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By J. L. Havenga, L. J. van der Walt, J. T. Nel, H. Bissett

"SynopsisNew technologies used to manufacture high-quality components, such as direct laser sintering, require spherical powders of a narrow particle size distribution as this affects the packing density and sintering mechanism. The powder also has to be chemically pure as impurities such as H, O, C, N, and S causes brittleness, influence metal properties such as tensile strength, hardness, and ductility, and also increase surface tension during processing.Two new metal powder processes have been developed over the past few years. Necsa produces zirconium powders via a plasma process for use in the nuclear industry, and the CSIR produces titanium particles for use in the aerospace industry.Spheroidization and densification of these metal powders require remelting of irregular shaped particles at high temperature and solidifying the resulting droplets by rapid quenching. Spherical metal powders can be obtained by various energy-intensive methods such as atomization of molten metal at high temperatures or rotating electrode methods. Rapid heating and cooling, which prevents contamination of the powder by impurities, is, however, difficult when using these methods for highmelting- point metals. For this reason plasma methods should be considered.Thermal plasmas, characterized by their extremely high temperatures (3000–10 000 K) and rapid heating and cooling rates (approx. 106 K/s) under oxidizing, reducing, or inert conditions, are suitable for spheroidization of metal powders with relatively high melting points. Thermal plasmas for this purpose can be produced by direct current (DC) plasma arc torches or radio frequency (RF) inductively coupled discharges. In order to obtain chemically pure spheroidized powder, plasma gases such as N2, H2, O2, and CH4 cannot be considered, while Ar, Ne, and He are suitable. Neon is, however, expensive, while helium ionizes easily and it is therefore difficult to obtain a thermal helium plasma at temperatures higher than 3000 K. Therefore argon should be used as plasma gas. Residence times of particles in the plasma region range from 5–20 ms, but this is usually sufficient as 7–8 ms is required for heating and melting of titanium or zirconium metal particles in the 30 µm size range at 3500 K. In this study the melting and spheriodization of titanium powders was investigated by DC non-transferred arc and RF induction plasma methods. The powders were characterized before and after plasma treatment by optical microscopy and scanning electron microscopy (SEM) to observe if any melting or spheroidization had occurred."

Jan 1, 2015

By Willis G. M

Preliminary experiments have shown that, when used in a fusedchloride electrolyte, titanium carbide anodes dissolve yielding lower titanium chlorides which nlay be electrolysed in situ to produce a cathode deposit of pure titanium metal. The anode residues are easily withdrawn from the cell. Further experiments have established the operating conditions for maximum efficiency in the process.The process is essentially two-stage, viz.: (1) titanium carbide production, (2) electrolysis producing metal. Power requirements appear to be moderate and this fact, combine·d with the simplicity of the process make it attractive as a possible method for the production of titanium.INTRODUCTIONDue to the high reactivity of titanium and its, affinity for oxygen and nitrogen, the extraction of this metal generally involves the use of halide. compounds as intermediates. For instance, magnesium reduction of titanium tetrachloride is the basis of the well established Kroll process and electrolysis of the lower chlorides in a molten salt bath has been proposed by Cordner and Worner (1951, p. 358) and others (Brenner and Senderoff, 1952, 223C; The TitaI Company (Inc.), 1952) as means of production of the metal. Thedifficulty of preparation of these compounds prompted a search for an alternative extraction process. The fact that aluminium, an equally reactive metal, has been prepared by electrolysis using aluminium alloy anodes suggested the possibility of a similar process for titanium production.The Titan Company (Inc.) (1952) has patented the use of crude titanium metal anode, but it was thought possible that a metallic compound, such as the carbide, could be used for this purpose. Although Lorenz and Kaufler (1909) suggested the use of carbide anodes for metal production, no...

Jan 1, 1956

By Paulo Masiero

Sintered titanium carbide has been extensively used since the early 1980s for demanding wear-resistant applications and, in particular, in environments characterized by high temperature and oxidation. Thanks to its physical characteristics, especially its low density, titanium carbide (TiC) has been successfully applied in the manufacture of cassette guide rollers for hot steel rolling. However, the peculiar characteristics of the sintered Ti carbides make it difficult their redressing and hence this has always represented the limit for a more extensive application. Very often iron based alloys are preferred even if, in general, they are less cost effective just because they are easier to be redressed by turning. The availability of a simple, compact, fully automatic and reasonably priced CNC machine; specialized in the grinding of guide rollers and able to operate accurately and efficiently -both in contour and in plunge- can definitively solve TiC’s redressing problems and render its use even more widespread and attractive.

Oct 30, 2017

By Bora Derin

The synthesis of titanium diboride (TiB2) by carbothermal reductions of TiO2 and B2O3 was investigated. For this aim, TiO2, B2O3 and carbon black powders were dried, weighed out and mixed in stoichiometric molar proportions (TiO2:B2O3:C = 1:1:5). The experiments were carried out in a graphite resistance furnace in argon media using different range of temperature (1400- 1700 °C) and time (0 and 15 min). The phase analyses observation of the products were examined by using XRD.

Jan 1, 2008

By Alan Stanley

THE Maclntyre Development of National Lead Co. is located at Tahawus, N. Y., in the heart of the Adirondack Mountains. Operations involve the mining and concentrating of a titaniferous iron ore to produce ilmenite and magnetite concentrates. A general description of the operation and metallurgy has been given by Frank R. Milliken.1 Pigment plant production demands that the MacIntyre mill produce a 44.7 pct. TiO2 ilmenite concentrate. To achieve the required ilmenite grade and tonnage it is important that the table concentrate grade be closely controlled. Unfortunately, however, the titaniferous orebody which feeds the Maclntyre mill is not uniform. Ore dressing characteristics vary from one end of the orebody to the other, and from one level to the next.. The changeable nature of the mill feed precludes a single adjustment of the equipment for long periods of time. Thus the operators must constantly watch the equipment to insure a uniform concentrate from the fine and coarse tables and Wetherills, or dry magnetic separators. Chemical assaying of mill products requires about 4 hr from the time the sample is taken until assay results are obtained, and this is available only on a two-shift basis. The ore may change rapidly, even several times during a shift, so that assay results lose most of their control value by the time they are reported to the mill operating crew. Members of the crew have therefore tried to evaluate the table and Wetherill concentrate by visual inspection, since through long experience the shift operators, under most circumstances, can gage closely the grade of the mill products. However, there are times when the, physical nature of the ore is radically different from normal. Under these conditions visual inspection is of no value, and at such times final ilmenite as low as 43 pct TiO2 has been produced and shipped before the assay results have been received. The specific gravity method of assaying for TiO2 has been attempted to eliminate the shipping of ilmenite below normal grade as well as to help control day to day and hour to hour mill production. Table I shows the minerals found in the Maclntyre ore along with their average weight proportions and specific gravities. The first two products considered for the specific gravity method were fine and coarse table concentrates. It was reasoned that these products were essentially ilmenite with the higher specific gravity gangue minerals. Since they were always produced the same way, and the desired grade of TiO2 was always constant, the specific gravity of these materials would increase or decrease as the amount of ilmenite increased or decreased. Thus for table concentrates which assayed 40 pct TiO2 a constant gravity would invariably be obtained, and as the TiO2 value changed the specific gravity would change in direct proportion. The third product considered was Wetherill ilmenite. It was assumed that a desired grade of 44.7 pct TiO2 would also always contain the same amount and type of gangue minerals along with the ilmenite, and thus would always have the same specific gravity. As the TiO2 value of the ilmenite concentrate changed so would its specific gravity. Dr. Kenneth Vincent, chief metallurgist of the Baroid Division of National Lead Co. at Magnet Grove, Ark., ran specific gravity tests on 17 samples of the desired products. The lowest specific gravity reading assayed the lowest in TiO2 and as the specific gravity increased the trend was for the TiO2 assay to increase, see Fig. 1. Since these results warranted further investigation, a 500-g capacity Torsion balance and 250 ml Le Chatelier specific gravity bottles were obtained. [ ] Shift samples of fine table concentrate, coarse table concentrate, and final ilmenite were tested. Each sample was split and 85 g weighed on the Torsion balance. The Le Chatelier bottle was filled with water to a zero mark. To avoid wetting the neck of the bottle it was found necessary to do this

Jan 1, 1952

By D McCoy

Titanium feedstocks are the building blocks of the titanium value chain. They can be mined directly, as is the case for ilmenite, leucoxene and rutile, or manufactured from ilmenite by extracting various quantities of non-TiO2 components from the ore by chemical and/or thermal processes.While feedstocks can be grouped into categories of materials with similar characteristics, they are essentially unique products from very different mining locations around the world. In fact, no two feedstocks are exactly the same. As such, the variations between the available feedstocks, in combination with the permutations in processing technologies to turn the feedstocks into titanium pigment or metal, mean that choices between feedstocks are specific to the location in which they are utilised.In this paper, the authors examine the key requirements of titanium feedstocks to the TiO2 pigment and metal sectors. Apart from the well known differences between feedstock choices for the sulfate and chloride process, the more opaque considerations in feedstock sourcing are examined.

Oct 5, 2011

By Newell H. Orr

Titanium's performance characteristics in acidic oxidizing and mildly reducing environments make it applicable to numerous currently defined and many projected hydrometallurgical applications. With titanium's current and projected availability and price stability increased use in pressure leach, piping systems and electrorefining is practical.

Jan 1, 1983

By Joseph Gambogi

In 1998, approximately 57,000 tons of titanium metal was consumed in the form of mill products (1). Only about 5% of the 4 million tons of titanium minerals consumed each year is used to produce titanium metal, with the remainder primarily used to produce titanium dioxide pigment. Titanium metal production is primarily based on the direct chlorination of futile to produce titanium tetrachloride, which is then reduced to metal using the Kroll magnesium reduction process. The use of titanium is tied to its high strength-to-weight ratio and corrosion resistance. Aerospace is the largest application for titanium. In this paper, we discuss all aspects of the titanium industry from ore deposits through extraction to present and future applications. The methods of both primary (mining of ore, extraction, and purification) and secondary (forming and machining) operations will be analyzed. The chemical and physical properties of titanium metal will be briefly examined. Present and future applications for titanium will be discussed. Finally, the economics of titanium metal production also are analyzed as well as the advantages and disadvantages of various alternative extraction methods.

Nov 26, 1999

By Stanley J. LeFond, Langtry E. Lynd

Elemental titanium has become famous as a space age metal, because of its high strength/ weight ratio and resistance to corrosion. However, the major use is in the form of titanium dioxide pigment, which because of its whiteness, high refractive index, and resulting light-scattering ability, is unequaled for whitening paints, paper, rubber, plastics, and other materials. A relatively minor use is in welding rod coatings, in the form of the mineral, rutile. United States consumption of titanium dioxide for these applications in 1973 was as follows: pigments, 891,000 st; titanium metal, 40,000 st (=24,000 st metal) ; and welding rod coatings, 10,000 st. The only commercially important titanium ore minerals at the present time are ilmenite, and its alteration products, and rutile. Titanium was discovered by Gregor in 1790, as a white oxide which he recovered from menaccanite, a variety of ilmenite occurring as a black sand near Falmouth, Cornwall. Barksdale (1966) states that the fundamental chemical reactions on which the present day titanium industry is based were known before 1800, although it was not until 1918 that these pigments were available commercially on the American market. Pings (1972) outlines the early history of the titanium industry in the United States, referring to the work of Guise (1964) and others: "Mining of titanium minerals in the United States began sometime between 1880 and 1900, in Chester County, Pennsylvania. Small quantities of rutile were also produced during the time in North Carolina and Georgia. In 1901 rutile was mined from a deposit near Roseland, Va., and was used in making titanium chemicals and for coloring ceramics. Ilmenite in the deposit was produced as a separate item in 1913, and rutile and ilmenite were obtained from this deposit through 1921. The mining of titanium bearing beach sands began in 1916 near Mineral City and Pablo Beach, Fla., for the purpose of making titanium tetrachloride to be used in tracer bullets, flares, and smokescreens. The titanium pigment industry was founded in 1918. By 1928 a large part of the domestic production of rutile, ilmenite, and zircon came from Florida. However production ceased in 1929 in Florida with the mining of newly discovered deposits in Virginia which were mined until 1968. The discovery of new deposits in Florida, and the development of better mining and concentrating methods for lowgrade sands, led to a return of activities in this area. The large deposits near Tahawus, N.Y., were brought into production in 1942 by National Lead Co. (now N L Industries Inc.), and by 1949 this company was the lead¬ing producer of ilmenite in the world. In 1948 the extensive deposits of ilmenite and ilmenite-bearing iron ores were discovered in eastern Quebec." The beginning of the modern titanium metal industry was in 1948, when E. I. du Pont de Nemours & Co. produced the first metal. U.S. Bureau of Mines reports, which gave details of the Kroll process, together with the attractive properties of the metal for

Jan 1, 1975

By Kerry J. Stanaway, Thomas E. Garnar

Titanium was discovered in 1791 and, four years later, was named after the Titans of Greek mythology. Titanium metal was first made in 1910, but was not used commercially until the 1950s when it was nick-named The Wonder Metal of the Age. The first titanium dioxide (TiO2) white pigments were produced commercially in 1915; more than 90% of the titanium minerals produced in the world today are used in the manufacture of white pigments. The remaining 10% are used to manufacture titanium metal and other uses such as welding rod fluxes. Titanium mineral mining began in the United States between 1880 and 1900 in Chester County, Pennyslvania. Rutile from a deposit near Roseland, VA, was mined in 1901. The use for the rutile was limited to production of a few titanium chemicals and for coloring ceramics. Larger scale mining for ilmenite, rutile, and zircon began in Florida to provide chemical materials for use in World War I in 1918. This mining ended in 1928. Large scale mining of titanium minerals in Australia began when Benick, Anderson, and Porter (later called Tamco) started mining the beach sands at Yamba in New South Wales in 1935. Ilmenite production from beach sands in the State of Kerala in southwestern India also began in the 1930s. The 1940s saw many changes in titanium mineral mining. Extensive deposits of ilmenite and ilmenite-bearing iron ores were discovered in eastern Quebec. The Pigments Department of E.I. Du Pont de Nemours & Co. lost their high grade Indian ilmenite supply after World War II began, and they were forced to use lower grade ilmenite from National Lead's (now NL Industries) Sanford Lake Deposit, near Tahawus, NY, in the Adirondack Mountains. At the end of the war, Du Pont undertook an intense search for a domestic ilmenite source. With the cooperation of the US Bureau of Mines, Du Pont geologists found a very large deposit east of Starke, FL, in 1946. In 1948 Du Pont entered into a contract with Humphreys Gold Corp., who operated a heavy minerals mine near Jacksonville, FL, to construct a plant and operate it for a period of ten years. The plant started up in 1949 and operated under Humphreys' management until the contract expired in 1958. Du Pont has operated the plant since that time. In 1956, a second plant was designed and built by Du Pont a few kilometers northeast of the town of Lawtey. The 1960s saw titanium mineral production expand in the southeastern US with Humphreys' contract mining Du Pont's ore body at Folkston, GA. In the early 1970s. American Cyanamid and Union Camp Paper Co. formed a joint venture company, Titanium Enterprises (TE), to mine and separate titanium minerals from Union Camp's ore deposit southwest of Green Cove Springs, FL. In 1975 the TE plant was shutdown and later sold to Associated Minerals (USA), Inc. (AMC), a subsidiary of Renison Goldfields Consolidated Ltd., an Australian company. It now operates under the name RGC (USA). Mineral production grew in the 1970s with the development of extensive heavy mineral deposits at Eneabba in Western Australia and Richards Bay in the Republic of South Africa. The 1980s saw the construction of a very large ilmenite mine and synthetic rutile processing plant in the state of Orissa southwest of Calcutta, India. At the same time, concern for titanium mineral shortages expected by the end of this century, gave rise to a flurry of exploration activity during the mid 1980s. As a result, large deposits were found in Virginia and North Carolina. New deposits were also discovered in Australia. Fig. 1 shows the distribution of world titanium deposits and mines. The world TiO, production capacities are given in Table 1.

Jan 1, 1994

By J. V. Thompson

The Powderhorn complex as a source of perovskite (calcium titanate) containing about 1.5% rare earths has been examined in several recent feasibility studies. Much promising exploration and process research has been done in recent years. This paper is presented with cautious optimism and with the acknowledgment that there may be some technical and economic areas yet to be explored. The Powderhorn carbonatite and alkalic stock in Gunnison County, Colorado, lies about 203 airlines km southwest of Denver at an elevation of 2450 to 2750 m (see Figures land 2). All of the mineable ore bodies are owned by Buttes Resources Company of Houston, Texas.

Jan 1, 1990

By Yoshio Waseda, Tetsuya Uda, Tom H. Okabe

"Halide salt has been tested as a reductant for producing titanium powder directly from TiCl4. From the results of thermodynamic investigation for several rare earth chloride systems, DyCl2 was found to be used for the reduction of TiCl4 instead of the conventional metallic reductant. When TiCl4 was fed into molten salts containing DyCl2 at 1073K, titanium powder of several ten micron meters in diameter was obtained. In contrast to the sponge titanium produced by the conventional Kroll process, the present new process using a halidothermic reduction in a reactive molten salt appears to be suitable for producing metal powder. From the thermodynamic point of view, the resultant DyCl3 can be reduced to DyCl2 by magnesium. By utilizing the multivalent halide redox couple, some possible ways of titanium powder production directly from TiCl4 by magnesiothermic reduction are shown to be feasible. This can also be applied to the development of a new continuous titanium reduction process.1 IntroductionTitanium and its alloys show attractive mechanical properties such as strength-to-weight, rigidity-to-weight ratios and excellent corrosion resistance. Nevertheless, the application of titanium alloys is limited compared to other structural materials (e.g. steels, aluminum alloys) because of its high cost of production. Currently, almost all of titanium is produced by metallothermic reduction of TiCl4 by magnesium (Kroll process)[1] in an airtight metallic reactor. This process is batch type and labor intensive. Therefore, many attempts to develop new process for producing titanium are investigated so far."

Jan 1, 2000

By G. Minhas, M. Pule, Y. Laffitte, M. c. McGurn, T. Tzanetakis, Peacey. J., R. Susilo

Titanium (Ti) metal production from titanium tetrachloride (TiCl4) using magnesium (Mg) as a reducing agent is the well-known Kroll process. A chloride route is used to avoid oxidation of the titanium sponge. The sponge is consolidated into ingots and can then be made into powder by melting and atomizing or by hydriding/dehydriding. Attempts at direct powder production have met with difficulties, including low Ti yield and the formation of very fine particles (particles between 25-100 µm are desired). This paper discusses two methods to produce Ti powder in a molten salt medium using magnesium powder as a starting material instead of a pool of molten magnesium. The first method is a direct reduction of gaseous TiCl4 injected in the melt with the magnesium powder in suspension in the molten salt. The second method is a two stage TiCl4 reduction reaction where recycled Ti was used to form titanium dichloride (TiCl2) in the first stage followed by addition of magnesium powder into molten salt in the second stage. A correlation between Ti yield and processing variables such as TiCl4 to Mg ratio, Mg particle size, TiCl2 concentration in the melt, and reaction temperature was studied. The Ti powder formed was also analyzed for particle size distribution. Despite challenges and difficulties encountered, this paper shows some promising results which could provide guidance to others working on direct Ti powder production.

Jan 1, 2015

By D. S. van Vuuren

Industrial production of titanium occurs via the batch-wise reduction of titanium tetrachloride (TiCl4) with a reducing metal, being magnesium in the Kroll process, or sodium in the Hunter process. In the search for low cost titanium, the CSIR is developing a continuous process to produce titanium powder directly via metallothermic reduction of TiCl4 in molten salt, dubbed the CSIR-Ti process. The move to a continuous process has been attempted by a number of organizations, but was until now always met with failure, due in no small part to challenges inherent in the process chemistry. The reaction between TiCl4 and the reducing metal can occur directly, when TiCl4 or any titanium sub-chlorides present, comes into contact with suspended or dissolved reducing metal. The reaction can also occur indirectly, without any physical contact between the reacting species, via an electronically mediated mechanism. The reaction mechanism via electronic mediation can cause TiCl4 to react at the outlet of the feed port, rapidly causing blockages of the TiCl4 feed line. The electrical conductivity of the metal reactor can also cause the electronically mediated reaction to favour the formation of titanium sponge on the reactor walls and internals, rather than titanium powder. Various methods were investigated to overcome the problem of blockages in the TiCl4 feed line, e.g. mechanical removal, sonic velocities, dilution of the TiCl4 and the use of ceramic feed lines. This article discusses problems experienced with the continuous feeding of reagents, and various methods attempted are shown and discussed. Information is also given on the morphology, chemical composition and suitability of the final titanium powder for powder metallurgical application as presently produced by the CSIR-Ti process. Keywords Titanium dioxide, titanium nitride, carbo-thermic reduction, ilmenite, slag, tunnel kiln, residence time.

Jan 1, 2011

By Langtry E. Lynd

The titanium industry is based on the unique properties of titanium dioxide and titanium metal. Because of its whiteness, high refractive index and resulting light scattering ability, titanium dioxide in its two main allotropic forms, rutile and anatase, is the predominant white pigment for paints, paper, plastics, rubber, and various other materials. Titanium metal, because of its high strength/weight ratio and resistance to corrosion, is widely used for aircraft, both in airframes and engines, for powerplant surface condensers, and a wide variety of chemical processing and handling equipment. U.S. production of titanium dioxide pigment in 1979 was about 658,000 tons - 2/, valued at about $770 million. Net shipments of titanium mill products were around 19,000 tons, worth about $380 million. These two major uses account for over 96% of domestic titanium consumption. The third largest application, the use of rutile for coating welding rods, required about 9,500 tons of rutile concentrate, worth about $4 million. Other applications of titanium-bearing raw materials include the manufacture of titanium carbides, ceramics, and chemicals, and the recently developed use of ilmenite as a substitute for barite in well-drilling muds.

Jan 1, 1980

By Worner H. K

The paper briefly summarises the work of the Titanium Research Section in the Metallurgy Department of the University of Melbourne and mentions the development of a new electrolytic process for titanium production. This process utilises the "hot-spot" cathode technique and titanium carbide anodes. An introduction is given to three further papers on titanium metallurgy to be presented to the Institute.INTRODUCTIONThe unique combination of strength, lightness and corrosion resistance possessed :by titanium and its, alloy has made them of great interest to engineers. However, high cost, difficulties of production and limited knowledge of techniques of application restrict their usage at present almost exclusively to high priority armaments.The cost of the metal is divided between extraction and processing and much research has been carried out to devise new and cheaper methods for winning the metal from its ores. Processing costs will be reduced when production volume increases.Extraction research is proceeding rapidly overseas and Kellogg (1955, p. 72) reports that 'at least seventeen companies in the U.S.A. are interested in titanium production. Of these, two are producing the metal by a modified Kroll process, three are building Kroll plants and the remainder are in various stages of research activity. The Horizons Corporation alone is contemplating electrolytic extraction and is building a pilot plant. Steinberg et aI. (1955, p. 252, p. 332) have reported the early work done by the HorizonsCorporation on electrolysis of potassium fluotitanate and titanium monoxide in fused salt electrolytes. Of these two, the former appears to be the more attractive process.

Jan 1, 1956

By S. J. Oosthuizen

This paper examines innovation in relation to the availability of anew material: the metal titanium. The paper aims to highlight the need for the inclusion of entrepreneurial innovation as a necessary focus area in the development of a titanium metal value chain. Both the Department of Science and Technology (DST) and the Department of Mineral Resources (DMR) have identified the creation of titanium metals production capabilities as a key growth area for South Africa. Using historical literature as a source of data, the activities of selected innovators who used titanium metal as a central component in their success, were investigated. The origin of the process innovation behind the titanium metals industry, and two titanium product innovations: namely, medical implants and sporting goods, were detailed as case studies. It was found that individual innovators were responsible for the creation, and rapid growth, of the titanium industry and titanium product applications. There is a need to link the current research and development into titanium metals production with individuals and organizations capable of commercializing innovative processes and products.

Jan 1, 2011

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