Record Details

Preparation of yttrium and rare-earth metals by metallothermic reduction

ScholarsArchive at Oregon State University

Field Value
Title Preparation of yttrium and rare-earth metals by metallothermic reduction
Names Block, Frank Elmer (creator)
Wicks, Charles E. (advisor)
Date Issued 1964-05-25 (iso8601)
Note Graduation date: 1964
Abstract An investigation was made of various methods for the
preparation of yttrium or rare-earth metals by metallothermic reduction.
Particular emphasis was placed on the use of high-purity chloride
salts as intermediates. Methods were stressed which appeared
adaptable to production of high-purity, ductile metal on a plant
scale.
Reactions were chosen for study on the basis of thermodynamic
considerations and also from a standpoint of chemical
and physical properties of reactants and byproducts. Consideration
was given to construction materials and their contribution of
impurities to the metal products.
Yttrium or rare-earth chlorides, fluorides, bromides
or iodides were investigated as intermediates for metal production.
Emphasis was placed on the development of methods for preparing
these halides and for refining them to a high state of
purity.
Rare-earth chlorides were prepared either by slow
dehydration of hydrated salts while in contact with ammonium
chloride, or by a more rapid technique involving the direct
chlorination of mixtures of rare-earth oxides and carbon. In
either case, chloride salts were purified by vacuum distillation
or by filtration of molten salts.
Lithium, sodium, potassium and calcium were tested as
reductants for anhydrous halides. These metals were compared
as reductants on the basis of operating characteristics, purity
of metal product, and yield of product.
Yttrium and rare-earth metals prepared in this study
were consolidated, usually by inert-atmosphere arc melting, and
the consolidated metals were evaluated on the basis of chemical
analyses and mechanical workability.
Of the many systems studied, best results were obtained
by the lithium reduction of rare-earth chlorides in Inconel or molybdenum apparatus. Metal made by this procedure was freed
of byproduct lithium chloride by vacuum distillation, and the
rare-earth metal, which appeared as a sponge, was consolidated
by arc-melting.
Yttrium was prepared by this technique on a scale of
15 pounds of metal per batch. Metal recoveries were greater
than 95 percent and the major impurity, oxygen, was usually
present in amounts less than 500 ppm.
Samarium and europium cannot be prepared by reduction
of their halide salts. These metals were produced by reduction
of their oxides in a high vacuum employing lanthanum, cerium,
or zirconium as reductants. Yields were usually over 90 percent
during tests conducted at 900 to 1450°C.
Genre Thesis/Dissertation
Topic Yttrium
Identifier http://hdl.handle.net/1957/48434

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