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By Patrick Ph. D. Kennedy, Osvaldo A. Ph. D. Bascur

With the revolutionary progress in information and computer technologies, applying the latest information technologies in metallurgical complexes has become a serious challenge to both a major opportunity and a serious challenge to both management and technical teams. The emerging component and object technologies are changing the way everyone can beneficially use their computer and networks to add to their corporate bottom lines. Most mining and metallurgical plants use predictive maintenance policies based on statistical analysis and special techniques, like vibration analysis and oil and lube analysis for critical equipment. Process control strategies are installed in several metallurgical sites. All process equipment and control strategies require maintenance from local personnel at the mine. Integrated use of existing and emerging technologies is making it possible to implement an overall process effectiveness control index. This index is based on key indices such as losses due to plant availability, performance efficiency and rate of quality. The availability of real time and process history to identify the most critical part of the processing system from mechanical integrity is highlighted. An emerging plant integration paradigm is described to simplify the implementation of business enterprise resources management and distributed plant management systems.

Jan 1, 1998

By L. K. Weaver

Bureau of Mines investigated the progressive impact that petroleum (crude oil and condensate) operations in the Gulf of Mexico have had on onshore operations and the expected effect of increasing activities in this area on future petroleum supplies from domestic sources. The data analyzed include capital expenditures, number of wells drilled, success ratio for exploratory wells, daily production per completion, annual producing rates, and oil reserves. The report compares offshore and onshore data and ascertains trends in petroleum industry operations. Observed data and trends indicate that in the near future Gulf of Mexico development and production will continue to increase relative to total U.S. petroleum activity. By 1975 annual oil and condensate production from the Gulf of Mexico is expected to be in the range of 750 million bbl to 1,150 million bbl, and account for approximately 20 to 30 pct of the estimated total domestic production.

Jan 1, 1969

By M. Misra

The dispersion of oily collector has significant effect on the flotation recovery of ultrafine coal. Generally, reagent dispersion is accomplished by mechanical mixing and/or ultrasonic agitation, followed by direct addition of dispersed collector into the flotation cell. However, such dispersion and reagent addition techniques are invariably inadequate and non-selective. A new collector utilization technique involving gas phase transport of atomized collector has shown improved results when compared to conventional reagent addition techniques. This new technique involves atomization of the collector into the gas stream. Under these circumstances an aerosol is introduced into the flotation cell. Initially, the oil is dispersed within the gas phase (continuous with respect to oil) and the gas phase is dispersed within the pulp (continuous with respect to aerosol). In the flotation cell, the atomized oil droplets coalesce on the bubble's surface and create a de-facto oil-encapsulated bubble. This approach provides excellent dispersion, increases selectivity, and most significantly increases the flotation rate of ultrafine coal. Furthermore, atomization of collector/frother combinations yielded improved flotation yields and maintained near uniform froth levels which is a desirable feature in coal flotation. In addition to flotation experiments, microscopic examinations of the attachment of oil-coated bubbles at a coal surface were conducted by attachment-time and contact-angle measurements. The oil coated bubbles attach at significantly faster rates and with a higher contact angle than do oil free bubbles.

Jan 1, 1987

By Robson Ferreira Vargas

No início de Março/2015 começaram a ser notados eventos de oxidação em bobinas armazenadas no pátio de expedição, e naquela época o fenômeno foi creditado às chuvas. Entretanto, passado o período chuvoso, ainda foram notados eventos de oxidação, que ocorriam também em produtos destinados à exportação. Isto mostrou que havia outra causa atuando no problema, e que era necessário descobri-la e tomar ações para sanar o problema. O produto final é a coroação do esforço produtivo anterior à sua obtenção, e leva consigo o nome do fabricante para onde for enviado. Por isto ele não pode ter falhas. A ArcelorMittal Tubarão montou um grupo de trabalho, que atuou em várias frentes, incluindo o condicionamento químico do sistema de resfriamento direto da laminação. Este grupo de trabalho obteve êxito na tarefa e as conclusões obtidas estão mostradas aqui.

Aug 17, 2017

The Kwademen Au deposit was discovered in 1977- 1978 following a regional geochemical survey carried out as part of a UNDP (United Nations Development Programme) and BUMIGEB (Bureau des Mines et de la Geologie du Burkina) mineral exploration programme. The climate in Burkina Faso is rather dry, with markedly seasonal rainfall averaging 800 mm pa in the Kwademen project area. The relief is low and the drainage poorly developed, so that soil sampling was preferred to stream sediment sampling. Rocks have been subjected to deep lateritic weathering, so that they are transformed into a mixture of Fe-oxides and kaolinite over depths varying between 30 and 40 m. At the regional stage, soil samples (30-40 cm depth) were collected a a 300 x 500 m grid. The Kwademen deposit was indicated by Cu, Zn, Mo and Au anomalies. Subsequently, an area of 9.2 km2 was covered by a detailed geochemical survey by soil (100 x 50 m) and auger sampling. The regional anomaly was fully confirmed, and subsequent drilling intersected mineralized ore shoots, justifying the establishment of an evaluation project led by the U.N.R.F. (United Nations Revolving Fund) in 1983- 1985.

Jan 1, 1988

By R. L. Grayson

Conventional mine safety wisdom states that "the most efficient mines are also the safest." Since the 1980s, small mines (and contractors) have been targeted as the most dangerous ones because of their fatality records. Statistical testing of 1993 West Virginia safety and production data indicated that the most efficient WV mines were not the safest ones, considering correlations between the severity measure and tons per employee-hour, except for very small mines. This paper will present the results of an extended analysis of WV mine safety using 1993 and 1996 data, concluding with the method used to suggest current priorities for focusing interventions.

Jan 1, 1998

By A. G. Eccles

"INTRODUCTIONWestern Mines' copper-lead-zinc operations are located in Strathcona Provincial Park, near the geographic centre of Vancouver Island. This park includes Buttle Lake, which flows into the Campbell River water system. The latter provides domestic water for the Town of Campbell River, approximately fifty-eight miles from the mine site.Operation of the concentrator commenced in December 1966, at which time the tailings were discharged into a small tailings pond near the plant. On May 8, 1967 Permit No. 185 was granted to the company, allowing discharge of the tailings, through a submerged outfall, to the bottom of Buttle Lake.Needless to say, the concept of operating a mine within a park, and the discharge of tailings into Buttle Lake generated considerable controversy. However, this has all but been eliminated over the years by the proven effectiveness of Western Mines' pollution control program. In 1973 this program was further upgraded with the addition of an alkaline chlorination plant. Effluent treatment by this method became necessary as a result of process modifications, and has been effective in maintaining the levels of characteristics in the tailings within the ever increasing pollution control requirements imposed on the industry."

Jan 1, 1977

By L Cain, C Every, S Mirlatifi, J Ashley

This paper presents a geographic information system (GIS) based method for the prediction of ground movement and the associated impact on existing buildings and structures due to tunnelling in the North West Rail Link (NWRL) project. The NWRL is a priority rail infrastructure project for the New South Wales (NSW) Government and includes 15 km of twin tunnels between Bella Vista and Epping, which will be Australia’s longest rail tunnels. The NWRL tunnels will be constructed in an urban environment where the prediction of ground movements induced by tunnelling and the associated impacts to existing structures must be assessed in the early design stages of the project. An assessment process was developed using GIS able to respond to design changes.An iterative GIS analysis methodology was developed to generate ground settlement contours and identify impacted buildings and structures in response to multiple changes in tunnel alignment during design development stages. The GIS analysis undertook to rapidly provide detailed and accurate parameter information including tunnel depth from surface, tunnel separation, diameter and sample point proximity to the tunnel and assess ground movement contours along the project alignment. Determination of the ground surface settlements were based on empirical methods proposed by Peck (1969) and Mair (1993). The control parameters and the relationship between damage categories and risk classifications for impact assessment were based on Burland, Broms and de Mello (1977), Rankin (1988) and Boscardin and Cording (1989) methods.The GIS-based ground movement impact assessment approach adopted for the NWRL project demonstrates an efficient, iterative and robust approach and could provide an initial framework for other similar tunnelling projects where rapid design changes and early understanding of tunnelling impacts are required to bring greatest benefit to all stakeholders.CITATION:Mirlatifi, S, Cain, L, Ashley, J and Every, C, 2014. An iterative geographic information system based approach for the assessment of tunnelling impact to existing buildings and structures, in Proceedings 15th Australasian Tunnelling Conference 2014 , pp 647–652 (The Australasian Institute of Mining and Metallurgy: Melbourne).

Sep 17, 2014

By J Loeb, J Dampney, P Cameron

Optimisation of Blast Design and Execution must be done right the first time. It is too late after the ore is broken. Consequences of poor design and execution negatively affect productivity from load and haul through the primary crusher to processing and hence reduce mine site profits. Harnessing and utilising ‘big data’ from geology, geometallurgy, drill hole location, powder loading, blast timing, blast movement and fragmentation to close the loop in blast design and optimise the blast increases productivity across the entire value chain from Mine to Mill. As the internet of things and artificial intelligence increases the quantity of data available, being able to capture and utilise this data to advantage is a challenge. Recent advances in software and hardware together with the increased power of cloud computing allows engineers to close the blasting loop to increase mine site productivity. Numerous case studies over the years detail significant gains from implementing the innovative technologies available to Mine to Mill projects. The opportunity is available for all members of the multi-discipline teams at each mine site to actively ensure productivity improvements are realised and maintained not only in their area, or silo of responsibility but across the entire mine site. This paper refers to recent case studies which outline how significant improvements in productivity are available to all mining operations to increase mine site profitability and dividends to shareholders.

Jun 22, 2022

By R Bertuzzi

"This paper presents preliminary results of ongoing research being carried out at the University of New South Wales Australia (UNSW) into improved methods for estimating rock mass strength. In this paper the rock mass strength of Hawkesbury Sandstone is assessed. An estimate is first made based on an extensive database of intact rock strength data being collated by the author and the assumption that rock mass strength can be determined following the geological strength-index (GSI) approach. The resulting strength envelope is then compared with nine documented case studies where stress induced failure has occurred in tunnels excavated within Hawkesbury Sandstone. The case studies cover a range of conditions: construction dates from 1880s to 2006 spans from 3.2 to 12.5 m depths from 17 to 124 m excavation methods of drill and blast, roadheader and tunnel boring machine (TBM).Finite element modelling is used to assess the likely magnitudes of the principal stresses that were present at the time of the failures. The finite element models are interrogated to provide the values of major and minor principal stresses in and around the mapped failure zones. Failure and stable points are then compared to the proposed strength envelope(s) of Hawkesbury Sandstone derived using the Hoek-Brown and the spalling criteria. The ability of the Hoek-Brown rock mass strength criterion to differentiate between the ‘failed’ and ‘stable’ zones is considered to be remarkable.CITATION:Bertuzzi, R, 2014. Estimating the rock mass strength of Hawkesbury Sandstone, in Proceedings AusRock 2014: Third Australasian Ground Control in Mining Conference, pp 417–424 (The Australasian Institute of Mining and Metallurgy: Melbourne)."

Nov 5, 2014

By Jaeheon Lee, Junmo Ahn, Isabel F. Barton

"Newmont’s Mike prospect, currently undeveloped, is a blind Cu-Au(-Zn) deposit on the Carlin Trend, containing >8.5 M oz. Au, 1027 M lbs. Cu, and 809 M lbs. Zn as Carlin-type gold and polymetallic Cu-Zn minerals in Paleozoic lower-plate carbonates and shales. This project was undertaken 1) to examine the effectiveness of different lixiviants for leaching the Mike supergene Cu-Au ores via bottle roll tests, and 2) to determine what ore minerals resist dissolution in each leaching agent by comparing the mineralogy and chemistry of head and tail samples. Sulfuric and sulfurous acids were used to leach copper and cyanide was used to leach gold. Thiourea, glycine, and other lixiviants were used to leach both base metals and precious metal. QEMSCAN and SEM study of six samples of different ore types and grades indicate that the Au occurs as varieties of native gold, including auricupride and electrum. Major Cu minerals are native Cu, cuprite, malachite, chrysocolla, and conichalcite (Ca-Cu arsenate), with locally significant Cu in jarosite and goethite. Gangue mineralogy is dominated by quartz, sericite, chlorite, alunite, smectite and kaolinite, K-feldspar, and iron oxides (sensu lato). Results of bottle roll tests and leach residue mineralogy will be presented and discussed at the conference.INTRODUCTION Resource and Geologic Setting The Mike deposit is a large, blind Cu-Au(-Zn) deposit in the Maggie Creek district of the Carlin Trend of Nevada, USA, near the Gold Quarry mine (Figure 1). The mineral inventory, based on drilling, is 8.568 Moz. Au, 1027 M lbs. Cu, and 809 M lbs. Zn at average grades of 0.72 g/t Au, 0.34 wt% Cu, and 2.13 wt% Zn (inventory for a cone at $400/oz Au and $0.80/lb Cu by Norby and Orobona, 2002)."

Jan 1, 2017

By T. R. Kostecki, K. V. Jessu

"Roof bolts are subjected to axial stresses, shear stresses, or both. Axial and shear stresses were compared between roof bolts machined with two and three slots. Shear stresses perpendicular to and at an angle to the shear planes were evaluated by analyzing a three-slot instrumented roof bolt, performing laboratory tests on two- and three-slot roof bolts, and conducting in-situ test analyses. Threeslot bolts appear to provide a complete bending strain profile, requiring no prior knowledge of the estimated shear-plane orientation. Minimum displacements occur in roof bolts installed perpendicular to rather than at an angle to the shear planes.RÉSUMÉ Les boulons d’ancrage dans le toit d’une mine sont sujets à des contraintes axiales, des contraintes de cisaillement ou les deux. On a comparé les contraintes axiales et de cisaillement de boulons d’ancrage usinés avec deux ou trois fentes. Les contraintes de cisaillement perpendiculaires et à angle aux plans de cisaillement ont été évaluées en analysant un boulon d’ancrage de toit à trois fentes, en effectuant des essais en laboratoire sur des boulons d’ancrage de toit à deux et à trois fentes et en effectuant des analyses de tests in situ. Les boulons à trois fentes semblent fournir un profil complet de résistance aux contraintes de flexion, sans avoir besoin de connaître l’orientation estimée du plan de cisaillement. Des déplacements minimums ont lieu dans les boulons d’ancrage de toit installés perpendiculairement, plutôt qu’à un angle, aux plans de cisaillement."

Jan 1, 2016

By A. B. Needham

A number of the pegmatites in the southern Black Hills of western South Dakota contain sheet mica; and as the demand increased during World War II the area became an important producer of strategic qualities of mica. During this period of maximum activity, the U. S.. Geological Survey made detailed studies of the geological structural control, the mineralogical associations, and the production Of many pegmatites in the Black Hills. On the basis of results of this study, and at the suggestion of the Geological Survey, several of the pegmatites were examined by the Bureau of Mines, and a few were selected for further investigation. Accordingly, the White Bear, Silver Dollar, Buster Dike, and Hot Shot mines were diamond-core-drilled in 1947. The Hot Shot mine was investigated further by deepening the shaft and crosscutting the pegmatite in 1948. The mica-bearing deposits occur in lenticular intrusions of pegmatite in schists of various mineral composition. Eleven diamond-drill holes, totaling 2,111.4 feet in length, were completed on the four deposits. The shaft on the Hot Shot deposit was deepened 44 feet to the 112-foot level, and crosscuts were driven from the bottom of the shaft to the hanging Wall and foot wall of the pegmatite. This publication briefly describes the location, ownership, and history of the deposits and gives details of the work done by the Bureau of Mines and the Geological Survey.

Jan 1, 1950

By W. P. Sykes

THIS investigation was undertaken primarily to establish the relations existing between temperature and mechanical properties in molybdenum, nickel, and an aluminum-copper alloy. Molybdenum (m.p. 2500° C.) was chosen because it is partly similar to tungsten and partly similar to the common ductile metals. Also it is known to furnish, by proper treatment, a desirable material to use in studying relation of grain size and physical properties. The molybdenum used was of the quality that is drawn into wire 0.003 in. in diameter for use as filament supports in incandescent lamps; chemical analysis shows less than 0.1 per cent. of impurities. Nickel belongs to the same class as iron. Its melting point is 1450° C. and an allotropic change at about 370° C. results in a loss of magnetism above that temperature. This feature made nickel doubly valuable for the purposes of these tests. The nickel used was obtained from the Driver-Harris Co. as 0.090 in. (2.3-mm.) wire, annealed; analysis showed 99.8 per cent. nickel and 0.150 per cent. iron. Aluminum is one of the low melting-point metals. Some tensile tests at elevated temperatures have been reported by Bengough but the possibility of learning more with the low temperature and sensitive apparatus available recommended this metal. The samples marked Al are an aluminum-copper alloy; they contained 3 per cent. copper, 0.42 per cent. iron, and 0.21 per cent. silicon. The presence of the copper somewhat complicates the analysis of the results; but the action of copper in aluminum has been studied so that its influence might have been foretold, in part at least. The material and analyses were furnished by the Aluminum Castings Co. The nickel wire, which was deformed at 400° C., was drawn under a bath of molten lead and through a die, which also was immersed in the bath. A thermocouple was suspended in the molten metal to indicate

Jan 1, 1921

By N. Kanari

Chalcopyrite concentrates and their pure constituents were chlorinated by C12+N2 between 25 °C and 750 °C. The reaction products were analyzed by SEM, XRD and chemical analysis. The effect of gas flow rate and chlorine content of the gas mixture on the reaction rate were investigated. At room temperature, these solids start to react with chlorine giving metal and sulfur chlorides. Complete reaction is achieved at about 300 °C and the iron and sulfur chlorides were fully volatilized. The chlorination residue is composed of valuable metals' chlorides. A simplified flow - sheet for the treatment of chalcopyrite concentrates by chlorine was suggested.

Jan 1, 1998

By Bruno Deves Flores

O presente estudo visou avaliar em escala laboratorial os efeitos da substituição de carvão importado por nacional em misturas típicas para fabricação de coque metalúrgico. Carvão da camada Barro Branco foi amostrado, beneficiado e caracterizado. Misturas entre carvões coqueificáveis importados, coque de petróleo e o carvão brasileiro foram produzidas de modo a permitir a avaliação da influência do carvão nacional na qualidade do coque. O coque gerado no estudo foi produzido em escala de laboratório e posteriormente avaliado a partir de testes de resistência mecânica e reatividade. Os resultados do estudo apontam que a substituição parcial de carvão importado por nacional é viável tecnicamente sem que ocorram prejuízos importantes à qualidade do coque gerado. As diferenças de qualidade dos coques produzidos com ou sem carvão nacional foram menores para misturas com alto teor de inertes, onde as características termoplásticas da mistura passam a controlar a qualidade do coque gerado.

Oct 30, 2017

By R. A. Busch, R. R. Backer, R. W. McKibbin

The Bureau of Mines conducted laboratory tests to determine the slur- ry transport and deposition properties of coal waste. A 188.5-ft pipe test loop was constructed with instruments to measure density, flow, and power and discharge, suction, and differential pressures. A 20-ton sample of Western coal waste was crushed and screened to 100 pct minus 1/2 in. Eight loop tests using this graded waste were run at slurry densities ranging from 1.15 (25 wt-pct solids) to 1.46 (60 wt-pct sol- ids). The resultant friction-pressure gradients ranged from 0.06 to 0.24 ft of water per foot of 4-in standard steel pipe. Particle-size degradation was significant. In a typical loop test lasting 25 min, the minus 200-mesh fraction increased from 19 pct to 34 pct. Deposi- tion tests showed that without the use of a flocculant, the slurries would not dewater when left to stand for 1 week. With flocculant, ad- ditional water was released; however, the settled slurries remained thixotropic. Further testing is necessary to determine their suitabil- ity for use as backfill material in active mines.

Jan 1, 1965

By Wolfang Ladewg

Desde enero hasta agosto de 1965 se probó un prototipo del telémetro electro-óptico EOS de VES Carl Zeiss JENA, a través de las mediciones en unos 70 días. En ese sentido, el objetivo del presente texto es determinar la exactitud de medición, así corno la constante de adición y el alcance del EOS. Para ello, se midieron distancias geodésicos a base estandard en los campos de ensayo geodésicos de Potsdarn y en una red de ensayo determinada trigonométricarnente. La medición de las distancias se realizó en tres días, empleándose un reflector de siete prismas con sus correspondientes cuñas adicionales. Mientras que en los campos de ensayo geodésicos se midieron 19 distancias entre O, 1 y 7,5 km. Las mediciones se efectuaron en un espacio de tres meses en total con diferentes números de series

Nov 1, 1970

By T. E. Leontis

The specific effect of various rare-earth metals on the room- and elevated-temperature properties of magnesium has been evaluated. Alloys containing didymium exhibit the highest tensile and compressive strengths at room and elevated temperatures. All the rare-earth metals increase the creep resistance of extruded magnesium at temperatures in the range of 400° to 600°F, but the degree of enhancement depends on the temperature and on the concentration of the added metal. THE effects of rare-earth metals on the properties of sand-cast magnesium were discussed in some detail in earlier paper by the author.' The present paper deals with the effect of the same alloying elements on the properties of extruded magnesium. This investigation also had as its aim the development of a wrought alloy having a better combination of room-temperature strength and ductility and elevated-temperature strength and creep resistance than is found in magnesium-Mischmetal-manganese alloys, which have been reported earlier.2-5 The only known attempt to study wrought magnesium alloys containing pure cerium instead of Mischmetal was made by Mellor and Ridley.6 They found that in the form of rolled bars there is a definite, optimum cerium content for creep resistance at 200 °C and that the creep resistance of these alloys at 200 °C is significantly Improved by heat treatment at 550" to 580"C. In the present investigation the compositional variation in mechanical properties of the following alloy systems is presented: I—magnesium-Misch-metal. 2—magnesium-cerium-free Mischmetal. 3— magnesium-didymium. 4—magnesium-cerium. 5— magnesium-lanthanum. Alloys containing predominately praseodymium are not included in this series because of the lack of this material. Experimental Procedures The alloying ingredients used in preparing the alloys described herein are the same as those reported in the earlier paper.' Cerium-free Mischmetal is the rare-earth mixture remaining when the cerium is removed from Mischmetal, which contains all the rare-earth metals as they occur naturally in mon-azite sand, the ore from which Mischmetal is produced. Removal of both cerium and lanthanum from Mischmetal leaves what is commonly called "didym-ium," consisting predominantly of neodymium and praseodymium. Although the composition of the particular batch of each metal used may differ somewhat from the analysis presented previously, these differences are not great enough to warrant repeat- ing the specific composition of each material. The electrolytic magnesium used as the starting material in these alloys has the same typical analysis as that given in the earlier paper.' The alloys were prepared in small laboratory melts applying all the necessary precautions for alloying rare-earth metals with magnesium described by Marande.' Most melts were large enough to cast one 3 in. diam billet 10 in. long. In a few cases, particularly the didymium-containing alloys, the lack of sufficient amounts of the rare-earth metal limited the size of the billet to 6 to 8 in. All billets were scalped to a diameter of 2 15/16 in. and faced to a length of 9 ¼ in. as limited by the size of the extrusion container. The alloys were extruded into ½ in. diam rod on a 500-ton direct-extrusion press using a 3 in. container. The details of the extrusion step are: billet preheat, 925°F (2 hr); container temperature, 900°F; die temperature, 900°F; extrusion speed, 10 ft per min; reduction ratio, 36:1; and percent reduction, 97.3. The lower melting point of alloys containing didymium' necessitated reduction of the extrusion speed to 5 ft per min in order to prevent hot shorting during extrusion. Adequate lengths were cropped from both ends of each extruded rod to assure that all the material used for tests was extruded under uniform conditions. Tensile and compressive properties at room temperature are reported in the several conditions of heat treatment. The ASTM designations are used to distinguish these conditions as follows: T5—Direct age at 400°F (16 hr) T4—Heat treat at 950°F (4 hr) for alloys containing didymium T4—Heat treat at 1050°F (4 hr) for all other alloys T6—T4 + age at 400 °F (16 hr) The lower heat-treating temperature for alloys containing didymium is necessitated by the lower melting point of these alloys. All heat treatments were conducted in electrically heated, circulating-air furnaces. A protective atmosphere containing 0.5 to 1.0 pct sulphur dioxide was used for the high temperature heat treatments. Tension and creep specimens 6 Yz in. long and compression specimens 1½ in. long were cut from the extruded rod. A reduced section of ? in. diam was machined on the tension specimens, whereas on the creep specimens a reduced section of 0.450 in. diam

Jan 1, 1952

By J. P. Nielsen, H. Margolin, E. Ence

The Ti-Ni phase diagram has been investigated up to 68 pct Ni with iodide titanium base alloys by metallographic, X-ray, and melting point methods, and from 68 to 90 pct Ni by examination of as-cast structures of sponge titanium base alloys. NVESTIGATION of the nickel-rich portion of the I Ti-Ni phase diagram was first reported by Vogel and Wallbaum in 1938.' This work was subsequently extended to lower nickel contents by Wallbaum' who indicated the possibility of a eutectic reaction for nickel contents below 38 pct. Long et al.3 studied the titanium-rich portion of the phase diagram and found eutectic and eutectoid reactions below 38 pct Ni. However, the temperature of the eutectic indicated by Long et al. was considerably lower than that suggested by Wallbaum. Long and his coworkers synthesized their alloys by powder metallurgical techniques and encountered oxygen and/or nitrogen contamination. Thus the diagram which was obtained did not represent binary alloying conditions. However from these results the features of the binary diagram were predicted. At Battelle Memorial Institute4 the Ti-Ni diagram was investigated up to approximately 11.5 pct Ni with sponge titanium alloys. The range of temperatures used was not sufficient to define the eutectoid temperature or composition. The data of Wallbaum2 and Long et al.8 were of particular interest for the present study, and although the work was originally concerned with the region below 40 pct Ni, the investigation was extended to higher nickel contents in an attempt to resolve the differences between these workers. Experimental Procedure Preliminary work on the Ti-Ni system was carried out with duPont Process A sponge titanium alloys to reduce the amount of subsequent work to be done with iodide titanium base alloys. The sponge titanium used contained 99.71 to 99.77 pct Ti, 0.1 pct Fe and 0.005 to 0.009 pct Ni. The iodide titanium obtained from the New Jersey Zinc Co. contained 99.9 to 99.95 pct Ti. Nickel used with sponge titanium was 98.9 pct pure. The high-purity nickel alloyed with iodide titanium was cobalt-free with approximately 0.05 pct C and was obtained through the courtesy of the International Nickel Co. The 15 g sponge titanium charges for melting were prepared by compacting in a die or by placing the weighed portions of nickel and titanium directly into the furnace. Iodide titanium charges were made by drilling holes in the as-received rod and inserting the nickel or by wrapping the nickel in sheet. Sponge titanium alloys containing from 0.2 to 90 pct Ni and iodide titanium alloys containing 0.2 to 68 pct Ni were prepared by these methods. In addition to these alloys several 1/2 1b sponge titanium alloys were supplied by the Allegheny Ludlum Co. The charges were melted in an arc furnace under an argon atmosphere. The procedures used were similar to those reported in the literature5,' and the furnace has been described.' Except for iodide titanium alloys with 40 to 68 pct Ni (see section on copper contamination), each alloy was melted for 1 min, then either turned over or broken before re-melting for an additional minute. Currents of 200 to 400 amp were used depending on the melting point of the alloy. Prior to heat treatment, alloys containing less than 14.5 pct Ni were hot-forged at 750°C. With the exception of alloys in the homogeneity range of the compound TiNi, alloys of higher nickel contents could not be hot-forged. Heat treatment of iodide titanium base alloys was carried out in argon-filled quartz capsules which were broken under water at the conclusion of heat treatment to quench the specimens. Temperatures were controlled to ±5oC and annealing times up to 48 hr were used. For melting point determination, specimens were placed in carbon crucibles which were in turn en-capsuled in argon-filled quartz capsules. The start of melting was determined by rounding of corners and by metallographic examination. Complete melting was considered to have occurred at that temperature at which the specimen assumed the shape of the crucible. Specimens were prepared for metallographic examination by mechanical polishing or by an electrolytic procedure." For alloys containing up to 80 pct Ni Remington A etch7 50 pct glycerine, 25 pct HNO,, 25 8 HF) was used. For higher nickel alloys aqua regia and Carapella's etch (5 g FeCl,, 2 ml HNO,, and 99 ml methyl alcohol) were employed. Specimens to be exposed for powder patterns were prepared by filing, by breaking specimens in a

Jan 1, 1954