Shimadzu/Kratos AXIS SUPRA+ X-ray Photoelectron Spectrometer

Overview

The Shimadzu/Kratos AXIS SUPRA+ is a high-performance, research-grade X-ray Photoelectron Spectrometer (XPS) engineered for quantitative surface chemical analysis with sub-nanometer depth resolution. Based on the principles of photoemission physics—where monochromatic Al Kα or optional Ag Lα X-rays irradiate a sample to eject core-level electrons whose kinetic energies are measured by a hemispherical electron energy analyzer—the AXIS SUPRA+ delivers precise elemental identification, chemical state differentiation (e.g., oxidation states, bonding environments), and spatially resolved compositional mapping. Designed for demanding academic, industrial R&D, and quality control laboratories, it integrates ultra-high vacuum (UHV) architecture (<5 × 10⁻⁹ mbar base pressure), dual-channel detection, and a field-proven electrostatic lens system optimized for both high sensitivity and high spatial resolution. Its heritage traces directly to Kratos’ legacy in ESCA (Electron Spectroscopy for Chemical Analysis), now enhanced under Shimadzu’s global manufacturing and support infrastructure.

Key Features

• Automated UHV sample handling: Motorized 6-position sample stage with robotic transfer arm enables fully unattended operation across multiple samples, including conductive and insulating substrates.
• High-brightness monochromated Al Kα X-ray source (1486.6 eV) with optional Ag Lα (2984.3 eV) for enhanced depth profiling and reduced charging effects on dielectrics.
• Hybrid detector architecture: Dual-channel delay-line detector (DLD) combined with a multi-channel plate (MCP) ensures high count-rate capability (>10⁶ cps) and excellent signal-to-noise ratio even at low beam currents.
• Micro-focused X-ray beam: Adjustable spot size down to ≤10 µm for localized micro-area analysis, compatible with charge neutralization via low-energy electron flood gun and Ar⁺ ion gun (optional).
• Modular design supporting in-situ and operando accessories: Integrated ports accommodate inert-gas transfer modules, high-temperature/pressure catalytic reaction cells (up to 1000 °C, 1 bar), and cryo-cooling stages.
• Real-time instrument health monitoring: Embedded diagnostics continuously track vacuum integrity, X-ray flux stability, lens alignment, and detector gain—feeding status data into the ESCApe software for predictive maintenance alerts.

Sample Compatibility & Compliance

The AXIS SUPRA+ accommodates solid samples up to 25 mm in diameter and 10 mm in thickness, including metals, semiconductors, polymers, thin films, catalysts, battery electrodes, and biological coatings. It supports both air-sensitive and beam-sensitive materials via load-lock chamber integration and controlled gas environments. The system complies with ISO 18118:2017 (Surface chemical analysis — XPS — Calibration of binding energy scale), ASTM E1905 (Standard Practice for Quantitative Analysis Using XPS), and supports audit-ready workflows aligned with GLP and GMP requirements—including full electronic signatures, 21 CFR Part 11–compliant data archiving, and time-stamped, immutable audit trails for all acquisition and processing steps.

Software & Data Management

ESCApe v3.x serves as the unified control, acquisition, and analysis platform. It features an intuitive workflow-driven interface with drag-and-drop method templates, automated peak fitting using Shirley/Tougaard background models and least-squares minimization, and batch-processing capabilities for spectral libraries and imaging datasets. Data export conforms to VAMAS (Versailles Project on Advanced Materials and Standards) and JCAMP-DX formats. Raw and processed data are stored in hierarchical, metadata-enriched HDF5 containers, enabling seamless integration with third-party chemometrics tools (e.g., Python-based scikit-learn pipelines) and institutional LIMS systems via RESTful API.

Applications

• Thin-film and interface chemistry in semiconductor device fabrication (e.g., SiO₂/Si, HfO₂ gate stacks, perovskite solar cell layers)
• Corrosion science and passivation layer characterization on stainless steels and aluminum alloys
• Catalyst surface speciation under reactive atmospheres (CO, H₂, O₂) using integrated reaction cells
• Organic photovoltaic (OPV) and OLED material degradation mechanisms via sequential depth profiling
• Biomedical coating analysis—e.g., plasma-polymerized hydrophilic surfaces on implants or drug-eluting stent coatings
• Forensic and failure analysis of adhesion interfaces, delamination sites, and contaminant residues

FAQ

What vacuum level does the AXIS SUPRA+ achieve during analysis?

The system maintains a base pressure of ≤5 × 10⁻⁹ mbar in the analysis chamber, achieved via turbomolecular pumping backed by dry scroll pumps and NEG (non-evaporable getter) panels.
Can the AXIS SUPRA+ perform angle-resolved XPS (AR-XPS)?

Yes—it supports continuous tilt from −90° to +90° with motorized precision (±0.1° repeatability), enabling non-destructive depth profiling and overlayer thickness quantification down to ~0.3 nm.
Is UPS (Ultraviolet Photoelectron Spectroscopy) supported natively?

Yes—via optional He I (21.22 eV) and He II (40.81 eV) UV sources, enabling valence band structure analysis, work function determination, and molecular orbital mapping.
How is charge compensation handled for insulating samples?

A dual-mode flood gun provides low-energy electrons (0–5 eV) and argon ions (0–500 eV) independently or simultaneously, with real-time feedback adjustment based on C 1s or adventitious carbon referencing.
Does the system support remote operation and multi-user scheduling?

Yes—ESCApe includes role-based access control, web-accessible queue management, and secure SSH/VNC remote sessions compliant with institutional IT security policies.