Instrument measurements

SEM (Scanning Electron Microscope) Jeol JSM-6510

Contact persons: Pavlína Fialová, Jan Šubrt

The JEOL JSM-6510 scanning electron microscope allows secondary and backscattered electron modes to be measured. The microscope can operate in both high-vacuum and low-vacuum modes. The low-vacuum mode enables the observation of non-conductive samples without the need for surface coating. The microscope has an SDD x-act 10mm² EDS detector from Oxford Instruments, which can detect elements from boron to plutonium.

TEM (Transmission Electron Microscope) Jeol JEM-3010

Contact person: Natalija Murafa

The transmission electron microscope is the only laboratory instrument capable of simultaneously providing information on the structure, elemental composition, and morphology of particles in a region as small as a few nanometers of the studied sample. The JEM-3010 transmission electron microscope from JEOL allows the study of material structures with atomic resolution, both in direct imaging (HRTEM) and through electron diffraction (SAED, CBED, NBED). The microscope is equipped with an EDX detector from Oxford Instruments, enabling elemental analysis with nanometer resolution. The attached DigiStar system from NanoMegas provides maps of crystallographically distinct phases and crystal orientations at the nanometer scale.

Quantachrome Instruments NOVA 4200e

Contact persons: Pavlína Fialová, Eva Pližingrová

The NOVA 4200e surface area and pore size analyzer from Quantachrome allows the simultaneous measurement of 3 samples. Nitrogen gas adsorption is measured at a temperature of -196 °C. The analyzer can also determine the external specific surface area, total pore volume, and average pore radius. From a maximum 100-point adsorption/desorption isotherm, the BJH pore size distribution can be determined. The compatible FloVac Degasser is used for sample pretreatment, allowing for both evacuations at elevated temperatures up to 300 °C and purging samples with nitrogen gas.

Belsorp-max II

Contact persons: Darina Smržová, Pavlína Fialová

The Belsorp instrument allows for determining surface area and porosity in mesoporous and microporous materials. Nitrogen or water vapours are used for gas adsorption measurements.

SETARAM SETSYS EVOLUTION-16-MS

Contact persons: Anna Vykydalová, Pavla Kurhajcová

The SETARAM thermal analyzer allows for measuring samples in inert (argon) and air atmospheres at temperatures up to 1300 °C. In addition to the thermogravimetric signal, a DTA (Differential Thermal Analysis) record is captured simultaneously. A sophisticated system connects the QMS module to a mass spectrometer for the analysis of released gases. The mass spectrometer can operate in either MID (multiple ion detection) or SCAN mode.

Netzsch STA 449 F1 Jupiter

Contact persons: Anna Vykydalová, Pavla Kurhajcová

The Netzsch thermal analyzer, which could be connected with gas chromatography (Agilent Technologies 7890B GC system) or mass spectrometry (Agilent Technologies 5977B MSD), is a sophisticated system capable of simultaneous TGA/DSC and GC-MS measurements. Measurements can be performed in inert (argon) and air atmospheres, with a maximum temperature of up to 1600 °C. This system is used to detect changes in materials under dynamic or isothermal conditions. It can also analyse gases that are generated or released from the material under thermal stress. The evolving gases during measurement can be analyzed using gas chromatography or directly via mass spectrometry (using either selected m/z values or scan mode).

Nexus 670 FT-IR Thermo Electron Corporation

Contact persons: Pavla Kurhajcová, Petra Ecorchard

Spectra are measured in the infrared region within the range of 4000-400 cm⁻¹ with a resolution of 4 cm⁻¹, using a DTGS KBr spectrometer and a KBr beamsplitter for detection. Sample measurements can be performed using transmission techniques such as a pellet (sample + KBr), or with a ATR Smart iTX equipped with either a diamond crystal or a ZnSe crystal.

HRSEM FEI NanoSEM 450

Contact persons: Jiří Henych, Petra Ecorchard

This high-resolution scanning electron microscope allows for capturing high-quality images of shapes, morphology, defects, or agglomerates of particles, even at the nanometer scale. Observation is enabled by the Everhart-Thornley detector or in low vacuum (10-200 Pa) using the Through-the-Lens mode. The instrument allows tilting of the sample within a range of -15 to 75°. The voltage is selectable in the range of 1-30 kV. The Field-Free mode makes measurements and recordings of magnetic samples possible. For even better resolution, measurements can be performed in immersion mode. The EDS detector provides a qualitative and quantitative determination of the present elements, which also offers the capability of graphical elemental mapping.

HRTEM FEI Talos F200X

Contact persons: Jan Tolasz, Natalija Murafa

The microscope is equipped with an FEI X-FEG electron source with high brightness, which can operate at the accelerating voltage of 80 to 200 kV. It features a Super-X EDS system with four silicon drift detectors (SDD) for precise and quantitative energy-dispersive X-ray spectroscopy (EDX) analysis, and selected area electron diffraction (SAED) that utilizes constructive interference of scattered electrons to produce diffraction patterns, useful for examining the crystal structure of materials. The double-tilt, low-background sample holder can be used for more specific applications due to additional sample movements and the use of beryllium components for X-ray analysis with a low background signal.
The FEI Talos F200X combines high-resolution S/TEM (scanning/transmission electron microscopy) and TEM with energy-dispersive X-ray spectroscopy (EDS) for chemical characterization and elemental composition mapping. In STEM mode, the HAADF (high-angle annular dark-field) detector can be used. This technique generates images by collecting scattered electrons with an annular dark-field detector and is sensitive to changes in the atomic number of atoms in the sample (Z-contrast imaging).
The Talos platform is fully digital and also allows for the addition of application-specific detectors or sample holders for dynamic experiments. Rapid TEM imaging on the Talos supports high-resolution and in situ dynamic observations. The FEI Ceta 16Mpix camera provides a large field of view and quickly captures images.

X-ray powder diffraction

Contact person: Petr Bezdička

Our laboratory has three X-ray powder diffractometers: two X'PertPRO MPD (Multi-Purpose Diffractometer) instruments from PANalytical and a third instrument, the Empyrean, series 3, from Malvern PANalytical.

The first is equipped with a cobalt X-ray tube and a fast linear position-sensitive detector, the X'Celerator. The conventional Bragg-Brentano reflective arrangement is primarily used to analyse samples with a high iron content. An in-situ high-temperature chamber (Anton Paar HTK 16) or an analysis chamber with controlled humidity (Anton Paar CHC+ chamber) can be installed. The reflective geometry can also be replaced with microdiffraction geometry, which allows for the non-destructive analysis of small heterogeneous micro-samples, typically those taken from works of art. In this geometry, a monocapillary with an output diameter of 0.1 mm is used in the primary beam.