2D X-ray Detector Reciprocal Space Mapping

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Solution Overview

Problem

Conventional X-ray diffraction crystallography methods are time-consuming and data-intensive, requiring extensive sampling and repositioning of detectors to construct reciprocal space maps, especially when analyzing multi-layer crystalline materials, which introduces errors and prolongs data collection times.

Innovation Solution

A multi-dimensional X-ray detector is used to integrate diffracted X-ray signals along the scan direction, producing a compressed multi-dimensional image that includes both on-axis and off-axis reflections from multiple crystal layers, allowing for simultaneous data collection and elimination of repositioning errors, with the ability to determine relative crystal orientations and lattice parameters from a single scan.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Measurement precision

If conventional point or one-dimensional detectors are used to collect diffraction data, then measurement precision can be maintained through extensive sampling, but data collection time increases to hours or days

Engineering Contradiction:
Improvelattice parameter measurement precisionVSAvoiddata collection time
Core Design Contradiction:
Measurement precisionVSLoss of time

Solution Approach 1:

The patent transitions from conventional zero-dimensional (point) or one-dimensional (line) detectors to a two-dimensional area detector. This dimensional change allows simultaneous collection of diffraction data across multiple orientations and angles, compressing what would traditionally require extensive sequential sampling into a single integrated measurement, thereby reducing data collection time from hours/days to minutes while maintaining measurement precision through the integrated reciprocal space mapping capability

Inventive Principle:
Principle #17Another dimension (Dimensionality change)

2Loss of information

If the detector is repositioned relative to the sample to cover all regions of interest, then complete reciprocal space mapping can be achieved, but repositioning errors are introduced and data collection is prolonged

Engineering Contradiction:
Improvecompleteness of reciprocal space mapVSAvoiddata accuracy
Core Design Contradiction:
Loss of informationVSReliability

Solution Approach 1:

The two-dimensional area detector captures the entire region of interest in a single fixed position, eliminating the need for sequential repositioning operations. The detector simultaneously records diffraction intensities across multiple scattering angles and orientations, achieving complete reciprocal space mapping without introducing repositioning errors that would compromise data accuracy

Inventive Principle:
Principle #17Another dimension (Dimensionality change)

Solution Approach 2:

The patent merges multiple measurement functions into a single detector position. Instead of moving the detector to separately measure different regions of reciprocal space, the two-dimensional detector integrates all necessary measurements in one fixed configuration, combining what would traditionally require multiple sequential operations into a single simultaneous measurement event

Inventive Principle:
Principle #5Merging (Combining)

Applied Scientific Principles

This section explains which scientific principles are used to turn an abstract innovation direction into a practical engineering solution.

Function Achieved in This Case

This method significantly reduces data collection time, eliminates repositioning errors, and allows for simultaneous analysis of multiple crystal layers, providing accurate lattice parameters and spatial relationships without the need for extensive recalibration, facilitating faster and more precise reciprocal space mapping.

Implementation Method 1

When a beam of radiation with wavelength on the order of the spacing between atoms is made incident upon a crystalline material, several interferometrically reinforced beams are emitted from the sample when the proper geometry of the incident beam relative to the spacing of interest is attained. The condition in which diffraction occurs was described by Bragg as λ=2d sin θ

Methodology Applied
Scientific EffectX-ray diffraction: Diffraction

Implementation Method 2

The condition in which diffraction occurs was described by Bragg as λ=2d sin θ, where λ represents the wavelength of radiation used, d represents the interatomic spacing and θ represents the angle at which the beam is made incident upon the crystal

Methodology Applied
Scientific EffectBragg diffraction: Bragg Diffraction

Implementation Method 3

the diffracted X-ray signal is detected with the detector, which may be a two-dimensional area detector, and which has a fixed position relative to the X-ray source

Methodology Applied
Scientific EffectX-ray detection: X-Ray

Data Source

PatentUS9864075B2Integrated reciprocal space mapping for simultaneous lattice parameter refinement using a two-dimensional X-ray detector
Publication Date: 2018.01.09 BRUKER AXS INC
  • US9864075B2 patent drawing
  • US9864075B2 patent drawing
  • US9864075B2 patent drawing

AI summary

A method for performing an X-ray diffraction analysis of a crystal sample using a multi-dimensional detector that integrates an X-ray diffraction signal while the position of the sample relative to an X-ray source is changed along a scan direction. The resulting image is compressed along the scan direction, but may be collected very quickly. The capture of both on-axis and off-axis reflections in a single image provides a common spatial frame of reference for comparing the reflections. This may be used in the construction of a reciprocal space map, and is useful for analyzing a sample with multiple crystal layers, such as a crystal substrate with a crystalline film deposited thereupon.