Equipment and Methods

 

Syntheses and Preparation

Type

Equipment / method

Autoclaves Different autoclaves (stainless steel with Teflon inlay) for (solvo)thermal syntheses up to 260°C and 300 bar as well as glass autoclaves (Büchi) (max. 200 °C, 10 bar)
Continuous synthesis Laboratory plant for continuous nanoparticle synthesis
Glovebox UNIlab Plus DP (MBraun) with mikroskope (Leica)
Microwave systems Discover (CEM) for syntheses in sealed 10 ml pressure vessels (max. 300 °C, 20 bar) or in conventional round-bottom flasks up to 100 mL as well as a multimode microwave system MARS 5 Synthesis (CEM) for parallel reactions under uniform conditions in pressure vessels up to 300 °C and 100 bar or open flasks with max. 5 L
Furnances Various types of furnaces, e.g. muffle furnaces (Nabertherm) for temperatures up to 1100 °C, a self-built furnace with quartz tube reactor for conditioning under inert gas or reactive gases, and a furnace with rotating tube reactor (Carbolite)

 

Laboratory Plants for Catalytic Investigations

Operation mode

Equipment

Semi-continuous Laboratory plants with stirred-tank reactors, continuous gas dosage and online gas analysis (micro-GC)
Continuous Test stand with fixed-bed reactor, gas dosage and online gas analysis (micro-GC)

 

Analysis

Type

Equipment / method

AFM Atomic force microscope Nanoscope IIIA (Veeco)
DLS Zetasizer NanoZS (Malvern Panalytical) for the determination of the hydrodynamic particle diameter as well as the zeta potential in liquid phase by dynamic light scattering
GC Micro GCs (INFICON) for online analysis
REM-EDX Gemini SEM 500 (Zeiss) with thermal Schottky field emission cathode and energy dispersive X-ray spectrometer (EDS), Oxford X-MaxN, silicon drift detector (80 mm2, resolution 127 eV). A variable pressure system allows pressures up to 500 Pa in the chamber
RFA S4 PIONEER (Bruker AXS)
UV-Vis Specord S600 (Analytik Jena) with diode array detector (wavelength range 190-1100 nm) and temperature-controlled cell holder (Peltier element, temperature range -5 °C to 105 °C) with integrated stirrer as well as DR5000 (Hach Lange; wavelength range 190-1100 nm)
XRD Powder X-ray diffractometer X'Pert Pro MPD (Malvern Panalytical) with copper anode (Κα 1.54187 Å) for measurements in reflection (autosampler for sample plates, Bragg-Brentano geometry) and in transmission (capillary); high-temperature furnace chamber (HTK 1200N, Anton Parr) for in-situ X-ray diffraction under different atmospheres up to 1200 °C