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Instrument and method for x-ray diffraction, fluorescence, and crystal texture analysis without sample preparation

a technology of crystal texture and instrument, which is applied in the direction of instruments, material analysis using wave/particle radiation, x/gamma/cosmic radiation measurement, etc., can solve the problems of destroying any water ice that msl may encounter, corresponding increases in power consumption, mass and risk, and evaporation in the low pressure environment of mars, so as to eliminate the need for sample preparation and reduce the need for power consumption. , the effect of reducing the need for sampl

Inactive Publication Date: 2011-01-13
UNIV OF MARYLAND BALTIMORE COUNTY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

The present patent provides an X-ray diffraction and X-ray fluorescence instrument that is particularly suitable for extraterrestrial applications, such as on a rover, landing vehicle, or craft. The instrument is designed to be robust, lightweight, and low in power consumption, with a minimum of moving parts, sample preparation needs, and risk. It is also designed to provide efficient geometry, improved sensitivity, and a compact and rugged packaging that consumes minimal power. The instrument can be used in both reflection and transmission geometries, and can measure atomic plane spacings, crystalline grain size, and crystalline texture of unprepared samples. The method is efficient and accurate compared to standard X-ray techniques. Overall, the instrument and method described herein offer a cost-effective and reliable solution for analyzing samples in space.

Problems solved by technology

However, in certain applications, such as extraterrestrial XRD analysis, the number of moving parts required increases (e.g., the CheMin device uses a carousel disc and associated drive system, sample preparation systems such as a fine-grinding mill, etc.), with corresponding increases in power consumption, mass, and risk.
For the CheMin XRD / XRF apparatus 32, which is presently slated for inclusion on the Mars Science Laboratory (MSL) mission scheduled for launch in 2009, sample preparation is required, which would disadvantageously destroy any water ice that MSL may encounter and cause it to evaporate in the low pressure environment on Mars.
Sample preparation also destroys valuable scientific and engineering information regarding grain size and orientation distributions and evidence of stresses and shock.

Method used

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  • Instrument and method for x-ray diffraction, fluorescence, and crystal texture analysis without sample preparation
  • Instrument and method for x-ray diffraction, fluorescence, and crystal texture analysis without sample preparation
  • Instrument and method for x-ray diffraction, fluorescence, and crystal texture analysis without sample preparation

Examples

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Effect test

example 1

Al 6061

[0095]FIGS. 7a-7e show results from a piece of aluminum-6061 obtained using the second prototype XRD / XRF instrument 100 in a 2-hour data run with the X-ray source 110 operating at an electron beam current of 100 microamps. FIG. 7a shows a density plot of the photon count intensity binned in the plane of event energy vs. event diffraction angle. In this space, photons which are due to XRF (e.g., due to contaminants in this case) appear as horizontal lines 205, as shown, and photons due to XRD from crystallized regions with discrete atomic plane spacings (Miller indices) appear as arcs 210, as shown, and trace out Bragg's law for n=1. After applying Bragg's law to compute d-spacing for individual photons, the XRD arcs 210 of FIG. 7a are straightened out as vertical lines 211 in FIG. 7b, while the horizontal XRF lines 205 of FIG. 7a remain as horizontal lines 206. The XRD feature apparent at 1.73 Å is an instrument feature.

[0096]In each of FIGS. 7a-7b, several of the XRD arcs 21...

example 2

Mineral Identification

[0098]FIG. 8 shows data from a bulk sample of hematite showing both diffraction and fluorescence features. As with FIG. 7b, the hematite data is binned and plotted in the space of energy (E) vs. d-spacing, as shown in FIG. 8. XRD data is shown as vertical lines 221, while the XRF data is shown as horizontal lines 225. FIG. 8 is labeled to show some of the expected and detected diffraction features, particularly showing the d-spacings of 1.49 Å, 1.70 Å, 2.21 Å, 2.52 Å, and 2.70 Å. A faint d-spacing vertical line is also observable at 3.69 Å. FIG. 8 is also labeled to show the expected fluorescence features (e.g., Fe Kβ, Fe Kα, and Ti Kα).

[0099]Because d-spacing information acts as an effective “fingerprint” for any given mineral, the specific combination of vertical features 221 in FIG. 8 can be used to identify the sample. D-spacing values for thousands of organic and inorganic substances are available in commercial and freely available digital databases (e.g.,...

example 3

Aerosol Identification

[0103]Applications involving aerosols require a high detection limit to measure trace elements and require high sensitivity to permit analysis of minute amounts of material. A typical aerosol filter configured to collect particles on its surface (e.g., the Nuclepore® filter) holds about 20 μg / cm2 of aerosol mass. For a X-ray beam 105 having a spot size area of about 2 mm2, which is the case for the current example, the total aerosol mass observed by the beam is about 0.4 μg.

[0104]FIGS. 9a-9c show an example of an aerosol filter, analyzed using the disclosed XRD / XRF instrument 100 and techniques disclosed herein, showing measurements of at least 9 elements with X-ray fluorescence and identifying at least three major minerals in the analyzed sample (i.e., calcite, hematite, and halite). The aforementioned second prototype of the XRD / XRF instrument 100 (see generally FIG. 2b) was used to analyze data from micrograms of dust collected on a thin polycarbonate Nuclep...

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Abstract

An X-ray diffraction and X-ray fluorescence instrument for analyzing samples having no sample preparation includes a X-ray source configured to output a collimated X-ray beam comprising a continuum spectrum of X-rays to a predetermined coordinate and a photon-counting X-ray imaging spectrometer disposed to receive X-rays output from an unprepared sample disposed at the predetermined coordinate upon exposure of the unprepared sample to the collimated X-ray beam. The X-ray source and the photon-counting X-ray imaging spectrometer are arranged in a reflection geometry relative to the predetermined coordinate.

Description

CROSS-REFERENCE TO RELATED APPLICATION[0001]This application is a continuation of, and claims benefit of priority to, U.S. patent application Ser. No. 11 / 706,693 filed Feb. 14, 2007, entitled “Instrument And Method For X-ray Diffraction, Fluorescence, And Crystal Texture Analysis Without Sample Preparation”, and U.S. Provisional Patent Application No. 60 / 773,244 filed on Feb. 14, 2006, entitled “Instrument And Method For X-ray Diffraction, Fluorescence, And Crystal Texture Analysis Without Sample Preparation” and U.S. Provisional Application No. 60 / 776,576 filed on Feb. 24, 2006, entitled “Instrument And Method For X-ray Diffraction, Fluorescence, And Crystal Texture Analysis Without Sample Preparation” all of which is hereby incorporated by reference in its entirety.STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH OR DEVELOPMENT[0002]The described herein was made in the performance of work under a NASA contract or grant and by employees of the United States Government and is subjec...

Claims

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Application Information

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Patent Type & Authority Applications(United States)
IPC IPC(8): G01N23/223
CPCG01N23/20G01N2223/076G01N23/223
Inventor GENDREAU, KEITHMARTINS, JOSE VANDERLEIARZOUMANIAN, ZAVEN
Owner UNIV OF MARYLAND BALTIMORE COUNTY
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