Preparative methods

For materials design, we synthesize a lot of the investigated solids in-house. Therefore, a lot of preparative infrastructure is available, mostly adapted for solid state synthesis under the exclusion of Air.

Gloveboxes – Workspace in inert (mostly Ar) atmosphere with O2 and H2O partial pressure monitoring and filtration (< 0.5 ppm).

Furnaces – Multiple tube and box furnaces up to temperatures of 1300 °C are available for classic solid-state synthesis as well as sample annealing and crystallization. A tube furnace with inert transfer and controlled flow atmosphere is used for larger scale and controlled atmosphere syntheses.

Ball Mills – Mechanochemically assisted solid-state synthesis (mechanochemical alloying), particle size reduction and powder composite mixing are performed in multiple ball mills under inert conditions. Frequency (up to 50 Hz) and planetary mills (up to 1100 rpm) as well as a setup to monitor temperature and pressure evolution in the ball mill cup during the milling are in use. 

Microwave Oven – A Microwave furnace with controlled power (1600 W) and temperature monitoring allows accelerated “microwave-assisted” solid-state synthesis.

Presses – Isostatic (up to 400 MPa) and uniaxial presses (up to 45 tons) are core instruments for sample preparation for the evaluation of bulk solids. Mostly inert processes are established and uniaxial warm pressing (up to 300 °C) is in use.

Sputter Coater – For electrical contacting, sputter coating in inert atmosphere with Au and Pt can be used.

Interested? – Feel free to request collaborative measurements or instrument access to marvin.kraft@uni-muenster.de or ptill@uni-muenster.de.