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By D Craw

The Rise and Shine Shear Zone is a mineralised low angle deformation zone traceable for at least 7 km through biotite zone schist of the Dunstan Range, central Otago. Rocks from the shear zone obtained from recent drillholes are unweathered and facilitate paragenetic studies. There is a progression of mineral deposition from semiductile foliation-parallel shearing, to subsequent folding, and brittle fracturing. Sheared rocks are dominated by microshears containing fine grained hydrothermal muscovite and rutile that has recrystallised from metamorphic muscovite and titanite respectively. Euhedral pyrite occurs within segregations in the schist and is locally brecciated by the shears.   Arsenopyrite occurs within microshears and is intergrown with hyrothermal muscovite. Fractures within relatively undeformed schist are filled with ankerite, siderite, chalcopyrite, sphalerite and galena and these veinlets also crosscut the microshears. Locally the schist is folded and zones of brecciation, silicification and vein deposition overprint the rock. Vein quartz and albite predominate and arsenopyrite and gold infill breccia matrix and crosscutting veinlets. Sulphide deposition began in the later stages of metamorphism with pyrite deposited in quartz-albite segregations. Subsequent shearing caused brecciation of some grains and accompanied deposition of arsenopyrite ¦ gold and rare sulphides along foliation-parallel microshears. Minor amounts of chalcopyrite, sphalerite and galena were then remobilised in ankerite veins that crosscut the shears. In areas of high strain, arsenopyrite was then deposited as euhedral grains in veins and breccias. Synmineralisation deformation caused the brecciation of some grains and gold was deposited infilling fractures in the arsenopyrite. The paragenetic sequence shows gold mineralisation occurred in two distinct sets of structures (semiductile and brittle) that formed at different times in the formation of the shear zone.

Jan 1, 2006

By Norman A. Jull

"Factors which affect the separation achieved in a hydrocyclone are discussed and illustrated with graphs of some mathematical relationships.Definitions of separation and sharpness include comment on use of elutriation devices.A plea is made for better evaluation of field data prior to their reporting or use in calculations. Methods of evaluation are suggested, with samples of the relevant calculations.An example of the effect of percent solids errors is given, with computer printout and plotted corrected recoveries.INTRODUCTIONThe range of interest in cyclones runs from a simple demand for classification results to a detailed study of published equations defining cyclone characteristics. Probably this group covers as broad a range and, in an attempt to offer something for everyone, I will begin with general operating comments, then move on to more analytical topics. Ideally, an author would compose his paper after the discussion period, when he would have a better idea of the areas of special interest to his audience.Sor'1e of you may share our incurable fascination with classification, especially as performed in cyclones. It is amazing that such a simple device could be in use for more than 20 years and retain as much mystery as it does. Substantial parts of the mystery have been solved but some remains, to keep up our curiosity. There is at least one valid reason: the unusual compactness of this device, which makes internal observation very difficult. What other unit can you think of which performs such a complex separation between particle sizes, shapes and specific gravities at such high capacity? Retention time in a cyclone is typically 3 seconds!Mutual Agreement - In a cyclone, every parameter of geometry and of operation interacts with every other. In an orderly discussion of individual parameters it would be necessary to repeat, in every section, 11 if all other factors are equal"". Could we agree now, for our mutual convenience, that that phrase is clearly understood between us during the remainder of this paper?"

Jan 1, 1972

By T. Phiri, Antoine Floribert Mulaba-Bafubiandi

Microwave energy has been recently used in minerals processing to speed up the leaching process or to improve the liberation of targeted minerals (Al-Harahshed and Kingman, (2003); Bradshaw et al., (2001)). Applied to the roasting of sulphide minerals, microwaves allow the ?tunning? of calcine types and products quality in addition to the energy savings as opposed to the conventional roasting (Mulaba, 2006). As more than 85% of world zinc is produced through the ?roast-leach-electrowin? route, an attempt was made to optimize cost, energy and product quality for metal extraction process route. The use of microwaves was the alternative process route selected for the optimisation. Pyrite concentrate (0.17% Zn, 0.09% Cu, 35.71% Fe, 43.76% S) and sphalerite concentrate containing 43.81% Zn, 0.37% Cu, 3.86% Fe and 44.39% S were microwave roasted in a multimode cavity of 2.45 GHz with varying power levels and for different durations. The produced calcines were characterized using AAS, XRF, XRD and Mossbauer spectroscopy while the determination of residual Sulphur was used as products quality control tool to ascertain the degree of roasting achieved on the feed. The leachability of the produced calcines in HCl, HNO3, H2SO4 and HNO3 + HCl has been studied in terms of the best leaching yield, process kinetics economics and environmental aspect. With 800 W power for 30 minutes, ZnO and Fe2O3 were formed corresponding to a 70% sulfur removed from sphalerite and 80% from pyrite concentrates respectively. While the roasting of the above concentrates appeared to be a first degree processes, it was noticed that the microwave assisted roasting of sphalerite and pyrite concentrates yielded lower sample surface temperature for a shorter time (i.e.less than 30 minutes) microwave exposition. Longer time (more than 30 minutes) microwave exposure showed a linear increase in temperature in function of power level used. While optimum roasting conditions were found at 800W, 30 minutes, a 10% increase of sulfur removal was noticed while pyrite concentrate was microwave roasted. Sulfuric acid was seen to give higher leaching yield than nitric acid. Zinc dissolution was hindered by the presence of franklinite.

Jan 1, 2007

By Wolfgang Gütter

India is targeting to boost its electrical capacity from 100 GW to 200 GW within the next 10 years. The National Hydroelectric Power Corporation (NHPC) has decided in2001 to take execution of the 800 MW Stage-II of the prestigious 2,051 MW Parbatihydrol electric project in Kulu district of the northern province Himachal Pradesh. Two parallel 30° inclined underground pressure shafts of 1.542m in length each will be excavated in different geological formations and lined with hexagonal concrete segments by a hard rock double shield TBM. That kind of heading will be a novelty to India and an innovative method for inclined pressure shafts. The 4.88m Mitsubishi DSTBM will be assembled underground on a swivelling steel platform especially designed for the launching as well as for the acceptance of the TBM in the upper cavern of each shaft. The hexagonal segmental lining system causes a significant higher job safety than an open TBM with conventional support. Each ring consists of four honeycomb segments with 20 cm thickness. After finalisation of the excavation a steel liner will be installed and concreted. The Joint Venture Jäger-Seli will perform the two pressure shafts as a sub-contractor for the Indian company Gammon India Ltd.

Jan 1, 2005

By M Kozikowski

The primary purpose of these investigations is to determine dewatering requirements and likely impacts associated with mining operations. Standard aquifer testing techniques were carried out at multiple locations within the Ord Range near Pardoo, Western Australia. Aquifer properties of an oxidised haematite orebody were calculated from test pumping data conducted in five fully penetrating test bores. Hydraulic properties of the Ridley magnetite orebody were calculated based on short term constant rate pumping tests, and packer tests. Packer tests were conducted in undeveloped and uncased exploration holes and diamond core holes. The new data sheds light on the hydrogeological properties of this previously unexplored region of Western Australia.Aquifer testing procedures for each bore included a preliminary step test followed by a constant rate test. Recovery data were collected in each bore over a period of four to six hours. Prior to testing, background water levels and water samples were collected in a network of monitoring and exploration bores to establish baseline water levels, gradients and water quality. Water quality within the bedrock of the Ord Range varies from 2000 to 5500 mg/L TDS whereas water quality within the alluvial sequence of the De Grey River is highly variable (400 to 2500 mg/L TDS), but is predominantly brackish with some water of potable quality which is used to supply Port Hedland. Test pumping supports the conceptual hydrogeological model that consists of a pod like orebody (aquifer) surrounded by low permeability waste rock (BIF), with very weak hydraulic connection to the adjacent alluvial systems. Calculated hydraulic conductivity from test pumping data across Pardoo ranged from 0.01 to 59 m/d, depending on deposit tested.A groundwater model was used to simulate dewatering required in proposed pits and to estimate the impact of dewatering on the surrounding shallow alluvial aquifers. Test pumping and numerical groundwater flow modelling indicate the proposed below water table pits can be successfully dewatered utilising in pit dewatering production bores. Yields from individual dewatering bores will reduce with time due to the reduction in saturated aquifer thickness.Based on the numerical groundwater modelling and field investigations the likely impacts to the adjacent De Grey River alluvial aquifer system (within the Priority 1 De Grey River Water Reserve) resulting from mining and dewatering activities is considered minimal. Recalibration of the groundwater model will be undertaken once several months of dewatering data are available.The aim of this paper is to present a range of aquifer parameters derived through standard aquifer testing techniques for an area previously unexplored in terms of hydrogeological characteristics. It is the goal of the authors to provide this comparison data set for future work in similar geologic media.

Jan 1, 2009

By Ezequiel Ordonez

MOST spectacular of Nature's contributions to the making of the postwar world is the Paricutin volcano, in Mexico, which I described in the July issue of this magazine last year, a few months after it was born. Now, after more than a year of continuous eruption, it is still and perhaps will remain a comparatively small though no less interesting volcano. The cone on April 1 had an altitude of nearly 1200 ft. above the level of the small flat field from which it began to grow on Feb. 20, 1943. This cone is now almost entirely surrounded by the lava flows that poured out at different dates, from its base or from outlets on the slopes near its base. To the north and northwest these lavas were

Jan 1, 1944

The purpose of this paper is to describe briefly the clean-up procedure adopted at the treatment plant of Paringa Mining & Exploration Co. Ltd. at Kalgoorlie, Western Australia.A clean-up is carried out at the end of each four-weekly period, and all figures subsequently quoted are taken from a summary of the results of the eight periods ending 8th April, 1941.STRAKING AND AMALGAMATIONOf the total gold won 22· 77 per cent. is recovered by straking and amalgamation.The discharges of both the primary and secondary ball mills are pumped over a common set of five ten feet long by three feet wide straking tables, set at an angle of 10 degrees, before passing to the 14 ft. diameter by 30 ft. by 8 ft. Dorr bowl classifier.This classifier is in closed circuit with both of the ball mills, hence the whole of the circulating load of the fine grinding circuit, which approximates to 800 per cent., is required to pass over the straking tables. For convenience in handling, corduroy cloths are used in lengths of 5 feet, and are picked up and replaced by clean cloths at four-hourly intervals. The avaHable straking area provided is, therefore, 900 square feet, or approximately 3·30 square feet per original ton per 24 hours. The density of the pulp passing over the tables is about 54 per cent. solids, the area provided per ton of pulp per 24 hours being approximately o· 2() square feet. Washing of the corduroy cloths is carried out on the day shift only, about 800 lb. of strake concentrate being obtained daily.This concentrate is sluiced from the washing trough on the elevated straking floor to the 4 ft. by 2 ft. diameter amalgamating barrel located in the gold room below.The barrel is of standard design and is rotated at 25 r.p.m. It is charged each day at 4 p.m., and grinding of the strake concentrate at approximately 70 per cent. solids is continued until 8 a.m. the following day. The barrel is then stopped, and the contents generously diluted with water, and after a few minutes rotation some of the slime is carefully poured off through the small discharge hole. This dilution and decantation is repeated until a good deal of the valueless slime has been removed.A further quantity of strake concentrate is then charged to the barrel, which is allowed a further 16 hours grinding period. After again diluting and decanting, approximately 25 lb. of mercury and 15 lb. of lime are added to the charge, which is then given an amalgamation period of 2 hours before cleaning up.By the process of grinding, diluting and removal of slime by decanting...

Jan 1, 1941

By Maurice E. Peloubet

This discussion of accounting will describe the statements and the information that the accounting system produces, from the point of view of those who use such systems rather than of those who prepare them and who do the detail and technical accounting work. In any well organized mine, quarry, or other enterprise exploiting a mineral deposit, no matter how small, some clerical and accounting work must be done. Miners and other employes must be paid, supplies must be purchased and issued, and various tax and information returns, which even the smallest enterprise must file, have to be prepared. In this chapter it is assumed that the enterprise has employes of this type and that they understand the fundamentals of record keeping and accounting. It would be impossible here to give sufficiently full explanations to enable a man with no previous clerical and accounting training to set up and operate an accounting and cost system for even the simplest extractive operation. Rather, we shall hope first, to tell the investor and the operator, from the chief engineer or president down to a subforeman, what to expect from the accounting statements and records and how to use this information in his daily work; and second, that it will enable the man with some knowledge of accounting or book- keeping, but with little or no experience in any extractive industry, to set up and operate a satisfactory system for a mine or other extractive enterprise. For readers who wish to go further, the bibliography at the end of this chapter contains many references. T he emphasis has, therefore, been placed on the statements to be produced and the purposes for which they are to be used rather than the underlying books and records. These are, with a few exceptions which will be described later, essentially what might be found in any industrial enterprise and would probably, in the extremely small enterprise, consist of handwritten journals, ledgers, analysis books, payroll books, and stores ledgers. In the larger enterprise, various types of mechanical accounting would be introduced in proportion to the complexity of the operation.

Jan 1, 1964

By S. D. Strauss

The marketing of nonferrous metals and of the ores and concentrates from which these metals are recovered is a fascinating trade, international in character, sensitive to every change in the economic tide, and complex in its organization. Each individual metal has its own marketing mechanism; no two are exactly alike. The differences sometimes are a matter of tradition rather than of necessity, but usually they have developed because of the very nature of the problems of producing or consuming the individual metal. This description, because of limitations of space, can do no more than indicate the major aspects of the trade and touch lightly on the marketing structure of each metal. The dictionary states that a market is a "meeting of people for selling and buying." In the case of nonferrous metals this meeting may occur on a half-dozen different occasions between the time the ore has been first mined and the time the refined metal is available for use by industry; or it may not occur at all until after the metal itself has been rolled, drawn, stamped, cast, or forged into a useful semifabricated shape. To illustrate: A Chilean miner may sell his small ore production to a custom mill, which produces concentrates that are sold to an ore dealer, who finances the shipments of the concentrates to a United States custom smelter, which buys these' concentrates for conversion into blister, which is subsequently refined into electrolytic copper and sold. Conversely, much of the production of aluminum is in the hands of integrated concerns that mine bauxite, convert bauxite to alumina, smelt the alumina to produce aluminum, and then fabricate the aluminum into semifinished or even finished products before title to the material changes hands for the first time. Some nonferrous ores are not converted into metal at all but are sold by the miners or dealers directly b the ultimate consumers. A good example would be chrome ores used by the chemical industry. And of course a substantial part of the commerce in nonferrous metals is in scrap, which is the reconversion into useful form of metals that have long since been mined and smelted. Thus, one-third of all the lead used in the United

Jan 1, 1959

By S. D. Strauss

The marketing of nonferrous metals and of the ores and concentrates from which these metals are recovered is a fascinating trade, international in character, sensitive to every change in the economic tide, and complex in its organization. Each individual metal has its own marketing mechanism; no two are exactly alike. The differences sometimes are a matter of tradition rather than of necessity, but usually they have developed because of the very nature of the problems of producing or consuming the individual metal. This description, because of limitations of space, can do no more than indicate the major aspects of the trade and touch lightly on the marketing structure of each metal. The dictionary states that a market is a "meeting of people for selling and buying." In the case of nonferrous metals this meeting may occur on a half-dozen different occasions between the time the ore has been first mined and the time the refined metal is available for use by industry; or it may not occur at all until after the metal itself has been rolled, drawn, stamped, cast, or forged into a useful semifabricated shape. To illustrate: A Chilean miner may sell his small ore production to a custom mill, which produces concentrates that are sold to an ore dealer, who finances shipments of the concentrate to a custom smelter, which buys them for conversion into blister, to be subsequently refined into electrolytic copper (sometimes by a refinery having no corporate ties with the custom smelter) and sold. Conversely, aluminum production is mostly by integrated concerns that mine bauxite, convert it to alumina, smelt that to produce aluminum, and then fabricate that into semifinished or even finished products before title to the material changes hands for the first time. Some nonferrous ores are not converted into metal at all but are sold by the miners or dealers directly to the ultimate consumers. A good example would be chrome ores used by the chemical industry. And of course a substantial part of the commerce in nonferrous metals is in scrap, which is the reconversion into useful form of metals that have long since been mined and smelted. Thus, one-third of all the lead used in the United

Jan 1, 1964

By Carroll C. Bailey, William F. Boericke

Mine financing, or providing adequate capital for developing and bringing a mining property into production, is an essential requirement for a successful operation. Today it presents a different picture than even twenty-five years ago. The day appears to be gone when a mining property could pay its own way from grass roots to production. The country has been quite thoroughly combed for surface showings from which sufficient initial profit could be immediately garnered to pay for further development and production facilities. The four M's for success in mining-mineral, market, management, and money-are still essential; but doubled or tripled wage costs and steep advances in cost of equipment and supplies throw increased emphasis on adequate capital funds for bringing in a prospect and making it a producer. Consequently, the old picturesque, although seldom rewarding, grub- staking procedure where a single venturesome citizen might advance funds to a prospector on a fifty-fifty basis for whatever discovery he might find, has largely disappeared. Its place, to some degree, has been taken by the small syndicate of venturesome members who band together for furnishing funds to a group of prospectors for the same general purposes. Such a syndicate has a definite organization and is usually assured of sufficient initial funds, or flow of funds, to carry on work for several years. It is headed by an engineer-promoter who has had considerable field experience as well as personal knowledge of his prospecting crews. For the owner of a potential mining property who has ample capital, the problem is to determine (1) justification for the necessary investment in exploration and development, and (2) the economics of the enterprise as to size and degree of integration of the final operating entity. If the owner of such a property has little or no capital, he also faces these same basic problems but, in addition, must be able to present the findings of fact and persuade the prospective investor that the enterprise will produce

Jan 1, 1959

Application of Gy?s formula is appropriate for calculation of the Fundamental Error (FE) prior to samples being collected at any stage of the minerals process, provided that sampling parameters K and a (alpha) have been determined by calibration of the ores. Two types of calibration procedure are well established in the industry, the Hetrogeneity test and the 32-piece sampling tree experiment. The sampling tree experiment uses the variance and average grade of metal analyses from four series of samples at different nominal fragment size, as the basic input data. Pierre Gy suggested the cube as an appropriate exponent of the nominal fragment size for use in his equation. More recent work suggests that this exponent is variable and characteristic of specific ores and therefore requires calibration. The method described here explains the experimental procedure of the calibration. It is then possible to calculate a sampling nomogram using the sampling parameters K and a. This allows the sampler to determine a suitable protocol for the sampling event that will ensure that the FE does not exceed a predetermined precision at any point in the sampling procedure.

Jan 1, 2007

By John H. Weigand, Stephen V. Crum

"VIBRONICS, INC. instrumented and monitored a residential structure for response to,blasting at aMidwestern surface coal operation. The residence was owned by the mining company and was extremely close to the operation. Blasting was conducted within 120 feet (36.5 meters) of the test structure. Up to seventeen (17), four (4)-channel seismographs were used during the monitoring period. The basement walls and floor were monitored. VIBRONICS, INC. also monitored a brick chimney in the basement and attic. Structural responses were then compared to outside vibration measurements taken in the soil near the foundation."

Jan 1, 1998

By J. C. Bokros, A. S. Schwartz

The irradiation-induced densification of pyrolytic carbon has been shown to take place by a simple first-order rate process. The values of the densification constant, kd, for isotropic carbons are 1.0 x 10-22, 1.4 X 10-22 and 2.8 X 10-22 (nut)-1 at irradiation temperatures of 520o, 670°, and 1000oC, respectively. The apparent activation energy obtained from the temperature dependence of kd for isotropic carbons is about 0.2 ev. Estimates of the maximum stresses that develop in isotropic carbons owing to shrinkage onto an unyielding support show that stresses in excess of 15,000 psi may be avoided during irradiatian at 600" and 1000°C if the initial coating density is kept above 1.5 and 1.9 g per cu cw, respectively. If a carbon coating on an unyielding support is not completely isotropic, stresses may continue to build up at high neutron exposures after densification is complete because of continued anisotropic distortion. Stresses in excess of 15,000 psi from this source may be avoided during irradiation at 1000°C if' the Bacon anisotropy factor is kept below 1.3. A variety of applications of carbon and graphite in nuclear technology has stimulated numerous studies of the effect of neutron irradiation on these materials One of the most interesting problems associated with the use of carbons and graphites in the high fast neutron fluxes of nuclear reactors arises as a consequence of the neutron-induced dimensional changes that occur during irradiation. Energetic neutrons displace car- bon atoms from their lattice positions; and, depending on the temperature, the interstitials and vacancies produced migrate to form clusters, recombine, or are annihilated at dislocations or crystallite boundaries. The competition of various sinks for the point defects results in structure-sensitive bulk-dimensional changes that vary with temperature in a complicated way. This paper deals with the neutron-induced dimensional changes in turbostratic carbons that are being used as coatings on nuclear fuel particles. Details of the structure of these carbons and the variations of their structure with deposition conditions have been reported.'-3 It has been shown in previous work that the neutron-

Jan 1, 1968

Jan 1, 1968

By Jameel Menashi

A process has been developed for recovering the refractory metal values contained in mixed secondary source materials such as contaminated grinding wastes, oxides and sludges. The wastes are calcined with sodium carbonate in air to convert the refractory metals to water soluble Na2CrO4, Na3V04, Na2Mo04 and Na2W04. The base metals, Fe, Ni, Co and Cu, are converted to water insoluble oxides. An aqueous leach of the calcine effectively separates the refractory metals from the insoluble base metals. Co, Ni and Cu can be recovered from the oxidic residue by conventional processing methods. The leach solution is purified and then treated to recover the refractory metals as Cr203, NH4VO3, (NH4)6Mo7024?4H2O and H2WO4. The purity of the products is sufficient for their use in many metallurgical applications. The Na+ values in the leach solution are recovered as Na2CO3(or NaHC03) and are recycled to the calcination step. It is shown that the process can accommodate a wide range of feed compositions and generates a minimum of aqueous effluents.

Jan 1, 1984

By F. Haessner, M. Wilkens, U. Jakubowski

ThOUGH at present there is a wide range of possibilities for the quantitative determination of preferred orientations, pole figures of identical specimen material have not been determined by different methods as yet.''' In this paper a comparison of (Ill), (200), and (220) pole figures is presented which were obtained from a 95 pct cold-rolled high-purity cop- per sheet (99.9998 pct Cu), by three different methods. The three methods are: a) The combined X-ray reflection-transmission technique of plane samples by schulz3 and Decker, Asp, and Harker. 4 A Siemens texture goniometer was used. The experimental details are described elsewhere. 6 b) The X-ray reflection technique of spherical samples by Jetter and Boric.' A Siemens texture goniometer with some modifications was used. The samples were prepared by sticking 140 polished sheets together with an adhesive and machining a sphere (20 mm diam).* Additional

Jan 1, 1967

By J. F. Breedis

The stabilization of austenite in Fe-Ni alloys against martensitic transformation after reversion has been attributed' to the lattice imperfections remaining from previous transformation. More recently, however, such stabilization has been associatedzy3 with compositional changes which occur in martensite during slow heating. Dislocation arrangements in deformed austenitic stainless steels strongly influence transformation to martensite on quenching.4 Therefore, it is of interest to observe the transformation behavior of stainless steel after reversion, especially since previous studies have been confined to Fe-Ni alloys. The transformation-product morphology also differs in the two iron-alloy systems;6 plate martensite forms in the latter while stainless steel transforms to lath-type martensite. Samples of Fe-16 wt pct Cr-12 wt pct Ni (maximum C + N = 0.005 wt pct, 0 = 0.02 wt pct), prepared by vacuum melting and casting from high-purity components, were annealed at 900°C for 24 hr, after cold rolling to produce a 40-p grain diameter. The M, temperature of this alloy is -80°C and samples are fully austenitic after annealing. The amount of martensite present after quenching, annealing, and requenching was determined magnetically, to within 0.01 wt pct, using a vibrating specimen magnetometer. Nearly 14 pct of martensite forms during the initial quench in 1 min at -196°C. Two-min and 2-hr anneals were done in air and in evacuated quartz capsules, respectively. All specimens were electro-polished before making the magnetic measurements.

Jan 1, 1967

Jan 1, 1967

By R. G. Vardiman, M. R. Achter

Observations of dislocation structure in niobium are presented using two techniques. Triangular pits developed by electroetching are confined to orientations in the stereographic triangle between the (111) pole and planes of the (1ll) zone and require the presence of carbon. Some unusual electroetching phenomena at other orientations are noted. A chemical etch of dislocations decorated by the addition of carbon to 50 ppm reveals the complete dislocation line structure in a surface layer up to 30 p deep, with a resolution of less than 1 p. This effect is independent of surface orientation. The structure of subboundary nets may be resolved for misorientations up to about 1'. Dislocation structures found in strain anneal grown crystals, such as helices, prismatic loops, and high-density areas, are observed. The measurement of dislocation density is discussed and values obtained in different ways are compared. IN the course of some work on the response of refractory metals to thermal-mechanical treatments, it was desired to examine the defect structure of relatively low dislocation density crystals of niobium in bulk form. Surface and bulk methods for the observation of dislocations have been reviewed by ~melinckx,' and include etch pitting, decoration, and various X-ray techniques. The dislocation line structure has been developed by decoration in a few metals, although observations were limited to certain orientations, or by the coarseness and nonselectivity of the precipitate. The most commonly used technique is etch pitting. In niobium, etch pits have been developed chemically'0," in material of high impurity content and electrolyti-cally'' in relatively pure material. In this paper, etch pits developed electrolytically, and the dislocation line structure of a surface layer developed by decoration and chemical etching, are examined, and observations are presented from both techniques. EXPERIMENTAL METHODS Our starting material was electron-beam-melted niobium, swaged to 4 or -in.-diam rod. Chemical analysis is given in Table I. Single crystals were grown by a strain anneal technique using 1 to 2.5 pct of strain and growth temperatures of 1700" to 2300"~.'~ Some crystals grown by zone melting were also examined. The desired surface orientation was exposed either by spark machining or by sectioning with a cut-off wheel and prepared for etching by electro-polishing.

Jan 1, 1969