Bruker Axs Gmbh

Other

Broker Axs, Inc.

Bob Baoping He

Roger David Durst

Ryan C Bollig

Carsten Michaelsen

Christoph Ollinger

Rolf Schipper

Christian Maurer

Olaf Meding

Gerald T Schwarz

Chuji Katayama

Christopher S Frampton

Frank W Burgäzy

Hans Mathias Lutz Brügemann

Frank Feng Jin

Max Li

Stephen I Foundling

Kingsley L Smith

An X-ray diffraction method measures crystallite size distribution in a polycrystalline sample using an X-ray diffractometer with a two-dimensional detector. The diffraction pattern collected contains several spotty diffraction rings. The spottiness of the diffraction rings is related to the size, size distribution and orientation distribution of the crystallites as well as the diffractometer condition. The invention allows obtaining of the diffraction intensities of all measured crystallites at perfect Bragg condition so that the crystallite size distribution can be measured based on the 2D diffraction patterns.

Measurement of crystallite size distribution in polycrystalline materials using two-dimensional X-ray diffraction

A method of determining the spatial orientation of a two-dimensional detector in an X-ray diffractometry system, and calibrating the detector position in response thereto, uses diffraction patterns from a powder sample collected at a plurality of detector swing angles. The overlapping of the detected patterns indicates relative errors in the detector orientation. In particular, intersection points between the different diffraction patterns may be located, and their relative locations may be used to identify errors. Such errors may be in the detector position, or they may be errors in different rotational directions, such as roll, pitch or yaw. Determination and correction of the detector orientation using this method may be part of a calibration routine for the diffractometry system. Roll error may also be determined using a single measurement with the detector at a swing angle perpendicular to the X-ray beam.

Two-dimensional X-ray detector position calibration and correction with diffraction pattern

A method is provided for performing an X-ray diffraction stress analysis of a sample such as a thin film, a coating, or a polymer. The sample has a surface with two perpendicular axes S, Swithin a plane of the surface, and a third axis Sperpendicular to the sample surface plane. An X-ray beam is directed at the sample surface at a relatively low angle with regard to the surface plane. X-ray energy is diffracted from the sample and detected with a two-dimensional X-ray detector at a plurality of rotational orientations of the sample about S. The third axis Sis maintained at a constant tilt angle during the entire X-ray diffraction stress analysis, thereby avoiding the significant error associated to the movement of a cradle track of a goniometer used for the X-ray diffraction stress analysis and on which measurements at a low 2&#x3b8; angle are highly sensitive.

X-ray diffraction device and method to measure stress with 2D detector and single sample tilt

A method and apparatus for performing an X-ray diffraction measurement with a diffractometer having an X-ray beam directed at a sample and a two-dimensional X-ray detector includes the performance of a physical scan during which the detector is moved through a scanning range in an angular direction about the sample position. To provide a uniform exposure time, the detector, when located at an extreme of the scanning range, is controlled to progressively change the portion of the detected X-ray energy that is used at a rate that maintains a uniform exposure time for each angular position in the scanning range. Alternatively, when located at an extreme of the range, the detector is kept stationary until a desired minimum exposure time is obtained for each angular position, after which the collected diffraction data is normalized relative to exposure time.

Method and apparatus for extending angular coverage for a scanning two-dimensional X-ray detector

An X-ray diffraction system uses a two-dimensional detector to detect diffracted X-ray energy at a plurality of radial positions surrounding a sample location, the results at each position being combined to form a final diffraction image. To minimize smearing in the final image, the detector pixel intensities at each position are reapportioned among the pixel locations prior to being combined with the intensities collected at other positions. A two-dimensional pixel array space of the detector is projected onto a cylinder to form a projected pixel array space, and a virtual cylindrical detection surface representative of an ideal cylindrical detector is determined. An overlap between the pixels of the projected pixel array space and the pixels of the virtual cylindrical detection surface is determined, and pixel intensities are reapportioned accordingly. The reapportionment may include dividing each pixel space into subpixels and redistributing the subpixels among adjacent pixels.

Method for collecting accurate X-ray diffraction data with a scanning two-dimensional detector

An area detector used in a two-dimensional system is used as a point detector in Bragg-Brentano and other geometries by providing the area detector with a mask the limits the area through which X-rays can enter the detector. Secondary X-ray optics and a monochromator that are part of the diffractometer geometry are attached to the area detector mask to allow a fast and easy switch between the two-dimensional detector mode and the point detector mode. A concave detector mask is used with a spherical detector in order to reduce the secondary beam path and increase detector efficiency and the opening in the detector mask can be offset from the mask center to achieve high 2&#x3b8; angle measurements. Single channel bypath electronics are used to disregard the dimensional position of each X-ray count to increase the efficiency and speed of the system.

Method and apparatus for using an area X-ray detector as a point detector in an X-ray diffractometer

Crystallite size in a sample is determined by performing a quantitative &#x3b3;-profile analysis on a diffraction ring in a two-dimensional X-ray diffraction pattern. In particular, a two-dimensional X-ray diffraction system is first calibrated with a sample having a known crystallite size, crystal structure and X-ray absorption coefficient. For a given instrument window, the number of grains contributing to a selected diffraction ring is determined by the effective diffraction volume, grain size and the multiplicity of the diffracting crystal planes. The grain size of an unknown sample can then be determined by a quantitative analysis of the diffraction ring.

Method for measuring crystallite size with a two-dimensional X-ray diffractometer

A diffractometer for X-ray diffraction measurements has two co-exiting sample stages which are mounted on the goniometer base simultaneously. A rotation stage is used for single crystal X-ray diffraction and an XYZ stage is used for general X-ray diffraction with bulky samples. The driving bases of both stages are located away from the instrument center so the measuring space in the vicinity of the instrument center is available to either of the two sample stages. With this arrangement, the rotation axis of the rotation stage stays aligned to the instrument center even when the XYZ stage is used for data collection. Therefore, realigning of the rotation stage to the instrument center is not necessary when switching the applications between the two stages.

X-ray diffractometer having co-exiting stages optimized for single crystal and bulk diffraction

A handheld X-ray diffractometer comprises a miniaturized X-ray source and multiple area detectors to allow the diffractometer to obtain two-dimensional X-ray diffraction images in a large diffraction space without rotating the sample. The source and detectors are located inside of a radio opaque enclosure that protects the operator during use. The handheld diffractometer also comprises a sample monitoring and alignment system that allows an operator to observe the measuring area and to align the diffractometer to the sample from outside of the housing. A specially designed mouthpiece, which mates the diffractometer to the sample area, prevents x-ray leakage and triggers off the data collection. The detectors can be positioned to perform measurements necessary to calculate a mechanical stress in the sample. Linear detectors may also be used in place of the area detectors.

Handheld two-dimensional X-ray diffractometer

An x-ray mirror provides focusing and monochromatization while maintaining a high degree of reflectivity. The mirror has at least two mirror portions, one with a multilayer surface that provides the desired monochromating, and the other with a total external reflection surface. The multiple surfaces combine to provide the desired focusing of the x-rays from a source to a focus point. A variety of configurations may be used, each of which does the desired focusing and monochromatization with minimal energy loss. Relative positioning of the mirror portions may also allow for adjustment of the focus length.

Hybrid x-ray mirrors

A multiple wavelength X-ray source includes an electron-generating cathode and an anode with multiple target regions, each of which emits X-rays at a different characteristic wavelength in response to the electrons. The different X-ray radiation outputs are focused by different focusing sections of a focusing optic. The multiple focusing sections are in different respective locations, and each focuses its respective X-ray radiation onto a sample. The focusing sections may be side-by-side mirrors in a Kirkpatrick-Baez configuration, or in a single-bounce, doubly curved elliptical configuration.

Multiple wavelength X-ray source

A sample analysis system makes use of both X-ray diffraction analysis and Raman spectroscopy of a sample. The sample is part of a sample library that is mounted on an XYZ stage that allows each sample to be examined in turn, as the XYZ stage is moved to position successive samples to a sample location. The system components may be mounted on a goniometer to allow their repositioning. A video system may be used for optical examination of the sample, and a knife edge may be used to prevent X-ray radiation from reaching a sample adjacent to the sample positioned at the sample location. A controller may be used to automatically control the operation of the analysis components and the movement of the sample holder to as to allow automated analysis of all of the samples in the sample holder.

Combinatorial screening system and X-ray diffraction and Raman spectroscopy

An x-ray source provides both a line focus output and a point focus output, and is mounted on a rotatable support to allow easy changing between the two. A housing has ports at different angular positions relative to an anode, and each port has an associated optic appropriate for an x-ray beam passing through that port. Three or four ports may also be used to allow for different types of beam conditioning. The different beam optics may also do conditioning based on wavelength, and the anode may be of a composite material to provide different wavelength ranges. The rotatable support may be manual or motorized, and a lockout mechanism may be used to ensure that only one port is active at a time. The support may also be located on a movable table that is movable in multiple perpendicular directions.

Multiple-position x-ray tube for diffractometer

An X-ray diffraction apparatus provides analysis in either transmission or reflective mode and easy conversion between the two modes. An X-ray source and X-ray detector are each connected to a different circle of a goniometer. The two circles may be rotated independently to position the source and detector on the same side of a sample library for reflection mode operation, or on opposite sides of the sample library for transmission mode operation. The sample library has a horizontal orientation that allows open sample containers of the library to maintain the sample without spillage, and it connects to an XYZ stage that can move in three dimensions. The system may use a beamstop, and the goniometer and XYZ stage be motorized and controlled for automated sample analysis.

X-ray diffraction screening system convertible between reflection and transmission modes

A scanning line detector according to the present invention uses a detector with a linear arrangement of detection elements that is moved along a range of diffracted x-ray directions to collect data across a multidimensional detection area. The scanning line detector allows for the simulation of a two-dimensional detector system without the need for a two-dimensional detector. The detector may follow a desired path to simulate a desired shape, such as a cylinder. A slit may be included to limit the detector line width, and a scatter shield may be used to minimize noise from air-scattered x-rays. The detector may also use a specially designed monochromator for conditioning the diffracted x-rays. The detector may be rotatable about an axis parallel to a direction along which x-rays are diffracted, allowing it to be used in different orientations.

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Madison, WI, United States of America

Bob Baoping He