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By W. L. Dare

This report is one of a series published by the Federal Bureau of Mines to describe methods and costs of mining uranium on the Colorado Plateau. The Navajo Uranium Division of Kerr-McGee Oil Industries, Inc., mines uranium from several deposits of carnotite-type ores, which lie buried in the Lukachukai Mountains on the Navajo Indian Reservation, Apache County, Ariz. The country is rugged and isolated Constructing and maintaining roads has been a continuous task. The ore bodies occur within the Salt Wash member of the Jurassic Morrison formation and are similar to other such deposits on the plateau. The current mining activity in the Lukachukai Mountains is a result of uranium-ore discoveries in 1949, although the Navajos undoubtedly knew of the outcrops of yellow uranium minerals long before that time. The ruggedness of the country and the heavy soil cover over much of the surface hampered prospecting, but probably the main reason the ore was not found sooner is that no one took the trouble to look for it in the Lukachukai Mountains.

Jan 1, 1961

By Israel Liebman

The Bureau of Mines developed three types of passive water barriers for suppressing slow-moving coal dust explosions. One type is a modification of a conventional tub barrier and depends on the dynamic pressure generated ahead of an explosion to tilt the tub to release its water and suppress the explosion. The other two barriers operate in response to an increase in static pressure developed ahead of the explosion. Tests indicate the first barrier begins to release its water at air speeds as low as 50 ft/sec, and the second and third barriers will operate at a rise in static pressure as little as 0.5 psi. All three barriers were found to be effective in suppressing coal dust explosions propagating at speeds as low as 100 ft/sec. A plan is described for installing a water barrier in a working mine on a trial basis.

Jan 1, 1976

By H. C. Gunning

DURING the past year the Cadillac-Malanie area in northwestern Quebec has been catapulted to the front as one of Canada's most active gold mining districts. Late in 1934 the area was lolling along in the doldrums, with one producing mine and a handful of active prospects. 1935 passed with only slightly increased activity, but saw the start of production at Canadian Malartic mine. Lightning struck in April, 1936, when a new and phenomenally rich ore-body was found in O'Brien Gold mine, and by midsummer the camp was ablaze with activity. An important new discovery on the Pan-Canadian property, and pleasing underground developments at Sladen Malarric, East Malartic, and Lapa Cadillac, in addition to other new developments, lent fodder to the flame, and at present several dozen properties are being actively developed. For the past three seasons, the Geological Survey of Canada has been engaged in a fairly detailed study of the geology and mineral deposits across Cadillac, Malarric, and Fourniere townships. Ir is the purpose of this paper to present a brief preliminary statement of the structural and economic geology and to discuss some of the more important problems that have been found to exist. The reader is requested to remember that the paper is a preliminary one and that therefore the conclusions presented are open to revision. It is impossible to make full acknowledgment for help received, for the writers are indebted to practically every operator and prospector in the area for generous co-operation in the work, and to several private, provincial, and federal geologists for data and frank discussion of problems encountered. Over a score of student assistants from McGill, Queen's, and Toronto have given excellent service. Published reports by Wilson, Cooke, James, Mawdsley, L. V. Bell, and J. J. O'Neill greatly facilitated the work. For adequate control surveys and a topographic base-map, the writers are greatly indebted to H. N. Spence.

Jan 1, 1937

By Lewis V. Wade

This paper summarizes the results of the rock mechanics monitoring program performed as part of Old Ben Coal Company's longwall coal mining demonstration project conducted in cooperation with the United States Bureau of Mines. The work described herein included installation of instruments, collection of data and data analysis performed during mining of the first longwall panel in Mine No. 24. The rock mechanics monitoring program included both surface and underground instrumentation and was designed to achieve the following purposes: 1 -To provide the capability to observe unusual situations during mining so that remedial measures could be instituted quickly 2 -To formulate design guidelines for future longwall mining efforts; 3 -To evaluate surface subsidence, and its character, rate and potential effects on cultural features, and to develop criteria to assist in predicting subsidence for other mines having similar roof conditions. Six previous attempts with longwall methods in Old Ben Coal Company's Hine 21 had been unsuccessful due to roof control problems. A description of these attempts is given by Moroni (1973). In preparation for the present longwall operation a study was performed to review existing data on the previous unsuccessful attempts, to establish coa1-and floor-strata bearing capacities in Mines Nos. 21 and

Jan 1, 1977

By C Laming, P M. Hetherington, F A. Pym, M P. Murphy, K E. Crook

Reconciliation is a powerful tool used by mining operations to compare the mass and grade of ore produced with what was estimated before mining. The primary objective of reconciliation is to verify that the estimated planned metal production is achieved during processing, allowing issues to be identified for which adjustments can be made throughout the mining value chain to improve recovery and maximise efficiency. Traditionally, the mine plan is based on estimated mine grades using sampled exploration drill hole or blasthole grades. Reconciliation discrepancies between the mine plan and mill are common due to such factors as insufficient or non-representative sampling, poorly conceived models, or unrecognised blast movement. MineSense Technologies Limited® (MTL) has developed an X-ray fluorescence (XRF) sensor-based ore classification system that is installed on mining equipment to provide real-time grade estimates of run-of-mine material at bucket, truck, or belt-scale. Bucket level grade estimates provide insights into grade variations at the mine face that were never before available. This data set eliminates some of the leading causes of reconciliation discrepancies and enables tracking of tonnages and grades from the mine face to the processing plant at bucket resolution with confidence. Bucket-by-bucket grades at the mine face enable dynamic optimisation of the mine plan to stabilise the mill feed grade through blending of mine and stockpile loads. Beyond stabilising feed grade, Mine to Mill reconciliation combined with the full XRF spectrum response can generate proxy relationships to ore characteristics like hardness and recovery. These properties can then be predicted at the mine face, enabling further optimisation of the downstream mill feed, not only for grade, but also for power and water consumption, reagent addition, and recovery. This paper presents the benefits of MTL technology for grade reconciliation and mill performance optimisation at a Cu Mine in BC (Canada).

Mar 22, 2022

By V Chamberlain, M Appeah Owusu, M Aniawu-Asumakah, A Anyimadu, R Peattie

This is an integrated geology and plant improvement study arising from the heterogeneity seen in mineralogy and gold association at the Obuasi goldmine in Ghana. This heterogeneity comes from the two ore types mined, the one being a sulphide ore, mainly composed of gold-bearing arsenopyrites. This gold is refractory and exhibits a strong relationship between gold and As. The other is quartz veins, that are high grade and free milling. The installed circuit consists of comminution – Gravity -Flotation – BIOX – Leaching and Adsorption processes. The opportunity tested involved improved mass pull - related flotation recovery of Au in the Sulphide stream; while balancing the need for a minimum Sulphide grade for the Bio-oxidation process, occasioned by the removal of 25 to 30 % of the (quartz) stream through preconcentration by Ore sorting. The current circuit is then utilized for the sulphide route, while a smaller grind-gravity circuit is utilised for the quartz stream in a relatively inexpensive way, followed by a common leaching and adsorption circuit. Added advantages of the strategy includes faster recovery of gold from the quartz stream, with less consumption of reagents from saving on flotation and BIOX reagents for this stream. Screening and Ore sorting was successfully tested with laser technology, achieving over 98% separation of quarts (containing up to 40% of the gold). The plant schedule of Ore, the suggested circuit design for the Ore sorting, the results obtained from the different flotation regimes, as well as consequent financial modelling have been presented and discussed in this paper. This illustrates the opportunity that arises out of a detailed analysis of material versus installed circuits, even if the gains in pre-concentration do not necessarily involve rejection of gangue material. An added opportunity for future investigation, briefly discussed but not tested in this paper, would be to maintain current mass pulls but with increase in throughput (by the space created by the sorted material). This will of course require the mining ability. It could also add LOM value by altering the cut-off grade.

Nov 10, 2020

By W. J. Fene

A comprehensive study of all bituminous coal-mine fatalities occurring in Pennsyl¬ vania during the 5-year period, 1926-1930, was made to try to determine the factors that in¬ fluence accidents which cause these fatalities. During this study some two thousand reports of fatalities were reviewed, and pertinent information as to causes and influencing factors were tabulated therefrom. These tabulations are discussed in detail, and in some instances recommendations are made with a view to reducing the hazards in certain classes of these accidents.

Sep 1, 1931

By B. F. Giyani, A. Salama

Tanzania is a country with a variety of mineral deposits, including metallic minerals, gemstones, mineral fuels, industrial minerals, and critical minerals. This study provides an overview of mining legal framework, mineral occurrence and production, challenges in the mining sector, and government initiatives. The aim is to demonstrate the development of the mining sector in Tanzania and explore the potential for further mining investment in the country. The mineral production data showed generally increasing trends over the years, for example, gold production increased from 42 tonnes in 2018/2019 to around 50 tonnes in 2023/2024. Despite the growth, the mining sector encounters several challenges, including a lack of detailed geological information on mineral deposits, inadequate infrastructures in some remote mining sites, the existence of informal artisanal miners, and mineral smuggling. The Tanzanian government has introduced several initiatives to address these challenges, including carrying out the highresolution airborne geophysical survey to increase geological information in some areas, the formalisation of artisanal and small-scale mining, establishing mineral markets to combat mineral smuggling, and encouraging mineral value addition within the country.

Oct 24, 2025

By Dongjie Zhang, Zeyu Liu, Shuxin Liu, Yang Liu

Lateral pressure provided by caving rocks plays an important role in keeping the stability of the sidewall rock mass and controlling the rock movement. Taking Xilinhot Fluorite Mine as an engineering background, we studied the control mechanism of the granular media lateral pressure on the rock movement by combining physical experiments, theoretical analysis, and field monitoring. The results indicated that with the increase of the granular media depth, the lateral pressure provided by the static granular media presented two stages of rapid growth and slow growth. The lateral pressure on the footwall was negatively correlated with the dip angle of the orebody, and the lateral pressure on the hanging wall was positively correlated with the dip angle of the orebody. Ore drawing only caused the granular media lateral pressure near the drawing point to decrease. As the granular media moved, the granular media lateral pressure outside the pressure reduction area further increased, and this part of the granular media would play a key role in limiting surface rock movement. On this basis, the improved calculation formula of GLMP was given, which could be better applied to calculate the GLMP and critical granular media column with different dip angles. The action mechanism of the GLMP in the control of the surface rock movement was clarified. The granular body in the collapse pit was mainly composed of three parts: the bottom loose granular media column, the middle compaction granular media column, and the upper critical granular media column. The critical granular media column was the most important area to control surface subsidence and rock movement. Finally, through field practice, after effective filling of the collapse pit, the surface vertical displacement of the hanging wall and footwall was decreased by 56.8% and 55.6%, respectively, and the control effect of surface rock movement was remarkable.

Sep 18, 2023

By Tanya J. Gallegos, Mojisola A. KunleDare, James V. Jones III, Charlotte E. Riggs

The United States Geological Survey (USGS) provides scientific information for the Department of Interior and the nation, consistent with its original mission expressed in the Organic Act of 1879 (43 U.S.C. 31): “the classification of the public lands and examination of the geological structure, mineral resources, and products within and outside the national domain.” Legislation such as the Energy Act of 2020 and the 2022 Infrastructure Investment and Jobs Act (43 USC 31l) and recent executive actions (Executive Orders 14154 , 14153, 14241 Secretary’s Orders 3417, 3418, 3422, 3436) underscore the importance of mineral resources and focus USGS activities on mapping and assessing mineral resources, with a particular focus on those presently identified as critical, both in ground and above ground in mine wastes. This article reviews selected activities and accomplishments by the USGS Mineral Resources Program related to critical minerals in 2025. Highlights include a new List of Critical Minerals, a first-ever national mine waste inventory, international minerals partnerships, mineral resource assessment advancements, and national data collection activities and outcomes of the Earth Mapping Resources Initiative (Earth MRI). The selected contributions are not comprehensive but are intended to demonstrate USGS leadership in critical mineral mapping and assessment, the importance of domestic and global partnerships, and the breadth of research activities that are responsive to national needs and priorities.

May 1, 2026

By Harold J. Rose

The economic situation in Switzerland during recent years has resulted in theoretical studies , engineering development work , and many commercial installations of ingenious methods for using energy more efficiently . The purpose of the present investigation was to learn of recent Swiss developments for the more effective use of coal , which comprises 98.9 percent of the romaining known mineral - fuel reserves of the United States .

Jun 1, 1947

By Dustin Vickress

The premature failure of copper staves in the lower stack and bosh is frequently the cause for an interim blast furnace repair at great cost to the blast furnace owner. Protective accretions may form on the stave hot face, but when these accretions are lost the staves can begin to deteriorate both due to abrasive wear from exposure to the descending burden materials and due to thermal cracking from exposure to hightemperature process excursions. These mechanisms can lead to failure of cooling passages, which forces blast furnace operators to shut off these channels, accelerating the rate of copper stave wear. Finger cooler technology was developed to extend blast furnace life by restoring cooling to damaged staves. Evidence for their effectiveness is presented herein in the form of experimental test work and conjugate heat transfer (CHT) analysis carried out using computational fluid dynamics (CFD) simulations. These tests demonstrate that under typical blast furnace excursion conditions, a stave fitted with finger coolers will undergo half the temperature rise of a stave fitted with conventional cigar coolers.

Aug 17, 2017

By Tanai Marin

Modelling of pyrometallurgical processes can become extremely challenging when the process involves complex chemical reactions, phase change, multiphase flows, heat and mass transfer and fluid flow. Traditionally modelling involving complex thermodynamic equilibrium and thermochemistry are treated separately from problems in which transport phenomena are dominant, such as CFD and heat transfer studies. The separation is also necessary due to the lack of modelling tools that can effectively couple both solution thermodynamic and transport phenomena or even multiphysics problems. However, there are, quite often, problems in high temperature process metallurgy in which it is not possible to simplify this two modelling approaches. Typical cases of this are for example, the modelling of slag freezing on furnace walls (electric or flash furnaces) to create a protective layer in front of the refractories hot wall, the formation of build up from the matte or metal phases at the hearth of the furnace, calcine smelting from charging piles into slag phase, etc. The problem is even more challenging in nonferrous pyrometallurgy as most, if not all, of the condense phases are highly non ideal solutions involving several components and exhibiting complex crystallization paths and miscibility gaps, such as the Fe-Ni-Cu-S matte, FeO-Fe2O3-SiO2, FeO-MgO-SiO2 slags, etc. In this paper, an approach to model coupled problems involving multiphysics and solution thermodynamic is presented. The approach consists in developing in-house a library containing the Gibbs energy minimization routines and using the local equilibrium concept for process modelling from a multiphysics commercial software (COMSOL). Simple test cases, such as building a non-ideal binary phase diagram on a CFD package is presented, the limitations and of other classic approaches such as equilibrium or Scheil cooling are discussed and compared to this model.

Jan 1, 2015

By Herty, C. H.

One of the numerous requirements of many grades of present- day steel is that the steel shall be free from non-metallic inclusions. These inclusions may be composed of oxides, sulphides, complex oxy- sulphides, and nitrides, which enter the steel with the furnace charge, result from sulphur absorption from the furnace gases, or are formed in the steel during the deoxidation process. Although few' data are available which indicate in any quantitative manner the specific effects of inclusions in steel, there is a large mass of circumstantial evidence which points to the advisability of producing steel free from these impurities for many purposes. At the present time there is a growing feeling among metallurgists that non-metallic inclusions should be divided into two distinct types: (I) those readily visible under the microscope at ordinary magnifications; and (2) those in colloidal suspension or in solid solution. Both types are profoundly influenced by the character of the charge, the manipulation of the furnace slag, and the method of deoxidation. The work described in this bulletin deals primarily with inclusions visible under the microscope at ordinary magnifications, but the steels made by the various methods of deoxidation are being used LO study certain effects which may be ascribed to the second classification, named above. This latter work will be the subject of further bulletins on the effect of deoxidation practice on the physical properties of the steels involved.

Jan 1, 1957

By D O. Hayba

Metal-rich slurries discharged from excess-enthalpy geothermal wells at Kawerau (NZ) indicate that an efficient ore precipitation mechanism operates in some feedzones. In our conceptual model, which takes into account the relative permeabilities of liquid and gas phases in boiling fluids, a metal-precipitating liquid phase is effectively immobilised along boiling fronts, leading to the formation of highly concentrated ore. Chemical equilibrium and heat/mass transport modelling demonstrate the general applicability of this conceptual model to hydrothermal eruption environments.

Jan 1, 1995

By V. K. Risinggård, M. Sparta

We report on the development of a finite-element method model for a pilot furnace for the production of manganese alloys. The model is a multiphysics model that addresses material flow, electrical conditions, heat transfer, and physical and chemical transformations. It is capable of studying both quasi-steady and transient states in time-dependent simulations. The model includes common charge materials and fluxes and can simulate production of both ferromanganese and silicomanganese alloys with acid and basic slags, as well as changing charge compositions. The model output provides access to the material distribution in the furnace during furnace runs, temperature profiles, current paths, energy balances, and alloy and slag production rates and compositions.

Apr 16, 2024

By A. Steiner, K. L. Komarek

Activities of aluminum in solid Ni-A1 alloys have been determined between 20 and 60 at. pet Al and 1200" and 1400°K by an isopiestic method in which nickel specimens, heated in a temperature gradient, are equilibrated with aluminum vabor in a closed all-alumina system. The activity of aluminum shows a strong negative deviation from Raoult's law at low concentrations but increases by three orders of magnitude within the ß(NiAl) phase. The partial molar enthalpy and entropy of mixing are negative. Using Wagner and Schottky's theory of ordered compounds, a degree of disorder of 4 x 10 -4 for NiAl and 1.25 X 10-2 for FeAl has been calculated THE Ni-A1 system has been studied by a great number of investigators, and the results, as far as the phase diagram is concerned, have been compiled by Hansen.1 The phase boundaries from 0 to 50 at. pet Ni are well-established. At higher nickel contents the boundaries are still in dispute and an additional phase, A12Ni3, has been reported.' The phase diagram is dominated by a very stable high-melting compound, NiA1, with a relatively wide range of homogeneity. Heats of formation of solid alloys have been determined calorimetrically by Oelsen and Middel3 from 20 to 95 at. pet Ni and by Kubaschewski4 from 25 to 80 at. pet Ni. According to the most recent compilation5 no other thermodynamic investigations have been reported for the Ni-A1 system. Due to the corrosive nature and the low vapor pressure of aluminum, a method has been employed for determining activities of aluminum which was previously developed for the Fe-A1 system.= Nickel specimens, heated in a closed evacuated alumina system in a temperature gradient, were equilibrated with aluminum vapor from a source within the system kept at constant temperature. After complete equilibration the specimens were analyzed and activities calculated from the known vapor pressure of aluminum. APPARATUS AND EXPERIMENTAL PROCEDURE Materials. The nickel specimens were made from wafers of electrolytic nickel (International Nickel Corp.) of 99.99 pet purity which were rolled to a 0.001-in.-thick foil by Driver-Harris Co. and to a 0.005-in.-thick sheet in our laboratory. The aluminum (Aluminum Corp. of America) had a purity of 99.99+ pct. The alumina tubes and crucibles were made of impervious recrystallized alumina with an alumina content of 99.7 pet (Triangle RR, Mor-ganite Inc.). Experimental Procedure. Annular specimens were punched from the sheet, the punching burrs removed, and the specimens degreased in carbon tetrachloride and acetone and weighed on a micro-balance to within an accuracy of ±0.01 mg. The specimens were positioned with alumina spacers along an alumina tube, and the positions measured. Aluminum metal was machined into cylindrical shape, and placed into an alumina crucible. The tube with the specimens was then inserted into a hole drilled into the aluminum metal. An alumina tube with its closed end at the top was slipped over the specimens so that its lower end fitted snugly into the alumina crucible. The assembled reaction tube was inserted into a mullite tube with a water-cooled brass head which had an opening for a quartz thermocouple protection tube and a metal-to-glass connection to a conventional vacuum system. A Pt-Pt 10 pet Rh thermocouple could be raised and lowered in the quartz tube which was placed along the outside of the alumina reaction tube. The mullite tube was heated by two separately controlled resistance-tube furnaces so that in the experimental temperature range an over-all temperature gradient of approximately 150o to 250°C could be imposed on the reaction tube. The position of the mullite tube was adjusted so that the surface of the aluminum metal was always at the temperature minimum. The reaction tube was thoroughly evacuated before and during slowly heating the assembly up to the melting point of aluminum. A pressure of less than 2 µ (Hg) was maintained during an experiment. Once the aluminum had melted, it isolated the contents of the alumina tube from the surroundings. Several times during an experiment the temperature gradient was carefully measured. An experiment lasted from 3 to 6 weeks and it was terminated by air cooling the evacuated mullite tube. For further details of the experimental procedure the paper on the Fe-A1 system6 should be consulted.

Jan 1, 1964

By John Chipman, Minu N. Dastur

This paper presents equilibrium data on the reaction of water vapor with vanadium dissolved in liquid iron at 1600°C. The thermo-dynamic behavior of vanadium and oxygen when present together in the melt is discussed. A deoxidation diagram is presented which shows the concentrations and activities of vanadium and oxygen in equilibrium with V209 or FeV2O4. STUDIES of the chemical behavior of oxygen dissolved in pure liquid iron1-3 have served to determine with a fair degree of accuracy the thermody-namic properties of this binary solution. The practical problems of steelmaking, however, involve not the simple binary but ternary and more complex solutions. Only a beginning has been made toward understanding the behavior of such systems. The silicon-manganese-oxygen relationship was studied long ago by Korber and Oelsen4 and more recently by Hilty and Crafts." The carbon-oxygen reaction was investigated by Vacher and Hamilton6 and by Marshall and Chipman.7 A number of deoxidizing reactions have been studied empirica1lys'10 with the object of determining the appropriate "deoxidation constants." The work of Chen and Chipman" afforded a clear-cut view of the effect of the alloy element, chromium, on the thermodynamic activity of oxygen in liquid ternary solutions. These investigators determined the oxygen content of experimental melts which had been brought into equilibrium with a controlled atmosphere of hydrogen and water vapor and were able to show that the presence of chromium decreases the activity coefficient of oxygen. They determined also the conditions under which the two deoxidation products, Cr2O3 and FeCr2O4, were formed and showed that the activity of residual oxygen is considerably less than its percentage. It was the object of this investigation to apply a similar method to the study of molten alloys of iron, vanadium, and oxygen. Vanadium was once considered a moderately potent deoxidizer, but this is now known to be erroneous, in the light of its behavior in steelmaking practice. Its reaction with oxygen retains a certain amount of practical interest in that a high percentage of one element places a limit on the amount of the other that can be retained. As a deoxidizer it will be shown that vanadium lies between chromium and silicon. Experimental Method The apparatus was that used by the authors3 in their study of the equilibrium in the reaction: H2(g) +O = H2O(g);K,= [1] PII., ao Crucibles of Norton alundum or of pure alumina were used. The latter were made in this laboratory and were of high strength and low porosity. Under conditions of use they imparted no significant amount of aluminum (less than 0.01 pct) to the bath. Temperature measurements were made with the optical equipment and calibration chart of Dastur and Gokcen.= The charge was made up of calculated amounts of ferrovanadium (20 pct V) and clean electrolytic iron totaling approximately 70 g. The first few heats were made in alumina crucibles with an insufficient amount of vanadium so that no oxide of vanadium would be precipitated under the particular gas composition. All the heats were made at 1600 °C under a high preheat and with four parts of argon to one part of hydrogen in the gas mixture to prevent thermal diffusion. The rate of gas flow was maintained constant at 250 to 300 ml per min of hydrogen. The time for each heat was three quarters of an hour after the melt had melted and attained the required temperature (1600°C). The water-vapor content of the entrant gas mixture was gradually raised in succeeding heats, keeping the vanadium content of the melt constant. This was controlled by manipulation of saturator temperature. A point was reached when for a given H2O:H2 ratio some of the dissolved vanadium was oxidized and appeared as a thin, bright oxide film on top of the melt. By raising the temperature of the melt it was possible to dissolve the oxide film which reappeared as soon as it was cooled down to 1600°C. The temperature readings taken on the oxide film were consistently higher by 80" to 85 °C as observed by the optical pyrometer. The heat was allowed to come to equilibrium under a partial covering of this oxide film. At the end of the run the power and preheater were shut off and the crucible containing the melt was lowered down into the cooler region in the furnace. This method of quenching proved quite

Jan 1, 1952

By L. A. Bromley, A. W. Petersen

The van Arkel-deBoer method for producing ductile titanium by thermal decomposition of Til, vapor and deposition on an electrically heated filament is modified by film boiling Til liquid on a heated filament, resulting in similar titanium deposition on the filament and liberation of gaseous iodine. The deposition rate is higher and the energy requirement smaller than in the van Arkel process. Many problems must be solved before the process is commercially feasible. TITANIUM of 99.9 pct purity, called ductile titanium, has been produced by a modification of the van Arkel-deBoer&apos; method. In the van Arkel-deBoer method, an electrically heated wire is suspended from two electrodes, which are placed in a container holding TiI, vapor at a low&apos; vapor pressure (usually <5 mm Hg). The vapor diffuses to the hot wire, usually maintained at 1100" to 1600°C,&apos; and decomposes according to the reaction liberating gaseous atomic iodine and depositing solid crystalline titanium on the wire. Estimations based on the data of Runnalls and Pidgeon,&apos; indicate that the rate-control ling step is the diffusion of atomic iodine away from the wire. There appears to be nearly thermodynamic equilibrium at the wire with TiI, and iodine as the main gaseous species. TiI, is almost certainly an important gaseous species in the cooler regions.&apos; The liberated iodine diffuses to a heated source of crude titanium and reacts to form more TiI, vapor, which again diffuses to the hot wire and completes the cyclic process. The foregoing process may be modified by suspending the hot wire in liquid TiI,, instead of the vapor, and obtaining film boiling. This type of boiling is characterized by the formation of a continuous film of vapor over the wire surface. Since only vapor contacts the wire sul.face, the temperature of this surface may be raised as high as desirable, within the limit of mechanical strength requirements for the wire. By properly adjusting the input voltage. the temperature of the wire may be maintained above U0C"C; and by evacuating the vessel holding the liquid TiI, and maintaining a suitable condenser temperature, the vapor pressure of TiI, may be held low. Thus, the conditions of operation of the van Arkel-deBoer method may be approximated with film boiling; and hence, it is postulated that ductile titanium may be produced by this method. Preparation of Til, There are many methods available for the preparation of TiI,; that used in this research was prepared by the direct reaction of titanium sponge in controlled amounts with liquid iodine. Although no difficulty was encountered with this reaction, it has since been pointed out that this method is sometimes dangerous and should be used with caution. The resulting TiI, was purified by distillation. First Film Boiling Experiments Apparatus: The apparatus shown in Fig. 1 was used for film boiling TiI, on short wire filaments. The current to the filament was supplied through a bank of three 5 kva transformers connected in parallel. The current was controlled by adjusting the voltage over a 0 to 67.5 v range with a 7 kva variable transformer on the low voltage side of the bank of transformers. The current and voltage were measured by Weston meters. The sealed-in-glass tungsten electrodes were hard-soldered to the filament for the film boiling of TiI,. The bottom part of the reactor, containing TiI,, was wrapped with ni-chrome heating wires to maintain the TiI, in the liquid state. An ice or liquid nitrogen trap, for solidifying I, vapor and any TiI, not condensed, was attached to the low pressure side of the air-cooled condenser. A Megavac vacuum pump was used. Procedure: A 0.010 in. diam tungsten filament was hard-soldered to the tungsten electrodes. TiI, was melted (mp 156°C) and poured into the reactor chamber; the top of the reactor chamber, containing the electrodes, was replaced. Freezing of the TiI, was prevented by controlling the current to the ni-chrome wires wrapped around the reactor with a 1 kva variable transformer. The mechanical vacuum pump was started and the system evacuated to about 2 mm Hg TiI, vapor pressure. The current to the filament was turned on and the impressed voltage slowly increased with the variable transformer. A sudden drop in current at nearly constant im-

Jan 1, 1957

By W. G. Lidman, H. J. Hamjian

&apos; I HE fabrication of many materials from powders involves a sintering process. A mass of powder will sinter because of the excess free energy over the same mass in the densified state caused by the higher total surface area of the powder. An understanding of the kinetics and mechanism of sintering should assist in improving the properties of such materials. The present investigation conducted at the NACA Lewis laboratory deals with the sintering of chromium carbide. Dry sintering (sintering at a temperature below the melting point) was divided into two stages by Shaler:&apos; the first stage, during which the particles preserve much of their original shape and the voids are interconnected, and the second stage, during which densification occurs and the pores are isolated. The mechanism of forming interfaces between particles, or welding together of particles, has been investigated by Kuczynski2 and may be described by any one or a combination of the following mechanisms: viscous flow, evaporation and condensation, volume diffusion, or surface diffusion. The mechanism by which pores are closed or eliminated (densification) during sintering, is of interest. Grain growth observed during sintering may be attributed to the variation in the surface energies of individual grains, causing some grains to grow at the expense of others. Grain boundary migration occurs presumably by a diffusion process, therefore the rate of grain growth would be expected to increase exponentially with increasing time and temperature. Thus, for practical sintering times of less than 1 hr, a certain minimum temperature may exist at which major structural and property changes will occur. Densification and kinetics of grain growth during sintering under pressure of chromium carbide were investigated to provide additional information which will aid in describing more accurately the sintering process and the mechanisms involved. This material was selected for this study because of the current interest in high strength, oxidation resistant refractory materials, such as carbides, which are sintered to produce solid, dense materials from powders. Sintering under pressure is a process where the heat and pressure are applied to the compact simultaneously, specimens for this work were prepared by sintering under pressure at different temperatures and for various time periods. Experimental Procedure Preparation of Specimens: Chemical analysis of the commercial chromium carbide used in this investigation was as follows: Cr 86.19 pct, C 12.14 pct, and Fe 0.2 pct. X-ray diffraction powder patterns gave characteristic diffraction lines of Cr3C2 crystal structure. Powder particle size was determined microscopically and the average initial particle size was 6 microns with 85 pct between 2 and 10 microns. Specimens sintered under pressure were formed in graphite dies3 heated by induction. Sintering temperatures were measured with an optical pyrometer by sighting into a 3/8-in. hole drilled 1 in. deep at the midsection of the graphite die. A load of approximately 1 ton per sq in. was applied to the powder. The die assembly was heated in 20 min to the highest temperature (2500°F&apos;) at which no increase in grain size could be observed, and less than 2.5 min were required to heat from this temperature to the maximum temperature (3000°F). Sintering temperatures and times for the specimens of this investigation are indicated in Table I. Analysis of Specimens: Specimens polished with diamond abrasives were etched to reveal the grain boundaries with a 1:1 mixture of 20 pct potassium hydroxide and 20 pct potassium ferricyanide heated to 160°F. Representative areas of each sample were photographed at 1000 diameters. The largest diameters of all well-defined grains were measured, but only the measurements of 15 of the largest grains were averaged in order to determine an index of grain size on the assumption that they were among the first to begin growth. Densities were determined from differential weighing of the samples in air and water. The reported density values are considered correct within ±0.01 g per milliliter. Results and Discussion Metal compacts have exhibited grain growth when sintered at temperatures about two-thirds of the absolute temperature of their melting point.&apos; Grain growth also occurs during the sintering of chromium carbide and is illustrated by the micrographs shown in Fig. 1. These micrographs were prepared from specimens sintered for 90 min at temperatures ranging from 1371°C (2500°F) to 1648°C (3000°F). Average grain size and density measurements of specimens investigated are presented in Table I. The relationship between grain size and sintering tem-

Jan 1, 1954