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 |