Solid state chemistry lab

Handschuhboxen J. Hänisch
glove boxes

For the production of polycrystalline powders and/or 1 inch targets (e.g. for pulsed laser deposition) by means of classical solid state synthesis the following equipment is available:

  • Glove box under argon inert gas for handling reactive materials and powders in controlled atmosphere with H2O and O2 content less than 0.5 ppm.
  • Planetary ball mill "PM100" from Retsch with rotational speeds of 100 to 650 rpm. Grinding bowls and balls made of the following materials are available: ZrO2, stainless steel, agate, tungsten carbide.
  • Uniaxial press "Atlas Autotouch 25T Hydraulic Press" by Specac enables a pressing force of 3 T to 25 T. Pressing tools are available for the following sample diameters: 1 0mm, 15 mm, 20 mm, 25 mm and 32 mm.
  • Vitrification station consisting of oxyhydrogen gas burner and distribution rake for vitrification of samples in quartz glass ampoules. The vials can be evacuated (up to 10-3 mbar) or flooded with Ar or N2/H2 (5% H2).
  • Tube and box furnaces can be flooded with any atmosphere (O2, N2, He, H2 and gas mixtures). The box furnaces heat up to 1200 °C, the annealing chamber has a maximum size of 300 x 300 x 400 mm. The tube furnaces heat up to 1300 °C. The maximum annealing diameter is 110 mm, the annealing lengths are up to 1.8 m.

We use the following thermal analysis methode to optimize the annealing process:

  • Differential thermal analysis with dynamic differential calorimetry and thermogravimetry (Netzsch STA 449C Jupiter) heats the samples from 25 to 1500 °C with heating rates between 0.1 and 50 K/min. The maximum sample weight is 5 g, the resolution is 1 µg. The signal-to-noise ratio is 15 µW, the baseline linearity is 3 µV and the temperature accuracy is < 1 K.
  • Dilatometer for measuring thermal expansion coefficients (Netzsch Dilatometer DIL 402C) for samples with a maximum length of 25 mm and a diameter of 12 mm in the temperature range from 25 to 1500 °C. The measuring path is 2.5 mm, the sensitivity 1.25 nm.

 

For target production (annealing temperatures > 1150°C as well as cold isostatic pressing) we cooperate with the Institute of Applied Materials - Ceramic Materials and Technologies (IAM-KWT).