XPS and Raman Spectroscopy Alignment in Vacuum Chamber

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Solution Overview

Problem

Current sample analysis techniques, such as Raman spectroscopy and X-ray photoelectron spectroscopy (XPS), face challenges in alignment and simultaneous data acquisition due to the need for separate instruments and atmospheric exposure, which complicates surface treatment analysis and feature alignment.

Innovation Solution

A system combining XPS and Raman spectroscopy within a vacuum chamber, utilizing a sample stage, Raman laser transfer optical assembly, video camera, X-ray source, and X-ray alignment indicator to achieve precise alignment and simultaneous data acquisition, enabling focused excitation beams and multi-pixel chemical mapping with perfect image registration.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Measurement precision

If separate dedicated instruments are used for Raman spectroscopy and XPS analysis, then each technique can be optimized for its specific requirements, but alignment of features on the sample becomes difficult and time-consuming

Engineering Contradiction:
Improvealignment precisionVSAvoidsystem integration complexity
Core Design Contradiction:
Measurement precisionVSDevice complexity

Solution Approach 1:

The patent combines Raman spectroscopy and XPS analysis into a single integrated system with a common sample chamber and coordinated beam delivery mechanisms. This merging eliminates the need to physically move samples between separate instruments, enabling precise alignment of Raman and XPS beams on the same sample features through electronic coordination of the sample stage and beam positioning systems.

Inventive Principle:
Principle #5Merging (Combining)

2Reliability

If samples are moved between separate analysis systems, then different techniques can be applied, but sample modification occurs due to time delay and atmospheric exposure

Engineering Contradiction:
Improvesample integrityVSAvoidanalysis time
Core Design Contradiction:
ReliabilityVSLoss of time

Solution Approach 1:

The integrated system maintains samples in a controlled environment (vacuum or inert atmosphere) throughout the entire analysis process by combining multiple techniques in one chamber. This eliminates the need to expose samples to atmospheric conditions during transfer between instruments, preserving sample integrity and enabling sequential or simultaneous measurements without time delays or contamination risks.

Inventive Principle:
Principle #5Merging (Combining)

3Adaptability or versatility

If separate systems are used for Raman and XPS, then each instrument can be independently optimized, but simultaneous investigation of surface treatments is not possible

Engineering Contradiction:
Improvesimultaneous measurement capabilityVSAvoidoptical system complexity
Core Design Contradiction:
Adaptability or versatilityVSDevice complexity

Solution Approach 1:

The system integrates Raman and XPS instrumentation within a shared vacuum chamber, using coordinated sample stage positioning and beam delivery systems to enable simultaneous or sequential measurements on the same sample features. The optical design incorporates beam combining elements and synchronized detection systems that allow both techniques to operate concurrently without interfering with each other, providing comprehensive surface analysis capability.

Inventive Principle:
Principle #5Merging (Combining)

4Measurement precision

If high magnification immersion objectives are used for Raman spectroscopy, then depth resolution performance is optimized, but the working distance becomes limited

Engineering Contradiction:
Improvedepth resolutionVSAvoidworking distance
Core Design Contradiction:
Measurement precisionVSLength of moving object

Solution Approach 1:

The system transitions from lateral/high-magnification imaging to axial/depth-resolved Raman spectroscopy by using confocal detection geometry and depth-gated measurement techniques. This dimensional shift allows the system to achieve excellent depth resolution through the sample while maintaining a large working distance, as the measurement sensitivity is directed along the optical axis rather than requiring high lateral magnification.

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 solution allows for simultaneous acquisition of Raman and XPS spectra and mapping, improving data registration and reducing analysis time by enabling precise alignment and efficient surface treatment analysis, facilitating the analysis of small surface features and reducing sample modification issues.

Implementation Method 1

X-ray photoelectron spectroscopy (XPS)

Methodology Applied
Scientific EffectPhotoelectric effect: Photoelectric Effect

Implementation Method 2

Raman spectroscopy

Methodology Applied
Scientific EffectRaman scattering: Scattering

Implementation Method 3

The X-ray alignment indicator can include a phosphorescent material that is sensitive to the X-rays

Methodology Applied
Scientific EffectPhosphorescence: Phosphorescence

Data Source

PatentEP3423813B1XPS and raman sample analysis system and method
Publication Date: 2022.03.02 VG SYST LTD
  • EP3423813B1 patent drawingFigure 1A
  • EP3423813B1 patent drawingFigure 1B
  • EP3423813B1 patent drawingFigure 2

AI summary

A process of analyzing a sample by Raman spectroscopy and X-ray photoelectron spectroscopy (XPS) includes providing a sample having a sample surface within a vacuum chamber, performing a Raman spectroscopic analysis on a plurality of selected areas of the sample surface within the vacuum chamber to map an area of the sample surface comprising the selected areas, the Raman spectroscopic analysis including identifying one or more chemical and/or structural features of the sample surface in one or more of the selected areas of the sample surface, and performing an X-ray photoelectron spectroscopy (XPS) analysis of one or more selected areas of the sample surface containing at least one chemical and/or structural feature identified by the Raman spectroscopic analysis, wherein the duration of the XPS analysis of a given selected area of the sample surface is longer than the duration of the Raman spectroscopic analysis of that given selected area.