Differential Pressure X-Ray Analysis for Atmospheric Samples

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Solution Overview

Problem

Current x-ray analysis techniques face challenges in analyzing specimens at atmospheric pressure due to vacuum instability, charge accumulation on insulating samples, and inefficient x-ray detection, which limits the analysis of 'wet' or non-conductive materials and reduces spatial resolution.

Innovation Solution

An x-ray analysis apparatus with a focused electron beam assembly and a distributed x-ray detector system positioned in a vacuum environment, utilizing a differential pressure element like an electron-transparent membrane to maintain pressure differential and minimize x-ray absorption, allowing efficient detection of x-rays generated from specimens at higher pressures.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Measurement precision

If the x-ray detector is positioned in the atmospheric pressure environment close to the sample, then the solid angle for x-ray detection is increased, but x-rays are strongly absorbed by the gaseous atmosphere

Engineering Contradiction:
Improvex-ray detection efficiencyVSAvoidx-ray absorption by gas
Core Design Contradiction:
Measurement precisionVSObject-affected harmful factors

Solution Approach 1:

The system divides the detection space into two pressure zones: a vacuum environment for the electron beam and high-energy x-ray detection, and an atmospheric pressure environment for sample placement. This segmentation allows each zone to be optimized for its specific function without compromise.

Inventive Principle:
Principle #1Segmentation

Solution Approach 2:

A differential pumping aperture acts as an intermediary between the vacuum and atmospheric pressure environments. It allows controlled gas flow while maintaining the pressure differential, enabling the detector to remain in vacuum while the sample is accessed from the atmospheric side.

Inventive Principle:
Principle #24Intermediary (Mediator)

2Adaptability or versatility

If the specimen is placed in atmospheric pressure environment, then 'wet' samples and insulating materials can be analyzed, but the electron beam scatters on gas molecules reducing spatial resolution

Engineering Contradiction:
Improvesample type compatibilityVSAvoidspatial resolution
Core Design Contradiction:
Adaptability or versatilityVSManufacturing precision

Solution Approach 1:

The electron beam generation and propagation is segregated into a vacuum environment to maintain beam quality and spatial resolution, while only the sample and x-ray detection interact with the atmospheric pressure environment. This allows high-resolution analysis of diverse sample types.

Inventive Principle:
Principle #1Segmentation

Solution Approach 2:

The differential pumping aperture serves as an intermediary that allows the electron beam to pass from vacuum to atmospheric pressure with minimal scattering, enabling the beam to maintain its focussed state while interacting with samples in atmospheric conditions.

Inventive Principle:
Principle #24Intermediary (Mediator)

3Reliability

If a small aperture is used to isolate vacuum for electron beam, then vacuum is maintained, but the aperture severely limits the range of deflection for the electron beam

Engineering Contradiction:
Improvevacuum maintenanceVSAvoidelectron beam deflection range
Core Design Contradiction:
ReliabilityVSEase of operation

Solution Approach 1:

The system dynamically manages pressure zones, maintaining vacuum only where the electron beam is generated and detected, while allowing atmospheric pressure where the sample is placed. This dynamic pressure management enables both beam control and sample accessibility.

Inventive Principle:
Principle #15Dynamics

Solution Approach 2:

The problem is solved by adding the pressure dimension as a differentiating factor between zones. Rather than using a single pressure environment, the system uses differential pressure zones to simultaneously achieve beam quality and sample accessibility.

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

Enables high spatial resolution x-ray elemental analysis of specimens at partial or full atmospheric pressure by minimizing x-ray absorption and ensuring clear line of sight for detection, thereby improving analysis efficiency for both conductive and non-conductive samples.

Implementation Method 1

x-ray spectrum is measured by sensing and measuring the energies of individual x-ray photons emitted by a specimen when it is hit by a focussed electron beam

Methodology Applied
Scientific EffectElectron impact excitation: Electron Impact Desorption

Implementation Method 2

An evacuated electron column generates, accelerates, and focuses electrons and is isolated from the ambient atmosphere by a thin, electron transparent membrane

Methodology Applied
Scientific EffectElectron transmission through thin membrane: Thin Films

Implementation Method 3

Each x-ray photon is an energetic particle and the energy is typically converted into charge using a solid state detector

Methodology Applied
Scientific EffectPhotoelectric effect: Photoelectric Effect

Implementation Method 4

low energy x-rays are strongly absorbed by air at atmospheric pressure

Methodology Applied
Scientific EffectPhotoelectric absorption: Absorption (EM radiation)

Data Source

PatentEP3050072B1X-ray analysis in air
Publication Date: 2024.06.19 OXFORD INSTR NANOTECHNOLOGY TOOLS LTD
  • EP3050072B1 patent drawingFigure 1~2
  • EP3050072B1 patent drawingFigure 3~4
  • EP3050072B1 patent drawingFigure 5

AI summary

An x-ray analysis apparatus comprises an electron beam assembly for generating a focused electron beam within a first gas pressure environment. A sample assembly is used for retaining a sample within a second gas pressure environment such that the sample receives the electron beam from the electron beam assembly and such that the gas pressure in the second gas pressure environment is greater than the gas pressure within the first gas pressure environment. An x-ray detector is positioned so as to have at least one x-ray sensor element within the first gas pressure environment. The sensor element is mounted to a part of the electron beam assembly which is proximal to the sample assembly and further arranged in use to receive x-rays generated by the interaction between the electron beam and the sample.