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A Review of the Mineral Processing and Extractive Metallurgy of Rare Earth Minerals
Patrick R. Taylor
The Kroll Institute for Extractive Metallurgy Colorado School of Mines

Resource Recovery Past & Present

Geology Education Engineering Economics

Geology Waste Treatment, Processing & Minimization Education Engineering Economics Energy Environment



Mineral Processing Extractive (Chemical) Metallurgy

Particulate Materials Processing Materials Chemical Processing


Physical Metallurgy

New Materials Development

Materials Science & Engineering

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Other Critical Materials

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The rare earth metals include sixteen elements: yttrium (atomic number 39), lanthanum (57), cerium (58), praseodymium (59), neodymium (60), promethium (61), samarium (62), europium (63), gadolinium (64), terbium (65), dysprosium (66), holmium (67), erbium (68), thulium (69), ytterbium (70), and lutetium (71). The elements with atomic weights 57 to 71 are collectively called the lanthanides since they all have properties similar to lanthanum. Scandium (21) is sometimes included as a rare earth metal since it is chemically similar to yttrium and the lanthanides.

Rare Earth Elements

Energy Critical Elements, American Physical Society & Materials Research Society, 2011.

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One major use of rare earth metals is as catalysts in petroleum refining. They also have many metallurgical applications as pyrophoric alloys. Another application is the use of lanthanide oxides as a constituent of high quality optical glass. The current high interest is due to rare earth applications (magnets) used in many new energy and defense applications and the Chinese control of supply.


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Ceramics 4%

Rare Earth Markets

Others Catalyst Glass 3% 5% 2%

Polishing 4%

Phosphors 31%

Metal Alloys 14%

Magnets 37%

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The two major minerals used as sources of rare earth metals are monazite (Ce-La-Nd-Pr phosphate) and bastnasite (Ce-La-Nd-Pr fluorcarbonate). Monazite is, or has been, mined in Australia, India, the United States, and other areas to a lesser degree. Bastnasite is primarily mined in the United States and China. Several other ores are mined for the rare earths as well, including xenotine, apatite, yttrofluorite, cerite, and gadolinite.


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Rare earth mineral ores have been mined domestically by two companies at mines locations in California (bastnasite ore) and in Florida (monazite ore). The bastnasite mining was principally for the recovery of the rare earths. The monazite mining occurred in conjunction with the processing of heavy mineral sands for titanium and zirconium recovery.

US Operations


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Covert the as-mined ore into a product that may be marketed or treated further. This involves the removal of impurity compounds from the material being processed. For Rare Earths, this is complicated by the special operations required to separate the rare earths from each other (chemically).

Mineral Processing


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In placer deposits, monazite may occur as a minor constituent along with sillimanite, garnet, and magnetite, while the major minerals are ilmenite, rutile, zircon and quartz. Other minerals that may occur in some locations are: cassiterite, chromite, picotite, baddeleyite, cinnabar, gold and platinum. Beach sand deposits may exhibit considerable variation and thus their flow sheets may be variable in detail. The next figure shows a general overview of beach sand processing.



Example Flow Sheet Mineral Processing Gravity, Magnetic and Electrostatic Separations

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Some resources may be treated by utilizing the differences in properties (density, magnetic susceptibility, conductivity) of the minerals.


The ore undergoes grinding, spiraling, or other similar operations for the initial coarse upgrading of the ore. Magnetic separation removes the magnetic ore constituents which can be processed separately or discarded as waste. The refined ore is then digested with sulfuric acid at 200220oC. Rare earth sulfates and thorium sulfates are then dissolved and removed from the waste monazite solids by filtration. Rare earth elements are then precipitated as oxalates or sulfates. These precipitates undergo separations to form rare earth oxides.

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Monazite Ore Processing

US Potential Resources The separation of heavy minerals exploits small

differences in specific gravity, magnetic susceptibility and surface ionization potential (conductivity). Monazite is typically the heaviest.

Mineral Separations

Ilmenite, garnet, xenotime and monazite, in decreasing order of magnetizability, behave as magnetic minerals. Xenotime is more strongly magnetic than monazite. In electrostatic separations, ilmenite and rutile act as conducting materials. Xenotime is a poor conductor and can be separated from ilmenite. Leucoxene can cause problems in the separation of monazite from ilmenite. A reduction roast of at 600 c converts the iron oxide in leucoxene into magnetite and enables easy separation.

Example Flow Sheet

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Flow sheet uses gravity, magnetic and electrostatic separation at different separation factors



Bastnasite mining near Mountain Pass in southeastern California may be a the major source of rare earth metals in the U.S. again. The previous recovery process of the rare earths from this ore is shown in the following figure. The ore was initially crushed, ground, classified, and concentrated by flotation to increase the rare earth concentrations from about 5% to about 60% (REO). The concentrated bastnasite undergoes an acid (HCl) digestion to produce several rare earth chlorides.

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The resulting slurry is filtered and the solution is treated with sodium hydroxide to produce rare earth hydroxides. This rare earth hydroxide cake is chlorinated, converting the hydroxides to chlorides. Final filtration and evaporation yields the solid rare earth chloride products.


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30-35% solids. Rougher flotation brings the grade from about 9% to 20% REO. Tails are 1-2% REO. Four stage cleaning is used tailings are re circulated. The scavenger cons are reground and recirculated to roughers. After four stage cleaning, the final concentrate is thickened, filtered and dried The grade is 60% REO and the recovery is 65-70%

Mountain Pass Flotation

Example Flow Sheet Mineral Processing Flotation and Chemical Treatment

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A very complex flow sheet that requires significant energy and chemicals. Research may lead to alternative surface chemistry and flotation processes.


Simplified Bastanasite US Potential Resources


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Numerous minerals occur intimately intergrown in the rare earth Bayan Obo iron ore. In addition to REO, products include: magnetite, hematite, fluorite and niobium oxide. Bulk flotation is carried out on 90% < 74 micron material with sodium carbonate to adjust pH, sodium silicate to depress iron and silicate minerals and a sodium salt of oxidized petroleum (paraffin soap) as collector. The flotation tailings are taken to iron and niobium recovery circuits.

Bayan Obo Ore


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The cons are retreated after eliminating excess fatty acids and de sliming using sodium carbonate (pH 5-6), sodium silicate and sodium fluosilicate (depressants) and hydroxamic acid (collector). Rougher cons are 45% REO and has both monazite and bastnasite. Recovery is about 80%. Final treatment by cleaning or high intensity magnetic separation gives two fractions a primary 68%REO concentrate and a secondary monazite concentrate (36% REO), with respective recoveries of 25% and 36% - 61% total.

Bayan Obo Ore

Extraction of REO from Bastnasite

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Once a concentrate is obtained, then the metals of interest must be extracted from the material. Several approaches are possible, usually involving calcining and acid leaching. The solutions are then subjected to ion exchange or solvent extraction for purification.


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The sulfuric acid method has been used extensively in the US. Thorium and rare earths may be selectively, or totally, extracted depending on the conditions. The processes available are shown in the following figure. Rare earth recovery is based on double sulfate precipitation. Yttrium and the heavy rare earths are very soluble and go along with thorium.

Monazite Acid Treatment

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Monazite Acid Treatment


Alkali Treatment of Monazite US Potential Resources



Processing of the Products

The rare earth hydroxides and chlorides which are recovered from monazite and bastnasite, typically would undergo further processing to produce and recover individual rare earth metal compounds for a variety of applications. Several processes are used to produce rare earth fluorides, nitrates, carbonates, oxides, and pure metals. Processes used include fractional crystallization, fractional precipitation, solvent extraction, ion exchange, and reduction.


Separations Processing
Using fractional crystallization, one or more rare earths in a mixture are precipitated by changing the salt concentrations in solution through evaporation or temperature control. Fractional precipitation involves adding a precipitating agent to selectively remove a metal from solution. A vide variety of processes have been developed to recover specific rare earths by these two techniques.








Solvent Extraction
Liquid-liquid solvent extractions are often performed to separate a mixture of rare earths from each other, i.e., tributyl phosphate, which selectively extracts one rare earth from the others. Several stages of extractions are needed to separate each rare earth metal. Example extractants are shown in the next slide.




Ion Exchange
Ion exchange may be used to produce highly pure rare earths. Since the rare earths form trivalent cations (3+), a cation exchange resin might be used. For separating a mixture of lanthanides, the resin is first flushed with a solution such as cupric sulfate to prepare the resin for ion Exchange. A solution containing the lanthanides is then passed over the ion exchange resin. The lanthanides displace the cation, in this case cupric, on the resin surface.

Ion Exchange
To separate individual rare earth elements, an element containing a complexing agent, such as ammonium ethylenediamine tetra acetic acid (NH4+EDTA), is passed over the resin. The EDTA has a high affinity for rare earths, and the lanthanides are complexed with the EDTA and displaced by NH4+ on the resin. Each lanthanide has a different affinity for EDTA, and individual lanthanides can be separated and recovered as a result of these varying affinities.


Metal Production
High purity rare earth metals can be produced by the metallothermic reduction of rare earth halides. This process is used when high purity is required. After converting the rare earths into fluorides, they are reduced to the metallic state through contact with calcium or barium at high temperatures. Fused salt electrolysis is also used.


Introduction to Reduction
Rare earth oxides are the end products of mineral processing, leaching and separations. These oxides are extremely stable and their reduction is difficult. This is compounded by the metals melting points and vapor pressures. Conversion of the rare earth oxide to a halide and reduction of the halide is a useful approach. Fused salt electrolysis is also a useful approach. This would be most useful for the lower melting point rare earth metals. The preparation of a rare metal by forming an alloy and then recovered from the alloy is another potentially useful approach.

Introduction to Reduction
Every process has certain advantages and limitations with respect to applicability to individual rare earths, purity of product, yield of the metal, batch size, operational convenience, economy and environment. In spite of their chemical similarity to their trivalent states, the rare earths do display considerable variation in properties like melting point and vapor pressure. Another factor is the possibility of di-valency in some rare earth elements. This frustrates attempts to produce them by the usual chemical and electrolytic reduction processes.


Introduction to Reduction
Under nonstandard conditions, that are more typical of real processes, pure components are not typical, so the activities play a significant role in the reaction potential. Activities less than unity changes the Gibbs energy of the reaction and can lead to more favorable conditions. Methods would include: the formation of a metal with a low boiling point and hence vaporizing in a metallothermic reaction, recovery of the reduced metal as an alloy, and trapping the compound formed by the reduction in a complex slag. Also, carbothermic reduction under vacuum may be an efficient reduction at high temperatures.

The metallothermic reduction reaction may be represented by the equation: M(I)Xn + iM(II) = M(I) + iM(II)Xn/I Where M(I) is the metal to be produced, X is the anion, and i,n are the stoichiometric coefficients. Feasibility is determined by thermodynamics. Practicality is determined by melting point, boiling point, vapor pressure, density, viscosity (for liquid components), and characteristics such as chemical reactivity, and alloying behavior of the reactants and products.

These reactions are generally exothermic, and by suitable choice of reactants, materials and process conditions it has been possible to realize many of the characteristics listed. The reactants in a powder form favors better contact and once initiated a quicker reaction. If the heat generated during the reaction is sufficient to raise the temperature of both slag and metal above their melting points, and if they remain molten for a sufficient length of time, so that the denser metal settles by gravity with the immiscible (slag) layer on top, a metal ingot and solidified slag may be obtained. When the heat of reaction is insufficient, other types of products can form.

If the reaction occurs but the slag does not melt, the metal is formed as a powder in the slag. The slag is then leached away to obtain a metal powder. Metal in the form of powder can also form when the slag melts, if the melting point of the metal is very high and the metal is not sintered; but may form a coalesced sponge. Metal is recovered by slag leaching or vacuum distillation. By suitable choice of reductants, reactors and reaction conditions, the metal can usually be obtained in the chosen form. Rare Earth metals have been obtained by metallothermic reduction in the form of ingot, sponge or powder.

Metal ingot has been obtained using metallothermic reduction of rare earth fluorides as well as some of the chlorides using calcium as a reductant. Sponge of some rare earth metals have been produced from chlorides using lithium as the reductant. Rare metal powders have been obtained by reducing oxides with calcium. Certain rare earth alloys can be directly produced in ingot, sponge or powder form, followed by vacuum distillation. Purity depends on the purity of the starting materials, pure oxides, anhydrous chlorides or fluorides, reductants and reaction steps

Preparation of Rare Earth Chlorides

The preparation of rare earth chlorides for use as an intermediate for reduction has been accomplished through two routes: wet and dry. Wet: hydrated rare earth chlorides are produced by dissolving the rare earth oxide in HCl, evaporating to a syrup, and then cooled to form the hydrated chloride crystals. Dry: various methods are shown on the next slide, along with various reduction methods.


Preparation and Reduction of Rare Earth Chlorides

These methods to reduce REOs is complicated by the stability of these oxides. This requires significant purification prior to reduction or very complex refining schemes. Research on new reduction and refining methods may lead to alternatives.


Gibbs Energy Minimization for Dry Chlorides (1 Nd2O3 + 2 C + 2.5Cl2)


Purification of Rare Earth Chlorides

The major impurity is oxygen, either unconverted oxide or oxychloride. Carbon may be an impurity in carbo-chlorination. Vacuum distillation and filtration are the two methods used for freeing the rare earth chlorides. Vacuum distillation depends on the vapor pressure of the chloride. A second distillation may be required.


Chloride Reduction Processes


Chloride Reduction
Calcium, in a dolomite lined steel bomb, has been used to reduce cerium trichloride. Additional heat was provided by using calcium iodide booster reaction. After completion, the slag was removed and the metal vacuum melted to remove any excess calcium or calcium chloride slag. Purity was 98% and yield was 95%. Also used for lanthanum, praseodymium and neodymium.

Intermediate Alloy Process

Chloride reduction for the five metals (La, Ce, Pr, Nd and Gd) can not be applied to the higher melting point metals because of excess chloride volatilization and decreased yields. This can be overcome by making an alloy with a lower melting point metal. Yttrium metal as a yttrium-magnesium alloy by calcium reduction in the presence of Mg. Excess Ca and Mg were removed by vacuum heating. Also, Scandium metal reacted with calcium and/or magnesium

Kroll Type Processes

This would form a sponge. Lithium/sodium reaction of Yttrium chloride used a stainless steel vacuum retort in a glove box. Mo crucible. Evacuated with vacuum and refilled with Ar. 850 C for one hour and 900 C for 16 hours to remove excess Li or Na and Li and Na chloride

Preparation of Rare Earth Fluorides

Wet method the oxides are dissolve in hydrochloric or nitric acid. The addition of aqueous HF to this solution results in the precipitation of hydrated fluorides. The product is dried at 100-150 and then heated to 300 C in a vacuum or 600 C in a stream of anhydrous HF.


Preparation and Reduction of Rare Earth Fluorides


Gibbs Energy Minimization with Nd2O3 + 6HF


Reduction of Rare Earth Fluorides


Gibbs Energy Minimization CeF3 + 3Li = 3LiF + Ce


Gibbs Energy Minimization Calcium Reduction (2 NdF3 + 3.3 Ca)


Oxide Reduction Processes

Rare earths form highly stable oxides. Only calcium forms an oxide that is more stable. The stability of Mg is only marginally higher than that of the heavy rare earth oxides and comparable to those of the light rare earths. The relative stability of MgO makes its use problematic. The high melting point of CaO (2600 C) is a disadvantage.



Reduction-Distillation - Lanthanothermy
Similar to the Pidgeon Process for Mg can be used for samarium, europium and ytterbium (not obtained through halide routes). Vapor pressure measurements of the rare earth metals have indicated that lanthanum was the least volatile of the rare earths and that dysprosium had a vapor pressure nearly 300 times higher. Samarium and europium are also very volatile. Lanthanum oxide has one of the highest (-) heats of formation among the rare earth oxides. This led to a process for reducing these oxides with lanthanum and volatizing the products.

Samarium and Ytterbium were prepared by heating the oxides with La in tantalum crucible at 1450 C and 0.1 Pa for one half hour. Europium was prepared by reaction with La in the reactor shown. Heated to 1000 C at 0.02 Pa and then to 1100 and 1200 C. Samarium, if present, is not volatile.

Gibbs Energy Minimization Lanthanothermy (Tm2O3 + 2.2 La)

kmol 2.0 File: C:\HSC5\Gibbs\GibbsIn.OGI La





Tm La2O3 N2(g) Tm(g)





Temperature 2000 C


Other Reduction Distillation

The metal product needs to have an appreciable vapor pressure while every things else has a negligible vapor pressure. Is some cases Cerium or Zirconium are used. Samarium or europium oxides are mixed with (La, Ce or Zr) placed in a Mo container and placed in a vacuum retort.


Other Reduction Processes

Nd2O3 is reduced with calcium in a calcium chloride-sodium chloride melt at temperatures around 710-790 C. The product is dissolved in molten zinc, followed by vacuum distillation of the zinc. Neodymium oxide can not be reduced with Na; but if CaCl2 is added, then the sodium reacts with the CaCl2 to form Ca which can reduce the Nd2O3 at 1100 C. Metal is dissolved in Zn or Fe.


Electrolysis Introduction
Unlike the chemical reduction processes, electrolytic reduction does not rely on the availability of reducing agents and limited by the relative chemical stability. The Gibbs energy is related to the decomposition potential by: Go = nFEo It can be shown that an applied potential as small as 4 V should be adequate to dissociate even the most stable of compounds. This is only one of several requirements for effective methods to reduce stable rare earth compounds to metals. The process for electrolytic reduction of salts or compounds is basically simple.

Electrolysis Introduction
The salt of a metal is dissolved in another salt or mixture of salts that are kept molten in an inert container. Two electrodes a cathode and an anode are inserted into the molten bath and an electric current is passed through the circuit, with a voltage sufficient to reduce the salt. The molten salts (carrier electrolyte) serves as a solvent for the metallic salt to be reduced (functional electrolyte).


Electrolysis Introduction
The carrier electrolyte is chosen to have a desirable solubility of the functional electrolyte, sufficient conductivity for the electric current, a melting point below the desired operating temperature of the cell, low vapor pressure, and a greater stability than the functional electrolyte. These properties are normally obtained using an alkali or alkaline earth fluoride or chloride or a mixture of both. Considerable variability in cells used is seen: size, shape, materials of construction and disposition of the electrodes.


Electrolysis Introduction
Iron, Graphite, ceramics such as fire brick and alumina, refractory metals such as molybdenum and tungsten have all been used as cell materials. The anode is usually made of graphite and the cathode is iron, molybdenum or tungsten. Often the cell itself is the anode or cathode. Heat is supplied in two ways: the electrical current to the cell is used to supply the necessary heat or an external furnace is used.


Electrolysis Introduction
The largest amount of commercial rare earth metals are produced by electrolytic methods. La, Ce, Pr and Nd have melting points that permit recovery in the liquid state by electrolysis of relatively inexpensive chlorides at temperatures less than 1100 C. This facilitates metal slag separation, minimizes contamination of the metal, and enables continuous operation and high volume levels of production. The technical feasibility of producing high melting point rare earth metals (Gd, Dy and Y) has been demonstrated by using fluorides in place of chlorides in specially designed high temperature cells.

Electrolysis Introduction
The advantage of liquid metal recovery and low temperature operation have been realized even in the case of high melting point Rare Earth metals by using metals like: Cd, Mg, Zn, Mn, Cr and Co as cathode. These metals form liquid alloys with the rare earth metals as it electrodeposits and liquid product recovery is facilitated.


Chloride Electrolysis


Oxide-Fluoride Electrolysis


Recovery as Alloys


Refining of rare earths

Refining is complex as well and may involve vacuum melting, vacuum distillation, zone refining etc.


What are the thrusts and requirements for a research program in this area? Re-evaluate the current state of the technology available for rare earth resource processing. Identify and do research on those aspects that could be improved utilizing new mineral processing, extractive metallurgy and metal refining technology. Address the ultimate disposition of problematic elements in the solid and aqueous discharge. Help developed a trained engineering work force to tackle the research, development and production aspects. Finally, keep in mind that economics is always the bottom line in any resource recovery operation.

Gravity Magnetic Electrostatic Separation Improvements

Improved mineralogical methods for both initial design and improved plant operations (audits). Improved gravity separation devices (spirals, multi gravity, centrifugal concentrators, etc.) Improved magnetic separators (Rare earth rolls, HGMS, WHIMS, etc.) Improved electrostatic separators. Improved fundamental models


Improvements in Flotation Fundamentals and Equipment

Improved understanding of mineral surface chemistry. Column flotation. Improved instrumentation and control. Development of fundamental models for design and operation (JK SimMet, JK SimFlot, MinOCad, etc.).

Extractive Metallurgy
Much of the current utilized extractive metallurgy technology for rare earth elements was developed many years ago and there have been several significant advancements in our understanding of chemical processing methods for extraction and separation. Among these advancements have been: Excellent chemical thermodynamics screening methods using Gibbs energy minimization. Improved extraction methods based on increased understanding of chemical kinetics, reactor design and transport phenomena (heat, mass and momentum). Improved understanding of solution purification techniques, such as solvent extraction and ion exchange. Improved models and software for chemical reactor and flow sheet design.


Metal Reduction and Refining

Much of the current technology used for rare earth metal reduction was developed many years ago. There have been several significant advancements in metal reduction and refining technology. Some of the more notable ones are: Excellent thermodynamics screening methods using Gibbs Energy Minimization. Improved reduction and refining methods based on increased understanding of chemical kinetics, reactor design and transport phenomena (heat, mass and momentum). Improved understanding of the electrochemistry in fused salt electrolysis Improved materials of construction to handle hot corrosive systems

Kroll Institute for Extractive Metallurgy

Patrick R. Taylor Director, KIEM G.S. Ansell Distinguished Professor of Chemical Metallurgy EXPERTISE Mineral Processing Extractive Metallurgy Recycling Waste Treatment & Minimization Thermal Plasma Processing Brajendra Mishra Director, CR3 Associate Director KIEM, Professor of Metallurgical and Materials Engineering EXPERTISE Pyrometallurgy Electrochemistry Materials synthesis Waste Processing Recycling Molten Salt Processing Corby G. Anderson Harrison Western Professor of Metallurgical and Materials Engineering EXPERTISE Extractive Metallurgy Mineral Processing Recycling Waste Treatment & Minimization

Edgar E. Vidal Research Associate Professor of Metallurgical and Materials Engineering EXPERTISE Extractive and process metallurgy Pyrometallurgy Recycling Waste treatment and minimization.

D. Erik Spiller Research Professor of Metallurgical and Materials Engineering EXPERTISE Mineral Processing Leaching Project management: feasibility, engineering, construction management, operations

Gerard P. Martins Professor of Metallurgical and Materials Engineering EXPERTISE Process and extraction metallurgy Electrochemical systems Transport phenomena Reactor Design & kinetics

Paul B. Queneau Adjunct Professor of Metallurgical and Materials Engineering EXPERTISE Extractive and process metallurgy Pyrometallurgy Recycling Waste treatment and minimization.

Judith C. Gomez Research Assistant Professor of Metallurgical and Materials Engineering EXPERTISE Extractive and process metallurgy Materials synthesis Recycling Waste treatment and minimization


Industrial Projects - Current and Recent

Magnetic separation of a vanadium containing titaniferrous magnetite; Beneficiation of iron ores (oolites); Extraction of titanium from pickling solutions; Hydrogen sulphide sequestration; Aluminum dross treatment; Methods for treatment of electronic scrap for feed to a copper smelter; CR3 Beneficiation of Photovoltaic (and other) Functional Coatings CR3 Recovery of Rare Earth Metals from Phosphor Dust CR3 - Recycling of Bag-house Dust from Foundry Sand On-line diagnostic leaching of gold Autoclave oxidation of Enargite; Development on a new laboratory scale mill for evaluating operational changes in milling operations Ion exchange separation technologies for PGMs 2 Industry funded projects on Rare Earth extractive metallurgy Column flotation of a scheelite ore for improved recoveries and grades; Ammonium carbonate leaching of a copper-zinc oxide ore; Bacterial oxidation in the presence of chloride ion; Selective flotation of elemental sulfur from sulfides; Development of an improved method for measuring and predicting abrasive wear in milling operation


What KIEM can do for the mining and rare earth industry
Offer senior/graduate level (full or short) courses in mineral processing-extractive metallurgyrecyclingwaste minimization in the evening, by web or video, or on-site. Develop engineering talent for future employment. Encourage and market opportunities in industry to our undergraduate and graduate students. Perform research in support of industry goals. Maintain at least one significant program in the US with an emphasis on mineral processing-extractive metallurgy.

Primary References
Extractive Metallurgy of Rare Earths, C.K. Gupta and N. Krishnamurthy, CRC Press, 2006 Various technical publications and patents


Hill Hall, home of KIEM Please come see what were up to. THANK YOU.
The Kroll Institute for Extractive Metallurgy George S. Ansell Department of Metallurgical and Materials Engineering Colorado School of Mines