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X27A Microprobe
CARS at the APS |
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Overview
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Research Program:
Development and application of analytical techniques
(e.g. microprobe, microspectroscopy, microdiffraction,
fluorescence
microtomography) in geochemistry, environmental science,
chemistry,
biology, and other fields.
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Ring: X-Ray
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Status:
Operational
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Time Dedicated to
General User Program: 25%
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PRT Institutions
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University of Chicago,
Consortium for Advanced Radiation Sources
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University of Kentucky, Dept. of Plants and Soil Sciences
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BNL, Environmental Science Dept.
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Research Types
- Environmental Science, Geology, Biology,
Chemistry
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- Spokesperson: Steve
Sutton (U. Chicago)
- Local Contact:
Antonio Lanzirotti (U. Chicago)
- Safety Coordinator:
Antonio Lanzirotti
- Training Coordinator:
Antonio Lanzirotti
- Beamline Staff:
William Rao (U. Kentucky)
- Scientific Staff:
Mark Rivers (U. Chicago), Paul Bertsch (U. Kentucky), Keith
Jones (BNL)
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Energy Range (keV) |
Beamline
Configuration |
Spot Size |
Total
Horizontal Angular Acceptance (mrad) |
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3-40 |
Unfocused White |
10 µm2 - 25mmH x
2mmV |
3.0 |
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4-18 |
Focused White |
150µmH x 350µmV |
0.5 |
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4-28 |
Unfocused Monochromatic |
10 µm2 - 25mmH x
2mmV |
3.0 |
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4-28 |
Focused Monochromatic |
5µmV x 9µmH |
0.5 |
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Radiation hutch, Canberra 9-element
Ge Array, Radiant Vortex-EX silicon drift, and Canberra Si(Li) x-ray detectors,
using camac based XIA DXP digital multi channel analyzer
system. Ion chamber and
PIN diode detectors, wavelength dispersive spectrometer
(deltaE/E ~ 10-3), xyztheta sample position
stage, remote optical microscope with Mitutoyo
infinity-corrected long working distance objectives,
microdiffraction capabilities using Bruker SMART 1500
CCD detector. |
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Three PC
workstations operating Windows NT, 2000, and XP Pro OS systems,
fastest operating at 3 GHz w/ 1 GHz RAM. One Apple Power Mac G5 (Power PC 970, 1.6 GHz)
using Mac OS X Panther as EPICS boot host. Hard disk, CD-R/W, DVD-R/W,
USB 2.0 Multi-Card Reader, 20Gb Travan tape data storage options.
EPICS Control System using an MEDM front-end. VME and CAMAC system
monitors, Ethernet data access and acquisition, Interactive Data
Language (IDL) software, optical and digital image capture and
processing system with hardcopy. Bruker SMART diffractometer control
system. |
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The x-ray microprobe at beamline X26A is primarily operated in
focused, monochromatic mode utilizing microfocusing optics
consisting of two, 100 mm long, dynamically bent silica
mirrors arranged in a Kirkpatrick-Baez (KB) geometry (designed
and built by P. Eng, CARS-University of Chicago). The KB
mirrors (40:1, 9 meters from the source) focus a 400 x 400 µm
beam down to about 5-10 µm (FWHM) resulting in a gain in flux/µm2
of about 1500 over a pinhole. Photon Flux at 18 keV is roughly 1x109 photons/sec
in focused monochromatic mode. The focusing mirrors are Rh coated and
reside inside a He enclosure. The beamline can also be
operated using a pinhole collimator (~5 µm beam) or an 8:1
ellipsoidal focusing mirror (~150 µm beam). The incoming white
beam is collimated using a water-cooled, copper 'ladder and
slit' assembly. Typically this beam is collimated to 400 µm in
the vertical to reduce effects of thermal heating on the
monochromator. A second set of tantalum, motor-driven 4-jaws
are then used to collimated the beam entering the hutch
(either monochromatic or white).
Two channel-cut, silicon crystal monochromators are available
to monochromatize the x-ray beam for XAFS applications, one
with a (111) lattice cut and the other with a (311) lattice
cut (still in comissioning) located 6 meters from source. Both crystals
are cut to a 7 mm gap and are rotated using a Huber 410 one-circle goniometer (40:1 gear reducer). Crystals are cooled to 11°C using a
Neslab chiller. The crystals can be
translated into position using a motorized translator. To
minimize backgrounds from Compton scattering, the X-ray
detectors reside in the storage ring plane and at 90° to the
incident beam. Currently the detectors we have available
include a Canberra 9-element Ge Array detector, Canberra
SL30165 Si(Li) detector, Radiant Vortex-EX Silicon Drift Detector, and a Microspec Wavelength Dispersive
Spectrometer. The Ge, Si(Li), and SD solid state detectors use the
DXP series of CAMAC based digital spectrometers produced by
XIA. Custom made mini ion chambers and PIN diode detectors are
also available for transmission analysis. The sample stage
sits at 45° to the incident beam, allowing an optical
microscope with TV attachment to be mounted horizontally to
view the sample surface in normal incidence.
The entire microprobe apparatus, including final beam
collimator, sample stage, optical microscope and x-ray
detector, rests on a 107 x 107 cm breadboard, which in turn sits
on a motor-driven lift table. The lift table allows the entire
instrument to be positioned vertically and horizontally to intercept the most intense and most highly
polarized portion of the synchrotron radiation profile and also pivot about an arbitrary fixed point in space. The
X26A x-ray microprobe is currently capable of trace element
analyses with ~ 1 ppm sensitivity and x-ray absorption near
edge spectroscopy (XANES) analyses with 10-100 ppm
sensitivity. Microdiffraction analysis is also available utilizing
Bragg techniques, instrumentation includes a Bruker SMART 1500 CCD array system.
This 2K CCD is bonded, using patented technology, to a 135mm
diameter fiberoptics taper, with 1.83:1 demagnification ratio,
combined with a custom phosphor screen. Combined with its
large input active area and highest available spatial
resolution, this CCD system is optimized for collection of
data out to higher 2 theta angles, and on very weakly
diffracting samples. Since X26A is optimized for spatially
collimated microbeams, we have been able to obtain
high-resolution microdiffraction data on very small (10 µm)
crystals. A fluorescence microtomography setup is also
available, but arrangements must be made in advance. |
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