is used for experiments a elevated temperatures (up to 900° C) and pressures (up to 10 bar) with integrated cooling and temperature and pressure controller. Use of this stage requires special application to and arrangements with the lab administrator to block out lab time for experimental use (@).

Detectors (@):

  • Rigkaku D/teX Ultra 1D (linear) detector provides extremely high data collection rates for standard data collection, enabling collection of full-range high-resolution data in 5-10% of the time required for a 0D (point) detector + monochromator combination. This detector (in combination with a Ni K-beta filter) is the "default" for use in most Bragg-Brentano (powder and other applicable materials) applications, and experiments involving the Anton Paar XRK900 stage.
  • High-resolution Scintillation detector combined with diffracted beam monochromator is used for all applications requiring a high-resolution point detector (including most uses involving parallel beam optics). Installation of the Scintillation detector takes about 30 minutes to complete, and must be requested of laboratory personnel in advance of use. The Scintillation detector + monochromator combination may also be used for routine powder diffraction data collection.

Close up of the Rigaku SmartLab Goniometer system. From left to right: Cu X-ray source and shutter assembly, Cross-Beam Optic unit (CBO) with Bragg-Brentano slit in place, 5-deg incident beam soller slits, attenuator with 10mm beam limiting slit, standard standard stage (center), first receiving slit unit (with Ni K-Beta filter), 5-deg diffracted beam soller slits, second receiving slit unit, automated attenuator unit and D/teX Ultra high-speed detector. (photo taken July, 2013)


Rigaku SmartLab instrument with access doors open. Detector in place is the Scintillation Counter with monochromator. (photo take March 2012)


The Rigaku D/max Rapid II

The D/max Rapid II Microdiffraction system is designed for collection of diffraction data from small areas on a variety of specimen types utilizing a large 2-dimensional detector to enable conventional diffraction patterns to be obtained from volumes of materials normally considered too small for conventional powder diffraction. The system utilizes a finely collimated x-ray beam (with pinhole collimators 800 to 30 micron diameter) precisely aligned with a CCD camera directed at the area to be analyzed with the resultant diffraction signal collected on a 46.5 x 25.6 cm curved image plate detector with exposure times ranging between 5 minutes to several hours. The source is a long-fine focus X-ray tube, with Cu, Co and Mo sources available; the default source installed is Co (to minimize fluorescence of Fe-rich specimens). Specimens are mounted on an manually adjusted X-Y-Z stage with each axis adjustment ±5mm. The chi (tilt) axis is fixed at 45°, and the omega (horizontal rotation) axis may be varied from -15° to 130° to maximize the amount of diffraction signal delivered to the detector. The specimen may also be rotated during analysis up to 360° at an operator-set rate to enhance scattering statistics.

Data are collected utilizing Rigaku's RapidXRD software that collects and processes the 2D image plate data, and a digital image of the exact area from which data are collected may be saved with the data for reference and documentation. Rigaku's 2DP software is used to digitally process the 2-dimensional diffraction data into a standard intensity vs. 2-theta diffraction pattern that can be analyzed with Rigaku's PDXL2 or MDI's Jade software. 2DP features either automatic or user-selectable masking of the integrated area to produce the best quality diffraction pattern from less-than-perfect diffraction data.

We expect to utilize the Rapid II system for a variety of sample types including:

  • Polished thin sections of rare materials (i.e., meteorites, etc.) that cannot be conventionally "powdered"
  • Small volume microcrystalline phases (i.e., discrete alteration areas, etc.)
  • Small amounts of capillary-mounted material
  • Powder mounts of small volume
  • Any material for which diffraction patterns must be obtained from a small area

This is a new instrument with unique capabilities, and one that we expect to utilize for some cutting edge research in the microdiffraction realm. If you have a research project that you think may be able to benefit from the capabilities of the Rapid II instrument, please contact the lab manager (connolly@unm.edu) so that we can discuss capabilities and possibilities for collaborative analytical work.


The D/max Rapid system including, from left to right, the X-ray source with shutter, micro collimator for focussing the X-ray beam on the specimen, the specimen holder (with illuminating goosneck light source. The large (26 x 46 cm) curved detector plate lies behind the curved surface of the black paper shield surrounding the specimen holder. See details in the photo below. (photo taken March 2012)


Detail of D/max Rapid II gonoiometer and stage assembly. X-ray source and shutter are to the left. Black CCD camera and beam collimator are precisely aligned so that the specimen is in focus when the exact center of the beam is in position on the specimen allowing precise control of the area from which diffracted X-rays are generated. Collimators are available in 800, 300, 100, 50 and 30 micron diameters. The beam stop prevents damage to the detector (that lies behind the black photo paper in the curved housing) from the direct beam. (photo taken March, 2012)


Scintag Pad V System


The X-Ray Diffraction Laboratory. Scintag PadV Goniometer/Diffractometer on left, computer used for diffractometer operations and data collection near the center, and computer used for data analysis and data printing on right. Photo taken in 2004. Lab now has additional systems and is reconfigured somewhat from what is shown here.


Our Scintag Pad V system was originally purchased in 1984. For many years, Scintag operated as a small, independent developer of XRD equipment with a reputation for excellence in both technology and service. In the 1990s, they were purchased several times, each time becoming part of a larger corporation and moving farther from their roots. They are now part of ThermoARL (a multi-national corporate giant) that makes one powder XRD unit in Switzerland. In 2004 they officially announced that they would no longer support the PAD V system.

This system is still a workhorse and by upgrading peripherals (like operating software, HV power supply, etc.), having our local electronics wiz Bob Macy available, and keeping a good supply of spare electronic parts around, we hope to keep it alive for many years to come.


The Scintag (Rich Seifert) goniometer shown in the 10 degree 2-theta sample exchange position. XRD tube housing on left is fixed. In a coupled scan, the sample holder (center) rotates at 1/2 the rate of the detector (right). The detector is a Bicron scintillation counter with a detector-side graphite monochromator located next to the detector (where the array appears to bend). Boxes on the deck to the left of the tube housing hold a variety of collimating slits for limiting the width of the incident and diffracted X-ray beam.


Our current system uses the original diffractometer (goniometer and detector electronics) and housing, but everything else is different from what was delivered in 1984. The current (as of Spring, 2012) incarnation of our Scintag Pad V Diffractometer includes the following hardware and software:

  • Rich Seifert, Inc. (Manufacturer) large-circle (150-275 mm radius) goniometer, vertically mounted with 0.8 degree to 160 degree 2-theta analytical range. This goniometer was manufactured by Rich. Seifert Co. in Germany in the early 1980s (since acquired by GE as Seifert Analytical X-ray) and has a significantly larger analytical radius than powder machines made later by Scintag in North America. It has been a very reliable goniometer for us since first delivered (with a lot of other long-since abandoned items) in 1984.
  • Bicron (Brand) Scintillation counter (now produced by Saint-Gobain Crystals of Paris) with curved-crystal graphite monochromator, EG&G Ortec preamp, NIM/BIN and power supply with RS-232 data/command interface. This exceedingly reliable hardware has also been with us since 1984.
  • Spellman DF3 Solid State high-voltage (maximum 60 kV) power supply. This unit, acquired in the mid 1990s, is an all solid state unit which replaced the original tube-based unit delivered with the system in 1984. A little bit larger than your average personal computer (but much heavier), it replaced several hundred pounds of transformers (which we have kept in the base of the unit to keep it stable). Though we had two failures in the unit over its lifetime (one of unknown cause and one related to a storm-related power surge), it is infinitely more reliable than the unit it replaced.
  • Haskris chilled-water closed-loop circulating cooling system for X-ray tube cooling. An extremely reliable unit from a company which is extremely helpful and responsive.
  • DataScan 4 Software from Materials Data Incorporated (MDI) is used on a Pentium IV (Windows XP Professional) workstation for data collection. MDI makes software for data collection and analysis which is designed to work with a wide variety of XRD units from different manufacturers. In 1985 the PAD V unit was delivered with a Data General computer system with an operating system called RDOS. A few years later, operations were switched to a Digital Equipment Corporation (DEC) VMS-based system which continued until DEC disappeared and we could no longer obtain licenses for the poorly-supported operating system. In 1997 we went with DataScan to move all of our operations to the Windows platform. Since we had already been using Jade for data analysis, we could now move to their format (a variety of the standard XRD data interchange format or DIF) and eliminate the data translation step. Since it communicates directly with the RS-232 interface on the Scintag unit, as soon as we got our cabling and communications parameters set, we were off and running.

Last updated August 30, 2013. Please send comment about (and suggested additions to) this page to connolly@unm.edu.

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