Solution Growth of Intermetallic Single Crystals: A Beginner's Guide

Abstract

Progress in experimental solid state physics, as well as in related disciplines, is often hampered by limited access to single crystals of novel materials. This lack of single crystalline samples constrains researchers to study or measure materials that are available rather than the materials that are most relevant to the questions at hand. The extreme example of this is the allegorical Ph.D. student who has to measure the one crystal that the advisor has on hand, regardless of the physical question to be probed. As part of the second Euroschool on complex metals I presented lectures on the design, discovery, growth and characterization of novel intermetallic compounds. In this paper I will focus on the basics of solution growth of novel compounds.

Charge density wave in layeredLa1−xCexSb2

“…Samples of La 1−x Ce x Sb 2 were grown from excess Sb flux [2,25,26]. Ce, La, and Sb materials (Ce and La from [27] and Sb from Alfa Aesar with 99.9999% purity) were put together in an alumina crucible and sealed in a quartz ampoule in inert He gas atmosphere.…”

Suppression of ferromagnetism in the La(VxCr1−x)Sb3system

“…Single crystalline La(V x Cr 1−x )Sb 3 samples were synthesized via high-temperature solution method with excess Sb as self-flux [18,27,29,30]. High purity (> 3N) elements with the starting stoichiometry of La : V : Cr : Sb = 8 : x : 8-x : 84, were placed in a 2 mL alumina crucible and sealed in a fused silica tube under a partial pressure of high purity argon gas.…”

“…High purity (> 3N) elements with the starting stoichiometry of La : V : Cr : Sb = 8 : x : 8-x : 84, were placed in a 2 mL alumina crucible and sealed in a fused silica tube under a partial pressure of high purity argon gas. The ampoule containing the growth materials was heated up to 1180 • C over 3 h and held at 1180 • C for another 3 h. The growth was then cooled to 750 • C over ∼ 85 h at which temperature the excess liquid was decanted using a centrifuge [29,30]. Single crystals of La(V x Cr 1−x )Sb 3 grew as rectangular plates, with shiny surfaces that had a few drops of residual Sb-rich flux on them.…”

Use of frit-disc crucibles for routine and exploratory solution growth of single crystalline samples

“…One of the key innovations in solution growth of single crystals was the routine use of a centrifuge to separate the hot, residual melt/solution from the crystalized phase at the end of growth [1][2][3]. Simple laboratory centrifuges readily produce rotational frequencies of 2000 rpm and can have effective radii (sample to axis of rotation) of 15 cm; such a system can produce accelerations 600 times Earth's gravitational acceleration.…”

“…Originally, a plug of moderately compressed silica wool would be inserted into an inverted catch crucible that was placed on top of the growth crucible. This is described in references [1][2][3] with specifically detailed pictures in reference [3]. As more reactive melts were used, e.g.…”