High Temperature Synthesis and Crystal Growth Laboratory

The High Temperature Synthesis and Crystal Growth Laboratory is a facility that has been implemented primarily for the preparation and single crystal growth of uranium intermetallic compounds. This facility has been supporting national and international projects and is the only place in Portugal where single crystals of intermetallic compounds can be grown. Furthermore it has all the safety requirements for work with U and Th.

Main facilities:
• Induction furnace equipped with cold crucibles and accessories for the growth of single crystals by the Czochralski, Bridgman and Floating Zone methods.
• Arc furnaces.
• Resistive furnaces (up to 2200 C).
• Two-zone furnaces (up to 1100ºC).
• Flux equipment (up to 1400º).
• Splat Cooling System.
• Melt Spinning System.
• Electrospinning System.
• Laboratory precision cut-off machine for small dimension materials.
• Low damage spark erosion unit.

Responsible Researcher:

A. P. Gonçalves.

Main Users: 

This laboratory has been used either in the framework of projects participated by the Solid State Group of the Campus Tecnológico Nuclear or by demand of other researchers inside and outside Campus:
• Preparation and single crystal growth of intermetallic compounds based on Fe and f-block elements (collaboration with Dept. Physics, Faculty of Sciences, Univ. Lisbon; Dept. Physics, FCT, Univ. Coimbra; Institute for Transuranium Elements, EC JRC, Karlsruhe, Germany; Laboratoire de Chimie du Solide et Inorganique Moléculaire, Université de Rennes 1, France; Faculty of Mathematics and Physics, Charles University, Prague, Czech Republic; Institute of Low Temperature and Structure Research, Polish Academy of Sciences, Wroclaw, Poland; Faculty of Humanities and Natural Sciences, Presov University, Slovakia).
• Preparation thermoelectric materials, including glasses (Institut de Chimie et des Matériaux de Paris Est, Thiais, France), pnictides and chalcogenides.
• Single crystal growth of B20 compounds (Dept. Physics, FCT, Univ. Coimbra).
• Targets for ion implantation and RIBs (CERN).
• Preparation of RMx (R = f element; M = 3d metal) for catalytic studies.

Molecular Materials Synthesis Laboratory

The activity in this laboratory is focused on the synthesis of molecular species to be used in the preparation of new molecule-based materials, with unconventional electrical and/or magnetic properties. General procedures in organic and inorganic chemistry are currently used in the laboratory and a very special attention is given to low and room temperature crystallization techniques, as single crystals are often required to subsequent characterization techniques (X-ray diffraction, electrical or thermal transport, magnetic studies).

The synthesis facilities of this laboratory include a microwave assisted reactor. The manipulation of air sensitive compounds is usual and this laboratory is equipped with two vacuum lines and a glovebox. The glovebox is equipped with a freezer, which is useful to store thermal air sensitive compounds and in some cases to do crystallizations. The glovebox is also equipped with a microscope in order to allow the analysis of small crystals and mounting them for single-crystal experiments (X-ray diffraction, etc.). Redox properties are often an important aspect of the new compounds, and cyclic voltammetry is a characterization technique currently used in the new molecular species prepared in this laboratory.

Main equipment:
• Vacuum lines (with N2)
• Glovebox
• Microwave assisted reactor
• Potenciostat
• Current sources for electrocrystallization (30)
• Rotary Evaporators (2); Vacuum-ovens (2); Melting point apparatus; Gradient sublimer; etc.

Responsible Researcher:

Dulce Belo