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By K. P. Mukherjee, K. P. Gupta, J. Bandyopadhyaya

Even though a lot of work has been done in the past to establish phase equilibrium in the Cu-Si system a re cent investigation casts some doubt about the existence and crystal structure of some of the phases that form in the composition range of 15 to 25 at. pct Si in Cu. The present investigation was carried out using high temperature X-ray diffraction technique along with other standard techniques to study the phases in this composition range. The high temperature 6 phase appears to be tetragonal with parameters a,, = 8.815A, c, = 7.903A, and co/ao = 0.896. The reported bcc E phase exists at room temperature and at least up to 780°C and appears to undergo a transformation near 600°C. The phase appears to be cubic but not of the bcc type. The ? phase appears to undergo a transformation, as has been indicated by earlier investigators, and the low temperature form of .? phase is tetragonal with parameters a, = 7.267A, co = 7.8924, and co/ao = 1.086. THE Cu-Si binary system has been investigated by several investigators1" and several intermediate phases,?,e,?' at lower temperatures and ?,ß,0,e, and ? at higher temperatures, were observed between terminal solid solutions of copper and silicon. Even though the existence of the e phase and the transformation in the ? phase were reported in many early works, in a recent study of this system Nowotny and Bittner6 doubted the existence of the e phase and phase at 550°C. Among the high temperature phases, the 6 phase was reported to have a complex cubic structure with parameter a, = 8.805A.7 Nowotny and Bittner, however, suggested that the structure of the 6 phase might be of CsCl type. In order to check these contradictory reports the present study was taken up to investigate the Cu-Si binary system in the composition range of 17 to 25 at. pct Si. EXPERIMENTAL PROCEDURE Weighed amounts of copper (99.99 pct) and silicon (99.9 pct) were induction melted in recrystallized alumina crucibles under argon gas atmosphere. The alloys containing 17, 18, 20, 21, 21.2, 22, and 24 at. pct Si were annealed in evacuated and sealed quartz capsules at 700°C for 3 days and subsequently water quenched. Other than this annealing, the 21.2 at. pct Si and 24 at. pct Si alloys were annealed at 550°C for 10 days, the 17 at. pct Si alloy was annealed at 750°C for 3 days, and the 22 and 24 at. pct Si alloys were annealed at 780°C for 2 days. All annealing temperatures were controlled to within *l°C. Alloys after quenching were subjected to metallographic and X-ray diffraction investigation. A solution containing 5 g FeC13 + 10 cc HCl + 120 cc H2O diluted with six times its volume with water was used as etching reagent. A 114.6 mm diam Debye Scherrer camera was used for obtaining diffraction patterns. The 17, 21.2, and 24 at. pct Si alloys were subjected to high temperature diffractometry using a Tempress Research High temperature attachment and a GEXRD VI diffractometer. For the 6 phase (17 at. pct Si alloy) powder specimen from a 750°C annealed alloy was reheated to 750°C in the high temperature attachment for 1½ hr before taking a diffraction trace. A 550°C annealed and slowly cooled phase (24 at. pct Si) alloy was first reheated to 550°C. a diffraction trace was made after annealing it for 2 hr, and subsequently it was heated to 716OC and kept at this temperature for 2 hr before taking a diffraction trace. For the e phase (21.2 at. pct Si alloy) a 550°C annealed and slowly cooled specimen was heated first to 425°C and annealed at this temperature for 2 hr before taking a diffraction trace. Subsequently, the specimen temperature was raised to 495", 540°, 603", 635", 682", 720°, and 748°C and homogenized at each temperature for 1 hr before taking diffraction traces. The powder specimen temperature was controlled to within +2oC at each temperature and argon gas, purified by passing it at slow rate through a fused CaC12 column, hot (800°C) copper and titanium chips and finally through a P2O5 column, was used to prevent oxidation of the powder. For all X-ray work copper-radiations at 25 kv, 15 ma (for Debye Scherrer technique), and 40 kv, 20 ma (for diffractometer tech-nique) were used. RESULTS AND DISCUSSION At 700°C the alloys containing 17 to 21 at. pct Si showed two phases while the 21.2 at. pct Si alloy was found to be single phase. The X-ray diffraction patterns of the two-phase alloys were consistent with the phase (ßP-Mn type structure) and the phase (21.2 at. pct Si) patterns. The diffraction patterns of the 17 at. pct Si alloy quenched from 750" and 700°C were identical. According to the accepted Cu-Si phase dia-gram4,5,10 the 17 at. pct Si alloy at 750°C should be in the (k + 6) two-phase region and very close to the -phase boundary. The identical patterns possibly resulted from the decomposition of the 6 phase on

Jan 1, 1970

By Tong Guan, Guangqin Fu, Lihong Deng, Yuanlin Chen, Xiaotong Zhou

"In natural world, some kinds of scheelite minerals are rich in molybdenum. Molybdenum exists in the crystal lattice of scheelite in the form of isomorphism, and the content of MoO3 varies from 2% to 10%. As a result, the flotability of seyrigite (scheelite with molybdenum) turns to be weaker. One seyrigite mine, which has been built for 3 years,still could not produce qualified seyrigite concentrate due to the weak flotability of seyrigite (Mo-bearing scheelite) in raw ore. In our experimental research, through adopting new seyrigite collector TA-3 and advanced mineral processing technology, the seyrigite concentrate with a grade of 65.62% WO3 at a recovery of 87.47% was obtained for the raw ore containing 0.19% WO3 and 0.074% Mo. By applying the new technical achievement, for the raw ore containing 0.272% WO3, the seyrigite concentrate assaying 68.03% WO3 with a recovery of 77.56% was obtained in industrial production.INTRODUCTIONIn natural world, some kinds of scheelite minerals are rich in molybdenum. Molybdenum exists in the crystal lattice of scheelite in the form of isomorphism, and the scheelite is changed to be seyrigite (Ca[(W,Mo)O4]) (Ma, Bian, & Wang, 2013). The content of MoO3 in seyrigite varies from 2% to 10% usually, the content of MoO3 in some of the seyrigite even reaches 34%. The flotability of seyrigite is weak (Zhang, 2007), and the seyrigite is difficult to be recovered by flotation with common collectors and regulators. One scheelite mine in Anhui China, which is a skarn type seyrigite mine, has not produced qualified concentrate yet since 3 years it has been built due to the limit of beneficiation technology. Therefore, it is necessary to conduct research on the collectors with high efficiency and developing advanced processing flow for this kind of ore."

Jan 1, 2016

By S. H. Morar

Froth flotation is a physico-chemical separation process that takes place in two phases; pulp and froth phase. It is widely recognised as a complex process, due to the range of interactions present within the system. Of critical importance is the role of the froth phase within the system. The pulp kinetics governs the maximum potential recovery within a flotation cell, while the froth phase governs the selectivity via the froth?s stability. Higher froth stability improves recovery at the expense of grade, and lower froth stability improves selectivity. It is well known that the two major factors affecting froth stability are attached particles and solution chemistry. This paper looks at a flotation bank at different froth depth and frother concentrations. The air recovery to the concentrate is determined at each condition and relates the effect of the operating conditions on froth stability and transport to the amount of solids that are recovered to the froth and concentrate by true flotation. The results presented show that, for a given process objective, which in this case was a consistent mass pull profile, depending on the operating conditions, solids recovery in the pulp is affected by the air rate required to maintain the target mass pull. To a smaller extent, the changes in the pulp composition affect down-stream pulp recovery. The variation in solids recovered into the froth drives the froth stability at the start of the flotation bank, while the frother drives the froth stability at the end of the bank. The performance in between these two extreme conditions arises from an interaction of these two effects. The consequences of these interactions can give rise to counter-intuitive responses that can confound efforts to optimise the performance of the bank.

Jan 1, 2014

By PERCY E. BARBOUR

SECONDARY copper1 has &come more or less of a bugbear generally. What is its influence is often the subject of heated argument. The inedapable fact usually quoted is that since in 1929 primary production of copper in the United States was 1,026,348 tons and secondary production was 626,550 tons, there- fore, 0.6 lb. of secondary is produced for every pound of primary, and "How can you get around that?" The matter seems very plain, now that I have reached my conclusions, but they are the result of much laborious study and research. I shall show that' the production of secondary copper is not 0.6 per lb. of primary, in spite of statistical appearances; that the production of secondary is a function of primary production rather than of price; that secondary production has 'only a sub-. ordinate influence on the price of copper and then only in abnormal times; that there is not an accumulating reservoir of secondary from which the country is some- time to be drowned in copper, as is believed by some, or a reservoir from which we are going to draw much needed and more or less inexhaustible stores in the future, as is believed by others; and finally, that the United States always produces more copper than it uses and exports the surplus. These are all controversial points, and for that reason and to anticipate argument I have set forth my reasoning in considerable detail.

Jan 1, 1931

On the following pages are abstracts of papers published by the Institute during the year 1934 as TECHNICAL PWLICATIONB, CONTRIBUTIONS, m bound volumes and in MINING AND METALLURGY. For abstracts of papers that appear In bound volumes in 1934 but that were published as TECHNICAL PWLICATIONS m 1932 or 1933, see the TRANSACTIONS for 1932 and the YEAR BOOK dated January, 1934. Many of the TECHNICAL PWLICATIONS have been reprinted In bound volumes Information regarding this disposition, and number of pages in each paper, may be found m the list beginning on page 92 Volume numbers are given as listed at the beginning of the index, page 99 The abstracts are grouped as follows:

Jan 1, 1935

By J. A. Organiscak

The U.S. Bureau of Mines investigated the relationship of bituminous coal seam parameters and the amount of airborne respirable dust generated at longwalls. Dust and coal samples were obtained from 20 longwalls operating in geographically representative coalfields throughout the United States. Statistical analyses of coal seam parameters and airborne respirable dust measurements indicate a likely causal relationship between seam type and respirable dust. Low-ash, high-volatile coal seams were associated with higher airborne respirable dust levels. A negative linear correlation (significant at the 95-pct confidence level) was observed between the seam's ash content and airborne respirable dust, explaining up to 18 pct (R2 = 0.18) of headgate dust level variation and up to 15 pct of tailgate dust level variation. Volatile matter was found to have a positive linear correlation with tailgate dust level, explaining 16 pct of the variation. Further data examination indicates that these relationships with dust are most likely nonlinear, because of improved R2 values over the linear correlations. However, a notable portion of longwall dust production is influenced by other operational parameters, so additional research under more controlled conditions is needed to determine the seam's causative functions.

Jan 1, 2010

By S. R. Maynard

The Ortiz Mountains lie 25 mi (40 km) northeast of Albuquerque, New Mexico in Santa Fe County (Figure 1). Approximately 350,000 ounces (11,000 kgs) of gold have been produced from the Ortiz Mountains since the 1820s. The 100 square mile (260 square km) Ortiz Mine Grant was secured from the Mexican government in 1833 by Jose Francisco Ortiz for the purpose of mining gold. The Grant has remained more or less intact to the present. The mineral rights are currently owned by Ortiz Mines, Inc. of Joplin, Missouri and are leased to LAC Minerals, USA, Inc. (west half) and to Gold Fields Mining Corporation (east half).

Jan 1, 1989

By H. E. Powell

This Bureau of Mines study describes two processes for recovering zinc, copper, silver, and iron from the magnetic fraction of a waste generated by the primary smelting of zinc in horizontal retort distillation furnaces. The laboratory-scale procedures include reduction melting to produce a high-copper iron and matte smelting to produce a copper-silver-iron matte and metallic iron. Zinc is fumed in each process and recovered as the oxide. Direct reduction melting yields a metallic iron high in copper and a small rich matte from the sulfur contained in the waste. The products of the second process are a matte containing essentially all of the silver, about 80 pct of the copper and 37 pet of the iron, and an iron-copper alloy containing all of the remaining copper. Extraction with metallic lead or sodium sulfate recovers essentially all of the copper from the molten high-copper iron and yields an acceptable foundry iron.

Jan 1, 1973

By Irving Hartmann, John Nagy, Donald Mitchell

"SUMMARY AND CONCLUSIONThe test data indicate that water infusion of the Pittsburgh coal seam does not reduce the amount of fine dust produced during mining operations to the extent reported elsewhere. Wide variations in the amounts of dust collected in the air current were noted in duplicate samples and repetitive tests. Changes in depth and location of the infusion holes and amount of water injected and addition of a wetting agent to the water had little effect on the amount of dust liberated.Water was forced readily into the coal. Some water flowed out along the cleats, but an appreciable amount remained in the seam. Little or no water pene¬trated the coal seam above the upper infusion holes.The average dust concentration (with and without infusion) in the return air, 40 feet outby the working face, was 25 million particles per cubic foot during undercutting, 20 million during drilling, 75 million during shot firing, and 20 million during hand loading. At the working face the average concentration was 3 to 6 times higher. The concentrations were measured at an airflow of 1,600 cubic feet per minute (c.f.m.) at the face.On the basis of this short investigation, no final conclusions can be made on the effectiveness of water infusion in reducing the amount of fine dust liberated during mining in the Pittsburgh coal seam. However, the data indicate that dust reduction resulting from infusion would be small.INTRODUCTIONThe production of fine coal dust is an inherent part of nearly every phase of mining. The use of large, high-speed continuous-mining machines and other mechanical equipment has increased dust production. In addition, in coal seams that have been subjected to high pressures for a long period, and particularly in dry and friable seams, some very fine dust is in the seam before mining. Much effort has been devoted to allaying and collecting at its source the fine coal dust released during mining. One of the comparatively recent techniques that has been developed for this purpose is infusion of water or other liquids into the coal seam. This method consists of injecting water under pressure into a coal seam to neutralize the fine dust released during mining. The water generally is introduced through bore holes in the face before undercutting."

Jul 1, 1957

By Donald W. Mitchell

Certification tests for urethane-foam systems and techniques for apply-ing foam safely in mines are described. Fire hazard from foam exists if flame propagates beyond the ignition source or penetrates the foam. Foam that passes the certification tests can be applied on stoppings, continuous sections of ribs of relatively wide passageways (with no foam on the roof), short sections of roof such as overcasts, roof cavities, and intersections (with no foam on the ribs), and between buntons on one wall of a shaft. Foam on the ribs and adjoining roof presents a fire hazard. Stoppings covered with foam passing the certification tests are resistant to penetration of heat, flame, and smoke than similar stopping without foam. Flame propagation can be arrested by water sprays. Spontaneous ignition of foam can be prevented.

Jan 1, 1966

By Sidney Snook

FLUORSPAR production is the most important industry in a compact area in southern Illinois and western Kentucky bordering the Ohio River. Producers' activities do not usually figure much in the mining news of the country, so that few know that the last year or so has been an unusually active one. Mine shipments more than doubled in 1939 compared with the poor year 1938. The average price changed but little, though it is now about one-sixth higher than at the beginning of last year. The outbreak of war in Europe a year ago lent an immediate stimulus to the industry, though only about 15 per cent of the domestic consumption is normally imported, thanks to a tariff of $8.40 per ton, equivalent to about 30 per cent ad valorem. Be- cause of the increased production and many expansions and improvements in the mines and plants, the period since the beginning of 1939 has been the most important one for the industry in the last 15 years.

Jan 1, 1940

By Ludimila Melo Vieira

O foco deste estudo é avaliar a capacidade de dissolução das partículas de cal a uma temperatura próxima da fase inicial de sopro do processo BOF. Os testes foram realizados em um forno elétrico utilizando amostras de Cal com diâmetros de 6 mm e 9 mm, 80% e 100% calcinadas em diferentes basicidades de escoria. Os resultados mostram que com o menor nível de calcinação a dissolução foi mais rápida. Podendo ser atribuído a algumas diferenças na porosidade da cal ou um efeito de formação de espuma observado durante os testes devido à evolução do CO2 da calcinação restante. O aumento na basicidade da escória resultou na redução da taxa de dissolução que pode ser atribuída a uma precipitação de fase sólida mais densa na interface das partículas aumentando a viscosidade da escória e reduzindo a porosidade da partícula. A partir de um modelo de regressão linear o nível de calcinação mostrou maior efeito sobre o coeficiente cinético do processo de dissolução seguido do tamanho de partícula. O efeito mais fraco foi a basicidade da escória. Este resultado sugere que a área de contato cal escória parece ser mais significativa do que a viscosidade no processo de dissolução de cal nos presentes experimentos.

Oct 30, 2017

By M R. Asef

Although generation of environmentally harmful hydrogen sulfide is considered to be related to sour gas fields, sweet gas reservoirs and waste fluids, travertine springs and geothermal fields may also produce acid gas (H2S and CO2) under certain conditions. The potential parameters influencing such a possibility need to be fully investigated to evaluate the extent of the consequences and predict hydrogen sulfide generation accordingly. Reports on hydrogen sulfide production at different regions and fields were gathered worldwide for the cases when some of them did not have such a problem previously. In order to inspect different aspects of these case studies, some other regions with no hydrogen sulfide content were selected as control. In all cases water samples were taken carefully for chemical analysis in the laboratory. Besides, mineral compositions were characterised in some cases for better evaluation. In order to give a thorough prospect of hydrogen sulfide production, a geochemical model was prepared. In situ engineering geological conditions, especially pressure and temperature, were assigned in the model to investigate the possibility of H2S generation using PHREEQC software. The results of modelling revealed that although many similarities existed between mineral compositions of the cases, certain formations were particularly prone to hydrogen sulfide generation. For better evaluation, important exchangeable cation ratios such as potassium/sodium, calcium/magnesium and ion proportions like sulfate and chloride were calculated as trends of the formations. As expected, the model could successfully monitor a higher ratio of SO42- and Cl- in potential H2S generator formations. Wide variation in percentage of HCO3- was considered as a secondary observatory parameter for better estimation. In addition, it was noticed that higher anion content created an environment ready to absorb any cations and this makes H2S generation easier. Finally, using correlations between predictors and estimators for low depth and deep samples defined the degree of effectiveness for every sample.

Sep 26, 2011

By D. Boreck

The Bureau of Mines is conducting research on the feasibility of incorporating in situ stope leaching into active underground metal mines. Stope leaching, a modified in situ leaching technique, proposes to recover metals by leaching fragmented ore in existing underground openings and collecting and processing the metal-bearing solution to recover the valuable metals. If leaching solutions escape from the stope, either through geologic discontinuities or highly permeable zones in the rock, valuable metals dissolved in the solution may be lost. Escaping solutions may also contaminate ground waters. Consequently, in fractured rock, the characteristics of the fractures in the vicinity of the leaching stope must be understood before introducing actual leach solutions into the stope. Effectively characterizing a rock mass requires the integration of several disciplines including structural geology, borehole geophysics, hydrology, geochemistry, and mining engineering. This paper will focus on the general geologic and geophysical techniques that can be used to characterize the rock mass at an underground simulated stope leaching site. The results of several geophysical logging methods, tested at the site, are compared to the geologic core descriptions. Then, the? effectiveness of the different geophysical techniques in delineating fracture zones will be assessed. Knowledge gained through the geologic and geophysical analyses can be used to supplement results from hydrologic testing. This information can also be utilized in designing blast patterns and developing strategies for controlling or blocking movement of escaping leach solutions.

Jan 1, 1991

By James R. Dunn

The mineral industry" has made and will continue to make important contributions to the growth of our economy. However, the industry is presently under continuous and increasingly severe attacks by organizations and individuals interested in the preservation of our environment. Yet neither the public interest value of preservation nor the public interest value of our mineral industry is known. In the absence of such values, judgments about best land use where minerals are involved are nearly always made on emotional grounds. An example of the sort of problem that has been created is in the New York Metropolitan Area. Because of institutionally-created shortages stemming largely from zoning decisions and building over deposits, the effective cost of fine aggregate delivered at dockside at Manhattan rose from $2. 65/cubic yard in July, 1969, to $4.10/cubic yard in May, 1970, this in spite of approximately ;l0,000 years of reserves on Long Island. The cost of fine aggregate for New York City alone has "Increased over $S million annually within one year, with the cost increase for the Tri-State Metropolitan Area (coastal Connecticut, New Jersey, and New York)" exceeding $10 million annually. The ab0ve situation has created a cost increase which is clearly the result of non-conservation of a mineral resource. That is, in readily measurable values, it Is costing the public about $10 million per year because good conservation practices were ignored-a public-interest loss. Admittedly, this is not the whole story because the public is simultaneously obtaining other values from the land surface that would otherwise have had to be dedicated, temporarily to be sure, to mineral recovery-a public-interest gain. However, the point is that we do not know where the balance lies-the net public interest value; it may lie one way for deposits zoned out of existence by a growing suburb, another for areas designed as permanent greenbelts, and still another for areas under new highways

Jan 1, 1971

By S. M. Marshall

The investigations recorded in this bulletin were conducted by the Pacific Coke & Coal Co. in cooperation with the United States Bureau of Mines and the University of Washington. They cover one phase of a comprehensive investigation to determine whether coals from an extensive, undeveloped area of Pierce County, Wash., can be used in the manufacture of coke for the iron blast furnace. The completed investigation had three parts: (1) A geological survey of the coal property, (2) washing and crushing tests of the coals, and (3) coking and by-product tests. The geological survey, which was not conducted in cooperation with the Bureau of Mines and the University of Washington, included systematic tracing of the coal beds by test holes throughout the property, except some portions covered by an impenetrable layer of glacial drift. By this means all of the beds were correlated, their thickness and general character were determined, and tonnage estimates were made. Only such parts of the survey results as are necessary to a full explanation of the investigations described herein are included in this bulletin.

Jan 1, 1931

By G. M. Potter, J. B. Rosenbaum, Masami Hayashi

Most Japanese copper smelters are located in areas of concentrated industrial activity and high levels of atmospheric pollution. A review of unofficial sulfur dioxide emission control data from major Japanese smelters shows capture of 91 to 99.7 percent of the sulfur in the smelter feed. The bulk of Japanese smel ting capacity was constructed in the last 10 years. Six of the major sme lters use flash furnaces, and two use reverberatory furnaces. A prototype three-furnace continuous system is in use as a parallel train with reverberatory furnaces at one smelter. Most of the sulfur dioxide is manufactured into sulfuric acid. The remainder is captured by gas scrubbers that yield gypsum and sodium salts. Ready markets exist in Japan for the acid and other su lfur byproduc ts.

Jan 1, 1967

In 1991, the USBM (U. S. Bureau of Mines) evaluated the mineral resources of the 174,550-acre Bear Creek-Poker Peak area. Located 40 air miles east from Idaho Falls, ID, the study area is in the Caribou National Forest but is mostly administered by Targhee National Forest. USBM personnel mapped and sampled mines, prospects, and mineralized sites in and near the study area. Five types of mineral occurrences were identified in the study area: phosphate, limestone and travertine, placer gold, coal and uranium (the latter contained in the coal), and oil and gas. The study area has a high potential for oil and gas; evaluation of these commodities were beyond the scope of this study.

Jan 1, 1992

By Rodrigo Alberto Moreira Gomes

Para a purificação do níquel laterítico explorado na mina localizada em Niquelândia/GO, pela Votorantim Metais Níquel (VMN), utiliza-se solução amoniacal durante a etapa de lixiviação do minério, seguindo a rota hidrometalúrgica de produção. A amônia é recuperada em torres de destilação por arraste com vapor vivo, para ser reutilizada em um novo ciclo de produção. Este trabalho apresenta a aplicação de uma tecnologia baseada em lógica Fuzzy no conjunto de 6 torres de recuperação de amônia, com o objetivo de controlar as alimentações de solução a ser purificada e de vapor. A plataforma de controle avançado utilizada, Leaf, foi desenvolvida pela I.Systems Automação Industrial, empresa localizada em Campinas/SP, e não necessita da criação de modelos matemáticos fenomenológicos para geração e sintonia dos controladores. Com a automatização da operação das torres, o consumo de vapor da unidade foi reduzido em 3,5% e a intervenção manual foi reduzida.

Sep 25, 2017

By K. Tangri, M. Chaturvedi

On water-quenching from within the (a + ß) phase region Zr-2.5 Nb and Zr-2.5 Nb-0.5 Cu alloys can undergo w transfirmation. This transformation has been attributed to the enrichment of ß Zr phase, at the solution-treatment temperature, by the solute atoms. The ß—w transformation is accompanied by a hardening 01 the alloys and in the optimum condition w-bearing specimens of the ternary alloy are about 14 pct harder than those bearing only a' phase. On aging crl reverls thermally to more stable phases, which results in a considerable softening of the specirnens, as follows: w quenched -waged + ß Zr (enriched) waged - a + ß Nb The high-temperature bcc ß Zr in certain zirconium alloys can transform to a metastable w phase which has a primitive hexagonal structure. In the Zr-Nb alloy system w phase has been observed in the composition range of 7 to 15 wt pct Nb by a number of investigators.'-' In this composition range w can form by water-quenching ß Zr or by aging. known as athermal and thermal w, respectively. Hatt and Roberts' have found that thermal w has a constant c/a ratio of 0.622 +0.002 regardless of the composition and tha: the lattice parameters are of the order of a = 5.02A and c = 3.0 ?. The actual lattice parameters depend upon composition and the temperature of aging. The lattice constants of athermal w. however, depend upon alloy composition.3 The presence of w phase in zirconium alloys can cause substantial strengthening which has been attributed as probably due to the coherency between w and parent ß Zr phase. Robinson et al.' found that the presence of w can raise the strength of Zr-5.0 Nb-2.0 Sn and Zr-5.0 Mo-2.0 Sn alloys to about 170.000 psi: however. the ductility is considerably reduced. With the growing use of Zr-2.5 Nb and Zr-2.5 Nb-0.5 Cu alloys in the nuclear reactors, and the significant effect of w transformation on the mechanical properties of zirconium alloys studies were undertaken to study the w transformation in Zr-2.5 Nb and Zr-2.5 Nb-0.5 Cu alloys. This paper is concerned with the formation and reversion of w phase in these alloys. 1) MATERIALS AND EXPERIMENTAL TECHNIQUES The following two alloys were studied: 1) Zr-2.5 Nb-0.5 Cu (referred to as the ternary alloy): 2) Zr-2.5 Nb (referred to as the binary alloy). The chemical analysis of the alloys is given in Table I. The alloys, in the form of 3/8-in.-diam rods and 1/8-in.-thick sheets, were supplied by the Chalk River Nuclear Laboratories of the A.E.C.L. Initial fabrication for preparation of various specimens was carried out by cold rolling and swaging with intermediate anneals at 1000°C. All the heat treatments were carried out after the specimens were wrapped in zirconium foils and encapsulated in silica tubes under a vacuum of 5 x 10-% m of Hg. For optical metallography and hardness measurements disc specimens + in. diam by + in. thick were used. After the required heat treatments the specimens were mechanically and then chemically polished in a 45 pct HNO3, 45 pct H20. and 10 pct HF solution. The hardness measurements on the chemically polished specimens were carried out on a Vickers hardness tester using a 10-kg load. For each specimen at least fifteen indentations were made in order to obtain a representative hardness value. The phase identification and structural analysis were carried out using X-rays and electron diffraction techniques. Wires of 1.5 mm diam reduced to 0.12 mm diam by chemical etching were used for making Debye-Scherrer powder patterns using copper K-a radiations in 114.6-mm-diam camera. Thin films for transmission electron microscopy were prepared by electropolishing heat-treated a by 7 by 0.005-in.-thick strips using a modified Bollmann-Window technique. The 10 pct perchloric acid-90 pct methyl alcohol electropolishing bath was kepl at -5OCC and polishing was done at 5 to 10 v. The thinned specimens were washed in ethyl alcohol at -30" to -40°C and dried between filter papers. The thin films

Jan 1, 1970