Transmission X-ray Diffraction Strip Beam Rotation Tilting

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Solution Overview

Problem

Existing powder diffraction analysis equipment using 2D detectors often records single diffraction spots and arcs instead of rings when analyzing organic crystalline materials, leading to incorrect peak intensities and unreliable 1D-powder diffraction patterns due to non-uniform exposure of lattice planes to X-ray radiation.

Innovation Solution

A method and apparatus for transmission mode X-ray diffraction analysis involving a strip-shaped X-ray beam, where the sample is rotated and tilted around predetermined angles to ensure uniform exposure, improving particle statistics and diffracted beam intensities by irradiating a sample slice with a strip-shaped X-ray beam and detecting the transmitted and diffracted radiation.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Productivity

If a 2D detector is used to record diffraction patterns, then the detection speed and information capture are improved, but the diffraction spots and arcs are recorded instead of rings due to non-uniform exposure, leading to incorrect peak intensities

Engineering Contradiction:
Improvedetection speedVSAvoidpeak intensity accuracy
Core Design Contradiction:
ProductivityVSMeasurement precision

Solution Approach 1:

The invention applies dynamic motion to the sample by rotating it around a rotation axis and tilting it around a tilting axis during X-ray irradiation. This dynamic movement ensures that all lattice planes of the crystalline powder material are uniformly exposed to the X-ray radiation, transforming the static non-uniform exposure into a dynamic uniform exposure that produces complete diffraction rings with accurate peak intensities on the 2D detector.

Inventive Principle:
Principle #15Dynamics

Solution Approach 2:

The invention introduces an additional dimensional aspect by incorporating tilting motion around a tilting axis that is perpendicular to the rotation axis. This dual-axis motion (rotation + tilting) adds a second degree of freedom to the sample movement, ensuring comprehensive and uniform exposure of all crystallographic planes, which resolves the dimensionality deficiency that caused incomplete diffraction rings in conventional single-axis systems.

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

2Ease of operation

If the sample is stationary during X-ray irradiation, then the equipment operation is simple, but the lattice planes are not uniformly exposed to radiation, resulting in incorrect peak intensities

Engineering Contradiction:
Improveequipment operation simplicityVSAvoidpeak intensity accuracy
Core Design Contradiction:
Ease of operationVSMeasurement precision

Solution Approach 1:

The invention transforms the stationary sample condition into a dynamic one by implementing controlled rotation and tilting motions. The sample is rotated around a rotation axis and simultaneously tilted around a tilting axis during irradiation, creating uniform exposure of all lattice planes. This dynamic approach maintains operational simplicity through automated motion control while dramatically improving measurement precision.

Inventive Principle:
Principle #15Dynamics

3Ease of manufacture

If only a few crystals or non-randomly oriented crystals are present in the sample, then the sample preparation is easier, but the diffraction spots and arcs are recorded instead of complete rings, leading to unrepresentative patterns

Engineering Contradiction:
Improvesample preparation easeVSAvoiddiffraction pattern representativeness
Core Design Contradiction:
Ease of manufactureVSReliability

Solution Approach 1:

The invention compensates for insufficient or non-randomly oriented crystals by implementing dynamic rotation and tilting motions during irradiation. This movement exposes all possible crystallographic planes of the limited crystals to the X-ray beam from multiple angles, effectively generating complete diffraction rings that represent the bulk material properties, even when only a few crystals are present in the sample.

Inventive Principle:
Principle #15Dynamics

Solution Approach 2:

The invention introduces tilting motion as an additional dimensional degree of freedom to compensate for the limited number of crystals. By tilting the sample around an axis perpendicular to the rotation axis, the system ensures that all lattice planes are exposed to radiation, transforming incomplete diffraction spots from limited crystals into complete representative diffraction rings.

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

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 approach results in more reliable diffracted beam intensities with reduced standard deviation and enables efficient analysis of multiple samples, improving the accuracy and effectiveness of X-ray transmission diffraction analysis.

Implementation Method 1

X-ray radiation is generated by means of an X-ray radiation source that generates a strip-shaped X-ray beam

Methodology Applied
Scientific EffectX-ray radiation generation: X-Ray

Implementation Method 2

Scattering of incident X-ray radiation from a sample of material can yield information about the atomic structure of the material. When such a beam of radiation strikes a sample, a pattern of diffracted radiation is created

Methodology Applied
Scientific EffectX-ray diffraction: Diffraction

Data Source

PatentUS7409041B2Methods of transmission mode X-ray diffraction analysis and apparatuses therefor
Publication Date: 2008.08.05 F HOFFMANN LA ROCHE INC
  • US7409041B2 patent drawing
  • US7409041B2 patent drawing
  • US7409041B2 patent drawing

AI summary

Methods for transmission mode X-ray diffraction analysis of a sample by means of apparatuses comprising an X-ray radiation source that provides X-ray radiation for irradiating the sample and a detector for detecting X-ray radiation transmitted through and diffracted by the sample. The methods include: (a) placing a sample to be analyzed on a substrate, (b) generating X-ray radiation by means of an X-ray radiation source, (c) positioning the substrate and the sample in an initial position, (d) rotating the substrate and the sample with respect to the initial position around a rotation axis over a predetermined rotation angle, (e) tilting the substrate and the sample with respect to the initial position around a tilting axis over a tilting angle, (f) detecting with a detector the X-ray radiation transmitted through and diffracted by the sample during a time interval, and (g) analyzing the X-ray radiation that is detected.