X-ray diffractometer

Details X-ray diffractometer X-ray diffractometer

2002-07-26

2003-12-16

Church, Craig E. (Department: 2882)

X-ray or gamma ray systems or devices

Specific application

Diffraction, reflection, or scattering analysis

C378S084000

Reexamination Certificate

active

06665372

ABSTRACT:

This application claims Paris Convention priority of DE 101 41 958.9 filed Aug. 28, 2001 the complete disclosure of which is hereby incorporated by reference.
BACKGROUND OF THE INVENTION
The invention concerns an X-ray diffractometer with an X-ray source from which X-rays are guided to a sample to be investigated, comprising an X-ray detector for receiving X-rays diffracted or scattered from or reflected by the sample, and a goniometer for adjustment of sequential relative angular positions between the X-ray source, the sample and the X-ray detector for detecting X-ray diffraction lines, X-ray scattered signals or X-ray reflectograms of the sample to be investigated, wherein the X-rays can be guided, at least in sections, along different optical paths.
An X-ray diffractometer arrangement of this type is known e.g. from the company leaflet “X′Pert-MRD” (Philips Analytical X-Ray B.V., Almelo, The Netherlands).
The company leaflet “DIFFRACTION SOLUTIONS D8 ADVANCE” (Bruker AXS Analytical X-ray Systems GmbH, 1997) describes in detail the functional principles of an X-ray diffractometer. Diffractometers of this type can handle a broad variety of analytical tasks in the most differing of fields, such as polymer chemistry, glass production, coating technology, ceramic production, pharmaceuticals, mineralogy, geology, semiconductor and superconductor technology, power plant technology, as well as in archaeology, environment analysis and criminology. Such an X-ray diffractometer facilitates high accuracy routine applications and also demanding special applications in powder diffractometry, such as qualitative and quantitative phase analysis, determination of crystal size and crystallographic investigations. In contrast to a multi-channel spectrometer, an X-ray diffractometer of this type comprises a goniometer for setting sequential relative angular positions between the source, the sample and the detector for carrying out e.g. “Step Scans” or continuous scans. All components mounted on the goniometer can be replaced in a rapid, simple and reproducible fashion.
The above-cited Phillips company leaflet “X-Pert-MRD” describes an X-ray diffractometer with which the X-rays can be guided along different optical paths. The system, however, requires a considerably larger number of components, i.e. several detectors and associated measurement electronics. Moreover, the complex arrangement requires a large amount of space due to its geometric structure which limits the respective angular region which can be analytically detected.
In contrast thereto, it is the object of the invention to present a diffractometer arrangement with the above-mentioned features having as simple a topological construction as possible and of considerably more compact structure to require considerably less space while maintaining full relative motion of the parts, and with reduced amounts of expensive components, in particular detectors and associated measuring electronics or optionally additional X-ray tubes with associated high voltage and cooling water supplies.
SUMMARY OF THE INVENTION
This object is achieved in accordance with the invention in a surprisingly simple and also effective fashion in that the X-rays emitted at a selected detection angle are guided from a position
1
to a position
2
along n≧2 different, switchable optical paths, wherein the different optical paths are rigidly adjusted relative to one another between position
1
and position
2
to form a unit, wherein the sample assumes either position
1
or position
2
, and wherein switching between the different optical paths can be effected by turning the unit relative to the sample, about the sample position to align a selected optical oath at the detection angle and by blocking all non -selected optical paths.
In this manner, construction of an X-ray diffractometer of this type is facilitated using means which are technically easy to realize. The useful angular region is considerably extended compared to the known arrangement for all possible applications using the different optical paths. In this connection, the optical paths can be constructed such that only one single X-ray source on the primary side of the sample and only one single detector on the secondary side of the sample are required.
In a particularly advantageous embodiment of the inventive X-ray diffractometer, the sample is disposed at position
1
and the detector at position
2
. The X-ray radiation from the sample can thereby be accommodated along different optical paths with different physical properties using one single detector and one single detector electronics thereby avoiding additional, expensive components.
In an alternative embodiment of the invention, the source is disposed at position
1
and the sample at position
2
. In this embodiment, the sample can be illuminated with differently prepared or selected X-rays to facilitate different types of measurement without requiring reconfiguration, realignment, and adjustment between measurements.
One embodiment of the inventive arrangement is particularly preferred with which at least one of the optical paths contains a dispersive or reflecting X-ray optical element such as e.g. a crystal, a channelcut crystal, a mosaic crystal, a multi-layered structure, an X-ray mirror, a diffraction grid or another dispersive or reflecting X-ray optical element. These elements produce substantially monochromatic X-ray radiation from an impinging polychromatic X-ray and can be applied to both the X-ray radiation incident on the sample as well as to the X-rays emanating from the sample.
One embodiment of the inventive X-ray diffractometer is particularly preferred with which at least one of the optical paths contains neither a dispersive nor a reflecting X-ray optical element. Such an optical path permits direct passage of X-rays between positions
1
and
2
, to provide a particularly high radiation intensity through direct optical guidance.
In an advantageous further development of this embodiment, the direct optical path has an X-ray lens which can be designed either as a converging lens, a diverging lens or a parallelizing half lens.
One embodiment of the invention is particularly advantageous wherein at least one of the optical paths contains an adjustable and/or exchangeable collimator. This allows adjustment of nearly any intensity for the X-rays passing through the respective optical path and the collimating out of undesired scattered light.
One embodiment is also advantageous wherein at least one of the optical paths includes a shutter. This also eliminates disturbing light. Moreover, certain specific optical paths can thereby be blanked out of the measurement.
One embodiment of the inventive X-ray diffractometer is particularly simple, having only n=2 different, switchable optical paths.
For somewhat more complex embodiments n>2 different switchable optical paths are provided. In simple versions, these may be coplanar to substantially concentrate the optical paths in a single plane.
For more complex versions, not all optical paths are in one common plane but are deflected within certain solid angular regions. These variants are mostly useful for point focus applications.
In a particularly advantageous further development of these embodiments of the inventive X-ray diffractometer, there are several optical paths which are bent relative to that optical path directly connecting position
1
to position
2
, each bent optical path being composed of two straight partial paths, wherein a dispersive or reflecting X-ray optical element is disposed at the bending point and the bending points of at least some of these partial paths are disposed on a common circle about the direct optical path between position
1
and position
2
.
A main application of this latter development is for cases in which a common wavelength is selected using one single crystal material and a common grating. The resolution, the divergence, the intensity and monochromaticity can thereby be differently adjusted along the different optical path

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