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By T. H. Courtney, B. R. Murphy

"Nominal room temperature mechanical alloying (MA) has been used to synthesize the high melting temperature NbC and Cu-NbC composites. Elemental powders of Cu and Nb were alloyed in the presence of either graphite or hexane to form nanocrystalline NbC or a Cu-NbC composite. Through control of hot-isostatic-pressing (H/Ping) parameters, we have been able to minimize microstructural coarsening during densijication, and have processed fully dense bulk compacts of both single phase NbC and two-phase Cu-NbC while maintaining a nanocrystalline or near-nanocrystalline structure. These materials generally exhibit high strength and low fracture toughness. However, mechanical properties vary significantly depending upon the Cu content and the method of NbC synthesis (graphite or hexane).INTRODUCTIONMechanical alloying (MA) has been recently used to synthesize a variety of inorganic solids; sulfides (1-2), nitrides (3), borides (4), and carbides (3, 5-8). One advantage of this processing route is that synthesis of fairly high melting temperature materials takes place at what is nominally room temperature. Another advantage is that the structures generated are often nanocrystalline in scale, with attendant interesting properties. The consolidation of these fine structures into near fully dense or fully dense materials while limiting microstructural coarsening is a challenge that has just recently seen limited success (5, 9). We report here on some recent studies of ours dealing with crystallite size and structural analysis of NbC and CuNbC composites consolidated to full density from mechanically alloyed powders. Bulk mechanical properties and their dependence on milling parameters are also presented."

Jan 1, 1994

By Andrew J. Troop

"VAUGHAN THOMPSON designed the Thompson retrievable diamond drill wedge and reaming assembly in 1948. Since 1950, the Hudson Bay Exploration and Development Company, Limited has used the method extensively. The wedge, setting tool, and reamer have been modified slightly since they were first introduced. In 1951, Mr. Thompson designed the Thompson arc cutter. The purpose of this tool is to decrease effectively the diameter of the arc cut, using standard drilling tools. This directional drilling device is usually employed when a branch hole is desired. The Thompson arc cutter has been used with success at Birch Lake, Saskatchewan, at the property of Cuprus Mines, Limited, Manitoba, and at Thompson Lake, Manitoba.UsesThe Thompson retrievable wedge provides a simple method for:(1) Re-drilling lost core sections(2) Re-sampling sections of old holes(3) By-passing lost tools Correcting the direction of a hole(4) Drilling a branch hole to obtain intersections at a higher elevation than the original holePrevious to the spring of 1951, the wedge was used only for the first four of these purposes. Recently it has been employed extensively for drilling branch holes."

Jan 1, 1953

By P. T. Bissert, D. S. Yantek, L. Yan, M. D. Klein

Federal regulations require that refuge alternatives (RAs) be located within 305 m (1,000 ft) of the working face and spaced at one-hour travel distances in the outby area in underground coal mines, in the event that miners cannot escape during a disaster. The Mine Safety and Health Administration mandates that RAs provide safe shelter and livable conditions for a minimum of 96 hours while maintaining the apparent temperature below 35 °C (95 °F). The U.S. National Institute for Occupational Safety and Health used a validated thermal simulation model to examine the mechanisms of heat loss from an RA to the ambient mine and the effect of mine strata composition on the final internal dry bulb temperature (DBT) for a mobile tent-type RA. The results of these studies show that 51 percent of the heat loss from the RA to the ambient mine is due to radiation and 31 percent to conduction. Three mine width and height configurations and four mine strata compositions were examined. The final DBT inside the RA after 96 hours varied by less than 1 °C (1.8 °F) for the three mine width/height configurations and by less than 2 °C (3.6 °F) for the four mine strata compositions.

Jan 1, 2016

By M. C. Malamphy

A general description of the activities and results of bauxite investigation by the Bureau of Mines at its bauxite project in saline and Pulaski Counties, Ark., has been given in Report of Investigations 4251. The factual data obtained during the project are reported in a series of Reports of Investigation beginning with No. 4251, of which this is the eleventh. The-data are accompanied by maps showing the location of holes drilled and the deposits developed. Each area upon which work was done is reported by half townships. Each bauxite deposit investigated was assigned a name and a number for ready reference and identification, and its location and name are shown on the appropriate half-township map. The description of each halt township is followed by a description of each deposit developed in that halt township. The 14 halt-township maps and 77 detail maps of the bauxite deposits in this series at reports give the locations and numbers of all the holes drilled on the project, except the deep holes drilled to test the geophysical anomalies. The locations of those holes show on figure 13 in volume 1. The descriptions of the deposits developed are followed by complete detailed logs of the drill holes. Many of the widely spaced exploratory holes did not discover bauxite of minable thickness and grade. The pertinent information obtained tram the widely spaced exploratory drill holes has been summarized and tabulated, and a table for each halt township is given with the discussion of that area.

Jan 1, 1948

By John C. LaScola

The Bureau of Mines investigated coal storage silos to determine how gassy coal must be for methane accumulations in a silo to become hazardous and where such accumulations are likely to occur. Methane concentrations were measured in the open space above the stored coal pile, in the pile, and in the reclaiming area. No methane layering was found in closed-top silos. Reclaiming areas were as gassy as the top part of the silos. Coal samples were collected from the conveyors entering the silos in order to assess the gassiness of the coal. No simple correlation was found between the gassiness of the coal stored and the measured methane concentrations. However, at mines where the average 24-hour gas emission from the conveyor belt samples was 14 ft3/ton or more, fans or open tops were used. It appears that a large fraction of the methane released during storage remains in the void space between the coal particles.

Jan 1, 1980

By K. Morin

"Silver and gold leaching by cyanidation is a well-known process used around the world. This reaction is often accompanied by the leaching of other species throughtout the cyanidation circuit that causes the diversion of cyanide towards non valuable by-products (SCN-, Cu(CN)x, Fe(CN)x, etc.). One of the detrimental impacts of the formation of these by-products is the precipitation of silver-cyanide complexes that occurs when cyanide concentration is too low. Without any extra-addition of free cyanide, the precipitated silver is lost and cannot be recovered causing an important economic loss. To overcome silver precipitation, cyanidation circuits are often operated at higher cyanide concentrations. Recently, COREM’s research team has been working on a technology to measure and control silver precipitation during the cyanidation process. Moreover, a methodology has been elaborated in order to evaluate threshold cyanide level which corresponds to the cyanide concentration at which silver starts to precipitate. This technology has been tested on site on a real cyanidation circuit at Agnico Eagle’s LaRonde mine."

Jan 1, 2014

By Glen Frank, David R. Chapman

Determining the number of boulders and cobbles that will be encountered in the tunnel envelope is one of the most difficult problems confronting the geotechnical engineer in the design of tunnels in glacial terrain. This issue is very important to the contractor, both in determining what methods will be used to construct the facilities and the advance rate that can be achieved for the chosen construction methods. The cost of constructing tunnels by pressurized face tunneling techniques is very sensitive to accurate characterization of the very coarse fraction (large cobble and boulder sized clasts), and no standard method is current available for characterizing boulders and cobbles. Careful use of large diameter borings and the sampling and analytical techniques outlined in this paper can provide a means to answer this difficult question. By performing large diameter borings and carefully recording and sampling the cobbles and boulders encountered, an estimate for the amount of these materials present in the formations sampled can be provided. Using this method allows the designer to communicate the expected geologic conditions to the prospective bidders in a manner that is both definitive and defensible. This paper describes the method as it was used in conjunction with the design of a large diameter sewer tunnel in the Columbus, Ohio area.

Jan 1, 2005

By S. Sakurai, N. Shimizu

The stability of slopes is a crucial problem not only in open pit mines, but also in civil engineering situations. The deformational behaviour of slopes is in general monitored during/after the excavation by carrying out field measurements where displacement measurements are commonly adopted. In monitoring the slope stability it should be emphasized that the measurement results must be properly interpreted so as to assess whether the slopes are stable or become unstable in the future. In order to interpret the data, back analysis is extremely useful. In this paper a slope stability monitoring system is described. It consists of displacement measurements by GPS, and a back analysis of measured data. The use of GPS has a great advantage, because of the fact that continuous displacement measurements with high accuracy for a large extent of concerned area can be easily achieved. On the other hand, the back analysis can reveal the mechanical characteristics of the ground, which make it possible to assess the stability of slopes quantitatively.

Jan 1, 2006

By Anastasia Alksnis

Pyrrhotite is an iron deficient, low nickel content sulfide mineral that is commonly associated with pentlandite, a nickel-rich sulfide; and are both main components of the nickel ore mined in Sudbury. Pyrrhotite tailings generated in the concentration of Ni ores are stored in tailing reservoirs and presents serious environmental risks including acid mine drainage. This study investigated the potential of converting pyrrhotite into a valuable resource through the use of fluidized bed roasting, in which the mineral will be oxidized to produce iron oxide and SO2 gas. These products can then be used to create iron for high-grade steel and elemental sulfur. Thermogravimetric analysis of Sudbury pyrrhotite was performed to study the oxidation kinetics, supporting the feasibility of this process. Further, energy and materials balance was carried out to establish the basic parameters of a possible roasting process.

By H. Nejati

Experimentally, the Semi-Circular Bending Moment (SCB) fracture toughness test results of Basalt Specimens Under Illumination (BSUI) have shown reduction in fracture toughness and failure force as a result of micro-cracking. The fractographic investigation of BSUI confirms initiation and extension of micro-cracks. Determination of a relation between strength reduction (herein fracture toughness reduction) and density, location and orientation of thermo-mechanical induced cracks due to microwave radiation is critically important. Numerical modeling can bridge strength reduction and the density of thermal microcracks generated due to microwave radiation. Discrete Element Modeling (DEM) is a power tool for simulation of micro-crack initiation, coalescence into macroscopic fractures and failure mechanisms in brittle rock specimens under different stress regimes (herein combination of pure tensile stress due to SCB testing, and thermal stress due to microwave radiation). For this purpose, a DEM modeling of SCB testing of basalt using EDEM (i.e., a DEM based software). DEM models are calibrated according to results of experimental SCB testing as reported in previous papers. This paper first reviews some background data on SCB fracture toughness, and experimental results of fracture toughness of microwave treated SCBs. Then it proposes a new methodology for simulation and validation of rock samples exposed to microwave illumination with regard to experimental results, and discusses the correlation between fracture toughness of BSUIs and density of micro-cracks, which is attributed to applied microwave power and duration of illumination.

Aug 1, 2013

By W. K. Pincock

Accident prevention can be portrayed as a science that deals with facts and natural phenomena and must be dealt with in the same manner as any other operating problem. Safety at the Copper Queen Branch dates back to 1913 when a Safety Organization was started and rules formulated for underground mining. Since then the mining industry has made substantial progress in the elimination of accidents and when the Lavender Pit was started in 1951, it adopted the general plan in use at all Phelps Dodge properties. Following is a brief description of the Pit Operations:

Jan 1, 1959

By H. G. Wolfhard

The mode of propagation of explosions through narrow passages is important for understanding flameproofed equipment employed in mines. Narrow channels have been used in this investigation that connected between a small explosion chamber and a large chamber containing fuel-air mixture. The oxygen index of the mixture in the small chamber was determined which caused an explosion in the outer chamber. Preliminary measurements have already been given in Bureau of Mines Report of Investigations 5457 and suggested that) flames do not pass through narrow channels. The hot, burned gases from the explosion in the small chamber, however, are able to ignite the mixture in the large chamber by a process of hot-gas ignition. Systematic measurements are reported in the present paper that cover the influence of channel length and diameter and the properties of the gas mixtures in the large chamber on the transmission of explosions. The influence of such properties as quenching diameter and flame temperature is also discussed. This paper concludes the work on this problem and presents a theory that describes in detail parameters that influence transmission of explosions through narrow channels. INTRODUCTION Flameproofed equipment in mines is usually provided with flanges. A gap between the opposing flanges allows ventilation and release of pressure. The safe gap width has been determined for a number of flange lengths by Smith4/

Jan 1, 1959

By H. R. Manouchehri

In flotation practices, as particles become finer, such as smaller than 20 μm, process efficiency declines markedly. Selective agglomeration of fine particles is a technique to enhance the recovery of fine valuable minerals in flotation circuits. Different agglomerating methods have been introduced and tested. One method that has recently received much attention is to make use of magnetic force to aggregate fine particles. A selective aggregation of fine paramagnetic particles, such as sulfide minerals, can be achieved in the high-intensity magnetic field prior to or during flotation. The method is simple, selective and effective for fine particles and has low operational cost, though a minimum magnetic susceptibility for fine grains is required to promote the process. In this paper, the implementation of the ProFlote magnetic conditioning device in Boliden’s Garpenberg old concentrator in Sweden, where a complex massive sulfide ore is treated, is presented and discussed based on Boliden’s Garpenberg plant. The results showed an increase in the flotation recovery of fine valuable minerals. Zinc (Zn) production was increased by between 1,100 and 1,500 t/a, while salable yearly silver (Ag) production was increased by 1,500 kg. The copper (Cu) grade in the final concentrate was increased by 1 percent, while reductions in its Zn and lead (Pb) grades were obtained. Moreover, considerable reduction in Zn deportment to the final tail was observed

By Aaron Evans, Chu E. Ho, Tom Richards

"This paper describes an innovative case history of using jet grouting to form a groundwater cutoff wall at the interface of a cut-and-cover construction and an existing tunnel. The design of the jet grouting layout was complicated by the presence of a left-in-place bulkhead of unknown dimensions abandoned by previous construction of the existing tunnel. Jet grouting was performed through predrilled holes within the narrow space between the existing bulkhead sheeting and tunnel structure. A systematic sequence of primary and secondary jet grout elements of varying diameters and panel lengths was executed to achieve an effective groundwater barrier. A key challenge in the jet grout design was the impact of potential deviations due to shadowing effects of the left-in-place bulkhead sheeting and pre-formed jet grout columns, as well as overbreak concrete in adjacent secant pile walls. The flexibility of the jet grouting methodology enabled a wide range of operational parameter combinations to be performed, allowing column diameters to be adjusted based on actual field installation measurements. Special precaution was exercised when grouting at critical locations to avoid over-pressurization and damage to the existing tunnel structure.IntroductionThe 96th Street Station box for the new Second Avenue Subway Line in Manhattan, New York included a transition tunnel, which connected the station to an existing tunnel built in the early 1970s (Figure 1). The new station and transition tunnel were both constructed using the cut-and-cover technique with bottom-up sequence (Aksman et al. 2012, Grigson et al. 2016). The main station structure incorporated permanent diaphragm walls for most of its length, except for the southern segment where high rock levels were encountered and the station box was constructed within temporary secant pile walls socketed into the rock. The permanent diaphragm walls were also utilized for temporary excavation support (Ho and Hu 2014). At the northern end of the site, the new transition tunnel was constructed within temporary secant pile walls that extended from the station diaphragm walls to the existing tunnel at the tie-in location. A temporary traffic deck spanning 60ft across the secant pile and diaphragm walls along the full excavated length of the site allowed traffic to continue operating at street level while construction of the station and transition tunnel progressed below grade."

Jan 1, 2016

By L R. Marshall, M J. Rubenach, T G. Blenkinsop, J S. Cleverley

The source and transport regions of fluidised (transported) breccias outcrop in the Cloncurry Fe-oxide-Cu-Au district, providing insights into the origins of other fluidised magmatic-hydrothermal breccias such as kimberlites. Discordant dikes and pipes with rounded clasts of metasedimentary calc-silicate rocks and minor felsic and mafic intrusions extend several kilometres upwards and outwards from the contact aureole of the 1530 Ma Williams Batholith into overlying schists and amphibolites. The brecciation initiated at depths >10 km and may have resulted in surface breaching. We used analytical equations for particle transport to estimate clast velocities (eÆ 20 ms-1), approaching volcanic ejecta rates (up to 80 ms-1). The wide range of CO2 fluid inclusion densities (up to 150 MPa), the localisation of the base of the breccias in contact aureoles, and the scale and discordancy of the bodies suggests the breccia transport process was triggered by an abrupt release of overpressured fluid. At these depths, such extreme behaviour may have been achieved by release of dissolved fluids from crystallising magma, in combination with a strongly fractured and fluid-laden source, sitting under a strong, low permeability barrier, and such parameters may be analogous to the asthenosphere/lithosphere boundary in the case of kimberlite initiation. The relationship of these breccias to the Ernest Henry iron-oxide-Cu-Au deposit suggests they may have been either fertile or æfailedÆ orebody feeders.

Jan 1, 2005

By Hajime Miki, Gde Pandhe Wisnu Suyantara, Tsuyoshi Hirajima, A. M. Elmahdy, Keiko Sasaki

"Seawater has been reported to depress molybdenite in a copper-molybdenum (Cu-Mo) flotation process at high pH due to the precipitation of Mg(OH)2. Meanwhile, to improve mineral recoveries, collectors are usually added into the flotation cells, thus adding the complexity to the mechanism of bubble-particle interactions involved in Cu-Mo flotation. Therefore, understanding the interaction mechanism in seawater flotation and in the presence of collectors is important to explain the minerals depression. The present work investigated the effect of kerosene on the bubble collision and attachment to pure chalcopyrite and molybdenite surfaces in MgCl2 solution as one of the seawater major components at pH 6 and 11. Mineral surfaces were characterized using atomic force microscopy (AFM). In addition, minerals floatability in the same system were tested in a column flotation. The study of bubble-particle interactions shows that following several collisions, bubble could displace the intervening liquid layer on the mineral surfaces, forming a three-phase contact (TPC). A TPC formed more rapidly in the presence of emulsified kerosene in a 0.01 M MgCl2 solution at pH 6 for both minerals. The reason is kerosene increased the surfaces hydrophobicity and destabilized the intervening liquid layer on the surfaces. Moreover, the average time required to form a TPC was shorter on molybdenite surface. This can be attributed to the effect of adsorbed kerosene on molybdenite surface and molybdenite surface roughness.INTRODUCTIONIn froth flotation, bubbles are used to separate hydrophobic mineral particles from hydrophilic particles. In this process, bubble-particle interactions (i.e., collisions, attachment, and detachment) are crucial with regard to mineral recoveries. The effectiveness of froth flotation depends on the formation of stable aggregates between the hydrophobic particles and the bubbles, allowing the bubble to carry the particles to the froth layer. To form such aggregates, the bubbles and particles must collide, and the intervening liquid layer must be drained below the liquid layer critical thickness, forming a stable threephase contact (TPC) (Ralston & Dukhin, 1999). Particles detachment may take place if the particles still have sufficient kinetic energy and the TPC is not formed. Previous studies of bubble-particle interaction in electrolyte solutions have been conducted using atomic force microscopy (AFM) (Assemi, Nguyen, & Miller, 2008), and by approaching the bubble using mica plate (Pushkarova & Horn, 2008), however, these studies did not focus on the bubble-particle collisions. Bubble collisions and attachment to hydrophobic (Teflon) and hydrophilic (glass) surfaces in a a-terpineol solution have been investigated by Krasowka et al. (2003)."

Jan 1, 2016

By C. J. Chindgren

Upgrading of commercial red cake and recovery of vanadium oxide from uranium-vanadium mill solutions were investigated by the Bureau of Mines. Alternative procedures potentially useful for manufacture of high-quality vanadium oxide at the mill site were explored and developed. The simplest and best procedure for converting commercial red cake containing about 10 percent combined sodium and potassium oxides (Na20) (K20) into a 98- to 99-percent vanadium pentoxide (V205 product appeared to be a metathesis in an ammoniacal solution of ammonium sulfate. Molybdenum, as well as the alkali metal oxides, was removed from the red cake by this procedure at a modest expenditure of labor and reagents. When preparing vanadium oxide of higher grade, it was necessary to dissolve the red cake and reprecipitate the vanadium as ammonium metavanadate. Calcination at 450° C, decomposed the metavanadate and yielded oxide of about 99.5 percent V205. By recyrstallizing the metavanadate before decomposition, an oxide product approaching 99.9-percent purity was obtained.

Jan 1, 1962

By Andreas Dietrich

Laser off-gas measurement of CO, O2 and temperature has been carried online in EAFs. A visualization screen shows the values of CO and Oxygen and temperature for the entire heat, and includes the status of furnace equipment. The historical data of the heats are stored such that the furnace performance can be evaluated and optimized. A short comparison between laser based and conventional systems has been carried out related to speed, influence of dust, water, pressure, protection for bag house explosions. A high water and/or dust content in the sample does not represent a problem for this type of system. The measurement method works without interruption even under worst conditions such as dirty scrap, carbon injection etc. The installation was developed in conjunction with Marienhuette, Graz. They are 100% scrap based with a tap to tap time of ca. 46 min. Keywords: Laser Measurement, Off Gas, CO, O2, Temperature

Jan 1, 2003

By Jean-Marc Lulin

"Depuis 1906, pres de 130 gisements ont ere decouverts dans la inture archeenne polymetallique (Cu, Zn, Au, Ag) du nord-ouest becois. Une etude regionale du developpement du potentiel inier est presentee puis detaillee pour quatre secteurs: RouynDranda, Val d'Or-Malartic, Bousquet-Cadillac et Matagami.L' analyse est conduite a l' aide des parametres suivants: temps, ethodes de decouverte, profondeur des gisements et poids metal. ~~ courbes cumulatives illustrant le nombre de gisements decouverts fonction du temps montrent une forme generale en ""S"" dont les i'iations de pentes correspondent aux variations dans les taux de ~ouverte. Initiation, realisation et stabilisation des cycles de decourte sont ainsi mis en evidence. Deux ""bourns miniers"", de 1922 a ~5 et de 1955 a 1965, rassemblent 72 % des mines identijiees squ' a present.La plupart des mines sont trouvees en subsurface: 90% ont leur fmet entre 0 et 100 metres de profondeur dont 70 % entre 0 et 10 etres. Dans le temps, il y ad' abord recolte par prospection puis par fphysique et enjin, developpement progressif du potentiel en proeur avec des methodes composites. Environ 80% du poids metal extrait de 4 camps miniers, couvrant 8% de Ia surface regionale quelques gros gisements dominent /a production.Ces donnees permettent de proposer une nouvelle approche pour lysed' une region miniere:La distribution de Ia profondeur des gisements en fonction du temps est indicatricede /amaturite d' uncampminieret peut servir a evaluer son potentiel residue/.L' analyse des courbes en ""S"" permet d' extrapoler les taux de succes relies aux differentes methodes et met en relief le role crucial de I' innovation dans I' exploration.ABSTRACTSince 1906, some 130 deposits have been discovered in the Archean polymetallic belt of northwestern Quebec. In this paper, the development of the mining potential is analyzed at the regional scale and for the following mining camps: Rouyn-Noranda, Val d'OrMalartic, Bousquet-Cadillac and Matagami.The analysis is based on the following parameters: time, discovery method, depth and weight of metal extracted. Curves showing the cumulative number of deposits discovered as a function of time are ""S"" shaped with slope variations corresponding to changing discovery rates. Initiation, realization and stabilization of discovery cycles are thus well represented. Two ""mining booms"", 1922 to 1945 and 1955 to 1965, account for 72% of the mines identified to date.Most exploitable orebodies have been found near the surface: 90 %have their top between 0 and 100 meters, including 70% between 0 and 10 meters. Early discoveries were made by prospecting, followed by geophysics while the progressive development of the depth potential is being realized by a combination of methods. Approximately 80 %of the metal extracted comes from four mining camps which cover 8% of the area, but most of the production can be allributed to only a few large deposits. Based on these data, a new approach to the analysis of a mining region is proposed:1) The distribution showing deposit depth versus time is indicative of the maturity of a mining camp and can serve to evaluate its remaining potential.2) The ""S"" curve analysis can be used to extrapolate the success rate of a specific exploration method and also stresses the crucial role of innovation in exploration."

Jan 1, 1990

By K. A. Svanstrom, W. R. Opie

Problems associated with deposition of titanium infused chloride baths using TiCl4 as a feed material are reviewed. A potentially workable cell design using Alumdum diaphragms is discussed. Problems inherent to diaphragm-type cells are emphasized and experiments described which led to the development of a cell without a diaphragm. INVESTIGATORS assigned the problem of developing a commercial electrolytic process for making titanium metal have found that they are faced with the difficulty of overtaking rapidly improving magnesium and -sodium reduction processes. The ultimate goal must be a simple process that can be conducted with low-cost raw materials in equipment that is inexpensive to build and operate. This paper deals with some work of a preliminary nature conducted by personnel of the Research Laboratories, National Lead Co., Titanium Division. Many others have reported on the general subject of depositing titanium from fused salt electrolytes. A partial bibliography is attached. PRIMARY CONCEPTS Anyone attempting to deposit titanium metal from fused chloride electrolytes using TiC14 as a source material is faced with at least the following problems: 1) Getting the titanium into solution in the bath. 2) Controlling oxidation and reduction reactions associated with multiple valency of titanium, which result in low electrical efficiency. a) Prevention of dichloride oxidizing to trichloride and trichloride to tetrachloride at the anode. b) Prevention of trichloride from being reduced only to dichloride at the cathode. 3) Prevention of metal formation away from the cathode thru disproportionation of titanium dichloride to satisfy the equilibrium. 3 TiCl2 == 2 TiCl3 Ti [I] 4) Protection of reduced chlorides in the bath from reaction with oxygen from the bath container or air. 5) Removing from the bath the deposited metal formed without allowing it to become contaminated with oxygen or nitrogen. 6) Selecting cell materials of construction which will not contaminate the metal product or cause cell inefficiencies. EARLY EXPERIMENTS The initial attempts made to electrodeposit titanium from fused chloride baths using TiCl4 as a source material indicated that TiCl4 was essentially insoluble in molten chlorides of alkali and alkaline earth metals. If, however, the TiCl4 was introduced close to a nickel cathode some metal could be formed and appreciable quantities of reduced chlorides would be present. These reduced chlorides reacted with any oxygen present in the atmosphere above the bath and would also diffuse quickly to the anode (graphite) where they would react with chlorine and be evolved as TiCl4. The net electrolytic efficiency of such a cell is essentially nil. The TiCl4 evolves from the anode at almost the same rate that it is introduced in the vicinity of the cathode although a small amount of titanium metal can be formed on the walls of the cathodic pipe. It becomes apparent from the operation of such a cell that: metal can be deposited on the cathode, although of small particle size and a nonadherent nature, and when reduced chlorides are present in the electrolyte, TiCl4 can be absorbed, probably by the following reactions: TiCl4 + TiC12 - 2 TiCl3 [21 2 TiCl3 + 2 faradays - 2 TiC12 + C12 [31 DIAPHRAGM CELLS These facts encouraged the development of cells containing diaphragms to prevent migration of reduced chlorides from the cathode area to the anode. Small-scale cells for process development are described by Alpert, Schultz, and Sullivan.20 A larger brick-lined cell incorporating internal heating by passing ac through the bath is shown in

Jan 1, 1960