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49th Lunar and Planetary Science Conference 2018 (LPI Contrib. No. 2083) 2554.

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NEW DEVELOPMENTS IN X-RAY DIFFRACTION FOR PLANETARY EXPLORATION. P. C. Sarrazin 1,


D. F. Blake2, M. Gailhanou 3, J. Chen 4 , P. Dera 5, R. T. Downs6, and T. F. Bristow2, 1 SETI Institute, Mountain View,
CA 94043 (psarrazin@seti.org), 2 Exobiology Branch, NASA Ames Research Center, Moffett Field, CA 94035, 3
CNRS, IM2NP UMR, Marseille, France, 4 Baja Technology, Tempe, AZ, 5 HIGP, Univ. of Hawaiˈi, Honolulu, HI, 6
Geosciences, Univ. Arizona, Tucson AZ 85721-0077.

Introduction: X-ray diffraction (XRD) is a gen- analysis of materials scooped at the surface.
eral purpose technique used for definitive, quantitative
mineralogical analysis. The MSL CheMin instrument
(Fig. 1), the first XRD instrument flown in space, es-
tablished the quantitative mineralogy of the Mars soil
[1], characterized the first habitable environment on
another planet [2], and provided the first in-situ evi-
dence of Martian silicic volcanism [3]. CheMin is now
employed in the characterization of the depositional
and diagenetic environments of lacustrine mudstones
that comprise the lower strata of Mt. Sharp [4].

Fig. 2: XTRA proof of concept prototype operating in


vacuum (X-ray tube, vibrated reflection sample cells,
CCD and electronics).

XRD without Sample Preparation: Hybrid-XRD


(HXRD) is a concept under development to analyze
rocks or soils without sample preparation [7]. If the
material is sufficiently fine-grained, a powder XRD
pattern is obtained, similar to CheMin or XTRA.
With coarse-grained crystals, the white
Fig. 1: The MSL CheMin instrument (left) and ex- bremsstrahlung radiation of the tube is diffracted into
ample of 2D XRD data (right). Resolution is ~0.3 °2θ. single crystal Laue patterns. Unlike typical Laue ap-
plications, HXRD analyzes the energy of each Laue
Conventional powder XRD requires samples com- spot, enabling the measurement of single crystal
prised of small grains presented in random orienta- Bragg diffractions. (Fig. 3). Dedicated crystallo-
tions. In CheMin, sample cells are vibrated to cause graphic software has been developed for identification
loose powder to flow within the cell, relaxing the re- of minerals responsible for the Laue patterns (Fig 4).
quirement for fine-grained samples [5]. Nevertheless,
CheMin still requires substantial sample preparation. High resolution XRD: With CheMin and any of
Deployment of XRDs on smaller missions will require the previously described XRD concepts, instrument
simpler sample preparation and decreased instrument resolution suffers from the system miniaturization and
size and complexity. It is also desirable to improve 2  is limited to about 0.3 °2θ. A planetary XRD based on
resolution to enhance the instrument’s capability to re- Guinier geometry is under development to provide a
solve complex mineralogies. Efforts in these directions compact high resolution instrument. This design
are underway. hinges on the use of a parafocusing geometry with a
curved 2D detector to cover the angular range of inter-
XRD with Limited Sample Preparation: XTRA est. A substantial gain in resolution has been demon-
(Extraterrestrial Regolith Analyzer) is intended to an- strated with a basic proof-of-concept instrument (fig.
alyze fines in as-delivered surface regolith, without 5). Both reflection and transmission geometries can be
sample preparation [6]. Fine-grained regolith coats the developed with the Guinier design and are being ex-
surfaces of most airless bodies in the solar system, and plored as part of a PICASSO funded project.
because this fraction is comminuted from the rocky re-
golith, it can often be used as a proxy for the surface Development of High TRL Components: Rapid
as a whole. XRTA uses a CCD in direct illumination and cost-effective development of flight instruments
for the collection of XRD and XRF signal from a sam- requires the availability of mature technologies of the
ple scooped and placed in a cell. XTRA can be config- critical components. High TRL subsystems are being
ured in transmission or reflection geometry using vi- developed for future XRD instruments in collaboration
brated cells for as-delivered powders, allowing direct with industry partners who can provide expertise in
49th Lunar and Planetary Science Conference 2018 (LPI Contrib. No. 2083) 2554.pdf

design and manufacturing of flight sub-systems. Spe- ence, Big Sky, MO, March, 2012. Paper #2.0905 [7]
cial full-frame and frame-transfer X-ray CCD detec- LPSC 40 #1496 .
tors are being developed with e2V (UK); some detec-
tors featuring internally cooled packages (Fig. 6a).
Custom FPGA based electronics for low noise CCD
operation with embedded data processing capabilities
are under development with Baja Technology (Fg 6b).
Miniature microfocused X-ray tubes capable of opera-
tion >10W are being developed by RTW of Germany
(Fig. 6c), with power supplies developed by Battel En-
gineering (Fig. 6d).

Fig. 5: Guinier proof of concept breadboard in reflec-


tion geometry (100mm focusing diameter); XRD pat-
tern of LaB6 standard showing <0.18 °2θ resolution.
Fig. 3: HXRD proof of concept prototype featuring 4
Ray tracing simulations have shown possible improve-
direct illumination CCD detectors for improved cov-
erage of the reciprocal space. ment of this figure in this geometry.

Fig. 4: Crystallographic analysis code developed for


the HXRD instrument allows mineral identifications
with the “color Laue” XRD approach.
Fig 6: Example of flight components under develop-
Deployment Opportunities: XRD instruments ment with industrial partners: A. X-ray CCD in flight
will be proposed for future landed instrument opportu- package with internal peltier cooler (e2V); B. CCD
nities on planets and planetesimals. Instruments will control electromnics (Baja Technlogies); C. miniature
be tailored to the specific mission constraints and will microfocused X-ray tube (RTW); D. X-ray tube power
be comprised of combinations of the features and module with HVPS stage (Battel Engineering).
flight hardware presented above.
Acknowledgements: The authors are grateful for
References: support from NASA/ARC’s Center Innovation Fund
[1] Science, 341, 1238932; doi:10.1126/science. and NASA’s PICASSO program (grant #
1238932, [2] Science, 10.1126/science.1243480. [3]
NNX15AM95G).
PNAS: doi: 10.1073/pnas.1607098113 [4] Science,
356 eaah6849 DOI:10.1126/science.aah6849 [5]
LPSC 35 #1794 (2004) [6] IEEE Aerospace Confer-

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