Central Facilities

               

NCMN Central Facility for X-Ray
Structural Characterization

The NCMN X-Ray Characterization Facility is dedicated to materials identification and characterization through non-destructive, X-Ray Diffraction (XRD) technique. The specific applications include Powder diffraction, x-ray reflectometry, small angle scattering, pole figure, reciprocal space mapping, Grazing incidence in-plane diffraction, x-ray crystallography etc.  Non-ambient powder and single crystal diffraction is also available at selected temperature range. 

Powder diffraction is routinely used for phase identification, finding relative ratio of phases, structural phase transitions, percentage of crystallinity analysis of partially crystalline materials, etc.  Advanced hardware and high resolution optics are available to investigate thin films, multilayers, highly oriented and epitaxial thin films.  Grazing incidence in-plane diffraction provides valuable information of the structural order in the plane of the film.  X-ray crystallography is unique in capabilities to unravel the absolute crystal structure from single crystal diffraction.  

The  following instruments are available at the NCMN X-ray Scattering Facility:  (1) Rigaku SmartLab Diffractometer (2) Bruker D8 Discover Diffractometer  (3) PANalytical Empyrean Diffractometer (4) Rigaku D-Max/B Diffractometer  (5) Rigaku Multiflex diffractometer and  (6) Bruker Smart-Apex Single Crystal diffractometer.

1. Rigaku SmartLab Diffractometer
This is a state-of-the-art instrument including a dedicated arm for detector movement in-plane and perpendicular to the sample surface, thereby able to probe structure in both directions without tilting the sample.  The instrument is equipped with cross beam optics device hardware that will allow switching between focussing (BB) and the parallel beam (PB) geometries easily.  Smartlab guidance software helps the optics and sample alignment automated and prepares optmum scan conditions.  SmartLab can be configured for grazing-incidence in-plane XRD, grazing-incidence XRD, x-ray reflectivity, high-resolution XRD (rocking curves, reciprocal space maps), texture (pole figures), residual stress analysis and small angle x-ray scattering study of nanoparticles.  The diffarctometer uses Cu Kalpha radiation (wavelength of about 1.54 Å).

2. Bruker-AXS D8 Discover Diffractometer
This also is state-of-the-art machine including Vantec-500 area detector, centric 1/4-circle Eulerian cradle, domed hot stage, hi-flux in-plane hardware, laser/video sample-alignment system, Göbel mirror, fine tilt stage, and dual-beam path analyzer module. The system can be configured for grazing-incidence in-plane XRD, grazing-incidence XRD, x-ray reflectivity, high-temperature XRD, high-resolution XRD (rocking curves, reciprocal space maps), texture (pole figures), residual stress, and microdiffraction and capillary diffraction. Bruker D8 Discover diffarctometer is configured in parallel beam geometry with Cu Kalpha radiation (wavelength of about 1.54 Å).

3. PANalytical Empyrean Diffractometer:
Empyream is a dedicated powder diffractometer with advanced detection capabilities.  It is equipped with PIXcel 3D detector that can be operated with 0D, 1D and 2D detection capabilities.  This instrument consists of 3 kW copper target and theta-theta goniometer.  The samples can be placed in zero-background holder and the holder remains horizontal as well as it can be soun continuously during the scan.  


4. Rigaku D/Max-B Diffractometer:

X-Rays are produced by a 1.8 kW, sealed tube Cobalt target. The diffracted beam then converges (is “focused”) into a diffracted beam monochromator which removes all radiation except the Co Kalpha wavelength (about 1.7903 Å) which then enters a scintillation counter. The sample and detector are rotated with respect to the incident beam at angles theta and 2theta respectively. A typical XRD scan consists of a plot of detector angle (2theta) vs. diffracted intensity. These diffractograms can be printed out or saved to disk in application-friendly ASCII format.

5. Rigaku Multiflex Diffractometer:
This instrument consists of 2 kW copper target and ?-? goniometer.  The sample holder remains horizontal during the scan and therefore, there is no need to use adhesive substances to mount samples on to a low background sample holder plate.  Similar to D/max-B, Rigaku Multiflex is also configured in focusing geometry where a secondary monochromator removes the scattered signal except that corresponding to Cu Kalpha wavelength.  Pre-aligned sample holder and friendly operating software makes the powder diffraction experiments very easy with this instrument.

6. Bruker Smart Apex Single Crystal Diffractometer:
Smart Apex Single Crystal Diffractometer  is a dedicated instrument for Crystallography studies (absolute structure determination using a single crystal sample).  This instrument delivers intense, monochromatic beam of Mo Kalpha radiation (0.7107 Å) produced using Graphite monochromator from a sealed Mo X-ray tube and collimated with a pinhole collimator. The single crystal is mounted on the tip of a glass fiber or a nylon loop affixed to a Goniometer head will be attached to a fixed ?, 3-axis goniometer.  The sample is optically aligned using Video camera and a manual control module.  The sample temperature can be varied from 100 – 400 K using Cryostream controller (Oxford Instruments).   The detector (Smart Apex CCD camera) is placed at about 5 – 6 cm from the sample and uses Peltier technology to cool the CCD chip (-40 deg C) to minimize dark currents. The frame buffer computer is provided with softwares for sample centering, data collection (sample unit cell determination, and detailed structure determination), data integration, absorption correction, and structure determination and refinement.      

Further analysis can be carried out in the facility on any of the user PCS equipped with qualitative and quantitative XRD software and the users have access to the latest International Center for Diffraction Data, PDF–4+ Database.

Most powder, thin-film, and bulk samples are acceptable. The sample holders can accommodate samples up to 30 x 30 x 10 cm in size (sometimes larger) with the 30 x 30 cm surface tangent to the diffracting circle. The amount of material needed for a diffraction pattern depends on the diffracting power of the sample and the type of analysis desired. For example, phase identification of a well crystallized powder, with small (< 40 mm) particle size, may only require 1 mg. or less.


UNL CAMPUS LOCATIONS MAP

Nebraska Center for Materials and Nanoscience
                

















RESEARCH HIGHLIGHTS
Crystal Structure research

Temperature dependence of the crystal structure transformations...

Bruker D8Discover, Cu Kalpha Parallel beam 0.5mm diameter

x-ray    x-ray     x-ray

Shah Valloppilly, Specialist
Dr. Shah Valloppilly, Specialist

 

Announcements:
NCMN Facilities Sign-In Calendar 

     Check with the Specialist for log-in access 

 Shah Valloppilly
Facility Specialist

855 N. 16th Street
Room 006, 008 Jorgensen Hall
  Lincoln, NE 68588-0298

phone: (402) 472-3693
    fax: (402) 472-6148
    email: svalloppilly2@unl.edu

David J. Sellmyer, Faculty Adviser

   855 N. 16th Street N. 110
    201 Nanoscience Research Center
  Lincoln, NE 68588-0298

    phone: (402) 472-2407 or 7886
 fax: (402) 472-6148
       e-mail: dsellmyer@unl.edu