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By A. E. Back

[Several processes for recovering manganese from low-grade ores have been proposed3/4/5/ in which an aqueous slurry of the ore is leached with gas containing nitrogen, oxygen, and sulfur dioxide as obtained from burning sulfur or roasting sulfide ores. The manganese dioxide is dissolved, and most of the sulfur dioxide is oxidized to sulfate, but an appreciable quantity of dithionate is usually formed, together with acid from oxidation of the sulfur dioxide. The over-all reactions may be represented as follows: (1) Mn02 + S02 = Mn++ + S04--. (2) Mn02 + 2S02 = Mn++ +S206--. (3) H20 + So2 + 1/2 02 = 2H+ 5S4--. (4) H20 + 2S02 + 1/2 02 = 2H+ + S206---.]

Jan 1, 1952

By D J. Kilkenny, D A. O’Toole, P B. Hills, K L. Seah

An investigation was undertaken to critically analyse the use of fibre reinforced shotcrete (FRS) for a variety of applications in large diameter shafts. Those applications included the use of FRS with or without the addition of subsequent rock bolting in the temporary support cycle prior to the installation of a permanent lining, most likely cast in situ concrete or as the final lining medium.Numerous authors have considered the early re-entry and strength characteristics of FRS in recent years. The current study has investigated the practical application of the recommendations of many leading authors in an endeavour to establish practical and acceptable risk-assessed procedures for the use of FRS for rapid, safe, efficient and cost-effective shaft sinking.Shaft sinking is regarded as a specialist and potentially higher risk activity due to the confined work environment, exposure to ground conditions and a high degree of manual handling associated with getting materials to the sinking face. The use of robotically applied FRS as a primary lining in shaft sinking has significant safety advantages in reducing manual handing associated with mesh safety support and bolting, as well as reducing direct exposure to ground conditions.The study involved both field testing and a literature review. The study established an initial set of criteria for the use of FRS in the development of large diameter shafts and demonstrated a number of scenarios where the technique of robotically applied FRS provided significant safety and cycle time advantages. The opportunity for a fully sprayed single pass lining was also investigated as part of the project.CITATION:Hills, P B, O’Toole, D A, Kilkenny, D J and Seah, K L, 2014. Exploring the use of fibre reinforced shotcrete in large diameter shafts, in Proceedings AusRock 2014: Third Australasian Ground Control in Mining Conference , pp 295–306 (The Australasian Institute of Mining and Metallurgy: Melbourne).

Nov 5, 2014

By S. H. Ash

The paramount responsibility of Government is to protect the general welfare. One of the chief functions of the Bureau of Mines is to investigate and publicize methods of increasing safety and efficiency in mining operations. In an industrial civilization, energy resources constitute the foundation of a sound economic structure (14).4/ Coal is only one source of energy, but it provides more than half the energy consumed in the United States.

Jan 1, 1946

By Dongwook Kim

Recently, load and resistance factor design (LRFD) is gradually being adopted internationally in geotechnical design due to the advantages of LRFD over the existing allowable stress design (ASD). LRFD is a more advanced design method compared to the ASD because resistance factor is calibrated based on the reliability analysis for a given target reliability index. Target reliability index changes with the importance of the structure. Typically, target reliability index of offshore foundation is less than those of onshore. The widely-used Imperial College Pile (ICP) design method is used for the calculation of pullout capacity of driven piles. The uncertainties regarding pullout capacities of driven piles are assessed using the statistical data reported in the literature. The first-order reliability method (FORM) is used to calibrate resistance factors for the pullout ultimate limit states of the driven piles for three different levels (2.5, 3.0, and 3.5) of target reliability index. The load factors used in this paper are the ones proposed in the AASHTO LRFD bridge design specifications.

Jan 1, 2010

By C.P. Clingerman

The recent iastallation of a combination dust catcher, gas washer and precipitator at Carrie blast furnaces of the Homestead Steel Works has given very satisfactory results. The following description of the gas-cleaning installation is based on actual operating experience. When Carrie blast furnace No. 3 was rebuilt the decision was made to fine-clean all the gas produced by the furnace, because the management wanted fine-cleaned gas for fuel in the stoves and boilers. In order to keep the installation cost as low as possible, the gas-cleaning system was streamlined. All by-pass lines and goggle valves for bypass lines were eliminated from the system. A radical departure from the use of 8-in. tubes in the Cottrell-type precipitators was made by using 12-in. diameter tubes in a single compartment, the single compartment being divided into two units by a single partition wall in the top header. The Furnace Proper A few of the characteristic points and dimensions of the furnace proper are: Hearth diameter.............. 26 ft. o in. Bosh diameter............... 29 ft. 1 3/4 in. Stock-line diameter........... 20 ft. o in. Large-bell diameter........... 14 ft. 8 in. Small-bell diameter........... 6 ft. 6 in. Height of furnace from center of iron notch to bottom of large bell, closed............ 94 ft. 4 in. Height of furnace from center of iron notch to main platform ...................... 105 ft. o in. The furnace top is equipped with a MC-Kee revolving distributor, the operation of which is electrically interlocked with the skips, bell hoists, and coke-weighing and charging apparatus through a Freyn automatic charging control. The gas leaves the furnace first through four offtakes, 5 ft. 9 in. in diameter, then through uptakes that, are approximately 85 ft. high, which feed into a single down-comer that is 9 ft. in diameter. Dust Catcher The primary dust catcher installed (Fig. I) may be described as a single-cone type. The inlet pipe at the top of the dust catchei is 9 ft. in diameter; it is flared to a conical shape as it extends down inside the dust-catcher shell, which is 35 ft. in diameter, 37 ft. high on the straight side, and has a conical top and bottom. The slope of the bottom is so0 with the horizontal. The cone-shaped pipe inside the dust-catcher shell is 42 ft. high and is 19 ft. 7 in. in diameter at its bottom lip where it releases the gas inside the dust catcher. The ratio of the area of the inside cone at its bottom lip to the

Jan 1, 1943

By C. P. Clingerman

The recent iastallation of a combination dust catcher, gas washer and precipitator at Carrie blast furnaces of the Homestead Steel Works has given very satisfactory results. The following description of the gas-cleaning installation is based on actual operating experience. When Carrie blast furnace No. 3 was rebuilt the decision was made to fine-clean all the gas produced by the furnace, because the management wanted fine-cleaned gas for fuel in the stoves and boilers. In order to keep the installation cost as low as possible, the gas-cleaning system was streamlined. All by-pass lines and goggle valves for bypass lines were eliminated from the system. A radical departure from the use of 8-in. tubes in the Cottrell-type precipitators was made by using 12-in. diameter tubes in a single compartment, the single compartment being divided into two units by a single partition wall in the top header. The Furnace Proper A few of the characteristic points and dimensions of the furnace proper are: Hearth diameter.............. 26 ft. o in. Bosh diameter............... 29 ft. 1 3/4 in. Stock-line diameter........... 20 ft. o in. Large-bell diameter........... 14 ft. 8 in. Small-bell diameter........... 6 ft. 6 in. Height of furnace from center of iron notch to bottom of large bell, closed............ 94 ft. 4 in. Height of furnace from center of iron notch to main platform ...................... 105 ft. o in. The furnace top is equipped with a MC-Kee revolving distributor, the operation of which is electrically interlocked with the skips, bell hoists, and coke-weighing and charging apparatus through a Freyn automatic charging control. The gas leaves the furnace first through four offtakes, 5 ft. 9 in. in diameter, then through uptakes that, are approximately 85 ft. high, which feed into a single down-comer that is 9 ft. in diameter. Dust Catcher The primary dust catcher installed (Fig. I) may be described as a single-cone type. The inlet pipe at the top of the dust catchei is 9 ft. in diameter; it is flared to a conical shape as it extends down inside the dust-catcher shell, which is 35 ft. in diameter, 37 ft. high on the straight side, and has a conical top and bottom. The slope of the bottom is so0 with the horizontal. The cone-shaped pipe inside the dust-catcher shell is 42 ft. high and is 19 ft. 7 in. in diameter at its bottom lip where it releases the gas inside the dust catcher. The ratio of the area of the inside cone at its bottom lip to the

Jan 1, 1943

By T. S. Blair

I feel a certain sense of responsibility in bringing before you the subject of the direct process in iron manufacture. I am aware that, in such a body as I have now the honor of addressing, there are few who are not already so well informed upon its past history that it would be a weariness to them to listen to anything else than an account of practical success. Yet, to claim that success involves so much that, if I do not make good my claim, I deservedly expose myself to severe criticism. The whole literature of the art, so far as it relates to the direct process, is, up to this time, but a history of failure. It is safe to say that more money, time, and talent have been fruitlessly spent in the pursuit of this object than in all the other unsuccessful efforts in the whole line of iron metallurgy. A distinguished authority in patent law has remarked that " the invention records of the United States and of foreign countries are filled with the waifs and abandoned relics of these abortive struggles." Dr. Percy, whose great work may be taken as an epitome of all that was worth mention, whether useful or curious, in pig-iron metallurgy, up to the date of its publication (1864), after giving elaborate accounts of various attempts at the direct process, condenses his own opinion of all that had been then effected, into a brief but summary comment upon a pamphlet of one of the sanguine inventors who had said: "It is evident that the present mode of working iron

By Steven D. Botts

The Antamina project, owned by BHP Billiton Plc, Mitsubishi Corporation, Noranda Inc., and Teck Cominco Ltd. , is a $2.3 billion copper/zinc project, located in the Ancash Department in Perú. The project consists of an open pit mine, a 70,000 ton per day concentrator, a 302 Km. long concentrate pipeline, port facilities, a new access road, power line, and town site. The project is designed to produce up to 1.5 million tonnes per year of copper and zinc concentrates over a 23-year project life, and will be the third largest producer of zinc and the seventh largest producer of copper in the world. This mega project is the largest mining investment in the country and, during its construction stage, was the most important construction project worldwide. On May 28th, 2001, Antamina commenced testing operations and four months later, it reached commercial production. Antamina was officially inaugurated on November 14th, 2001 by Peruvian president Alejandro Toledo. The construction stage of the project generated 8,000 direct jobs, with a peak of 10,000 employees, and 30,000 indirect jobs. The permanent workforce consists of approximately 1650 employees, the vast majority of which are Peruvian Nationals; around 30% of whom came from the department of Ancash where the deposit is located. Approximately 5,800 indirect jobs will be generated from the project. Independent sources state that Antamina will increase the Peruvian mining exports by 30% and Peruvian GDP by 1.4% within its first year of full operation in 2002. Since winning the privatization bid for the project in 1996, the company has implemented a successful approach to community development and environmental protection based on sustainable development principals. Throughout the development of the project, a number of initiatives have been undertaken to ensure full involvement of the local populations in community development activities and the company?s environmental program. Due to its size, difficult logistics, cultural considerations and financial aspects, the project has faced a number of unique challenges in the area of environmental protection and management of community interaction. Antamina has been innovative in its approach to these issues, and as a result, has set new standards in Perú for environmental and community management, and sustainable development.

May 1, 2002

"The JKMRC researchers have been redeveloping the suite of breakage testing techniques to more realistically align with the breakage environment in comminution equipment. Computational modelling, especially with the DEM, has highlighted the modes of impact and contact, along with the energies of these interactions in a wide range of equipment. This has driven the need to match these modes in laboratory ore characterisation tests. The objective has been to build a continuum of breakage tests and associated models that span the required range of breakage forces and environments. The ore sample is subjected to a sequence of tests covering: abrasion (surface breakage) of angular through to smoothed particles; single particle impact from high energy single impact breakage down to low energy; incremental breakage covering 60 mm down to 50 µm particles; particle strength distribution; and bed breakage over a range of compression and energy input. These tests are suited to multi-component ores with a distribution of strengths. A modelling technique is also being developed to utilise primary breakage for modelling breakage under different types of confinement. This paper draws together these techniques, previously published by the authors, into a coherent whole. The suite of tests is approaching the point where a fixed set of tests can be used to model the performance of a full range of equipment, removing the need to conduct repeat ore characterisation tests for each different piece of equipment incorporated in a circuit design. This path should open up the application of different circuit configurations and novel equipment in comminution circuit design.1 INTRODUCTION Comminution modelling utilizes a wide range of ore characterisation techniques and methods to deal with the range of comminution equipment available for production use. In general, the tests have been designed to correlate with specific pieces of equipment, using calibration factors to provide the link between the small-scale test and industrial-scale performance. The majority of tests focus on estimating the power requirement of process equipment to achieve a desired throughput and grind size. Overall, this approach has achieved acceptable outcomes in the past, but the reality is that equipment sizing suffers from considerable uncertainty, in excess of ±20% is not uncommon. This uncertainty is covered by safety margins and automatic scaling factors in equipment selection. In striving to improve reliability, the industry tends to add more adjustment factors to the tests, and design margin rather than question the basic validity of the testing process. As the tests are often correlated to production equipment via carefully guarded databases, they are also locked into historic operating inefficiency, not providing direction or revealing opportunities to improve production efficiency in comminution equipment or circuits. Safe in the knowledge that they are achieving the expected production based on test work predictions, a site is unlikely to set their sights on reducing specific energy consumption by 10%."

Jan 1, 2018

By William K. Cunningham

The investigation described in this report was begun as part of the Bureau of Mines progress to develop acid processes for the extraction of alumina from low-grade bauxite and. clays. A domestic shortage of high-grade bauxite sui table for treatment by the Bayer process became acute as a result of' World War II; an intensive search for a practical acid process using lower-grade alumina-bearing raw materials was therefore warranted. The laboratory development was described in a preceding Bureau of Mines publication wherein the basic theory for the design and erection of a pilot plant maybe found. A 2-ton-per-day continuous pilot plant was constructed and successfully operated at College Park, Md., which demonstrated conclusively the chemical and mechanical feasibility of a solvent purification process for aluminum sulfate. The estimated production cost of $38.64 indicates that under present market conditions the process would not be economically feasible.

Jan 1, 1948

By G. H. Gronhovd

This report describes the design and initial operation of a slagging gasification pilot plant installed by the Bureau of Mines at the Lignite Research Laboratory, Grand Forks, N. Dak., in 1958-59. The tests covered in this report were conducted over a period of about 2 years, beginning in April 1959. The pilot plant was designed for eventual operation at pressures ranging from 400 to 600 p.s.i.g. (pounds per square inch gage); however, for the preliminary test reported here, the gasifier was fitted with a low-pressure slagging section and operated at atmospheric pressure and at 80 p.s.i.g. The reason for using a low-pressure slagging section for initial operation was to facilitate modifications in design during the development of a reliable slagging procedure.

Jan 1, 1962

By E. J. Gleim

The Bureau of Mines customarily publishes lists of equipment meeting its safety standards to keep the mining industry informed as to the development and availability of mining equipment that can be used safely. The present list supplements Bulletin 543, Permissible Mine Equipment Approved to January 1, 1953, as well as Information Circular 7722, Permissible Mine Equipment Approved During the Calendar Years 1953-54. Because standards have been revised and new ones added by the Bureau, this list contains classes of equipment not previously covered.

Jan 1, 1958

By K. L. Paciorek

The aim of the present study was to determine the thermal oxidative behavior of materials used in coal mines, with emphasis on the type and relative concentration of the products, in particular the toxic species formed. To supplement this work and to gain understanding as to the type of products possibly formed and also to assess the limitations and advantages of the various analytical methods used a literature survey of the past investigations performed on the compositions of direct interest to the subject program was conducted. The compositions thus covered were cellulose, polyvinyl chloride, neoprene, urethanes, polyamides, polyesters, polyethylene, epoxy, phenoxy, urea-formaldehyde and melamine formaldehyde resins. The results of this review are compiled in the Appendix. The experimental work consisted of thermal oxidative degradation of 36 materials and 4 composites using a stagnation burner apparatus developed in these laboratories which affords a dynamic system approximating somewhat the conditions encountered in underground coal mines. This technique as employed during this program gave only the relative product concentration at specific periods of the decomposition process, The advantage of this approach is that in this manner screening of materials can be accomplished in conjunction with some assessment of the decomposition rate as influenced by temperature and material composition. Limited static tests were performed using a sealed tube method. The materials studied were grouped according to their compositions. The following were the main groups: (a) polyvinyl chloride-containing materials, (b) neoprene compositions, (c) rigid foams (urethanes, isocyanates), (d) miscellaneous materials (including jute, fiberglass, polyethylene and some articles of unknown composition), (e) coal and fluids (phosphate esters, organic esters, oil-water emulsions), and finally (J) composites. The latter comprised a mixture of a phosphate ester fluid with (a) coal, (b) a representative polyvinyl chloride sample, and (c) a neoprene type composition.

Jan 1, 1972

"The Ohio River Bridge East End Crossing Tunnel requires a 75-year service life of its cast-in-place reinforced concrete lining. This twin-tube 3-lane (each tube) highway tunnel is about 55-ft wide and 30-ft high. Since unified tunnel service life prediction methodology does not exist in the US, challenges occurred during the design-build phase of this project. These challenges include the methodologies in determining the reinforced concrete’s degradation mode, the lining’s surface chloride concentration level, the reinforcing steel’s critical chloride threshold value for corrosion, how to verify the concrete’s diffusion coefficient, and the durability impact from concrete crack width. This paper presents a methodology in verifying the proposed concrete mix can achieve the service life requirements. This methodology can be adopted for service life prediction for future tunnels to be built in the US. INTRODUCTION The Ohio River Bridge East End Crossing (ORBEE) Tunnel is part of a Public Private Partnership project, which connects transportation network between Louisville, Kentucky and southern Indiana. Located in Louisville, Kentucky, the twin-tube highway tunnel provides northbound and southbound lanes of the Kentucky approach to a new bridge across the Ohio River. Tunnel lengths are approximately 1,675-ft and 1,685 for the northbound tube and the southbound tube, respectively. Connected by two cross-passages, both tubes have a roadway width of 40-ft, for 3-lane traffic, and a vertical clearance of 26.5-ft.The tunnel was constructed by drill and blast method with shotcrete and rock dowels as initial ground supports. The final tunnel lining system includes: •,Nominal 16” cast-in-place reinforced concrete lining, with 2” and 3” concrete covers over reinforcing steel for its extrados and intrados, respectively. •,20” cast-in-place reinforced concrete invert slab, with 4” and 3” concrete covers over reinforcing steel on its top face and bottom face, respectively. •,PVC waterproofing system around tunnel perimeter, excluding invert slab. •,Perforated PVC groundwater collection pipes on both sides of the tubes and one below the invert slab of each tube."

Jan 1, 2016

By C. J. Fleisch, C. P. Clingerman

THE recent installation of a combination dust catcher, gas washer and precipitator at Carrie blast furnaces of the Homestead Steel Works has given very satisfactory results. The following description of the gas-cleaning installation is based on actual operating experience. When Carrie blast furnace No. 3 was rebuilt the decision was made to fine-clean all the gas produced by the furnace, because the management wanted fine-cleaned gas for fuel in the stoves and boilers. In order to keep the installation cost as low as possible, the gas-cleaning system was streamlined. All by-pass lines and goggle valves for bypass lines were eliminated from the system. A radical departure from the use of 8-in. tubes in the Cottrell-type precipitators was made by using 12-in. diameter tubes in a single compartment, the single compartment being divided into two units by a single partition wall in the top header. THE FURNACE PROPER A few of the characteristic points and dimensions of the furnace proper are: [Hearth diameter 26 ft. o in. Bosh diameter 29 ft. 1 3/4 in. Stock-line diameter 20 ft. o in. Large-bell diameter 114 ft. 8 in. Small-bell diameter 6 ft. 6 in. Height of furnace from center of iron notch to bottom of large bell, closed 94 ft. 4 in. Height of furnace from center of iron notch to main platform 105 ft. o in.] The furnace top is equipped with a McKee revolving distributor, the operation of which is electrically interlocked with the skips, bell hoists, and coke-weighing and charging apparatus through a Freyn automatic charging control. The gas leaves the furnace first through four offtakes, 5 ft. g in. in diameter, then through uptakes that are approximately 85 ft. high, which feed into a single down-comer that is 9 ft. in diameter. DUST CATCHER The primary dust catcher installed (Fig. I) may be described as a single-cone type. The inlet pipe at the top of the dust catcher is g ft. in diameter; it is flared to a conical shape as it extends down inside the dust-catcher shell, which is 35 ft. in diameter, 37 ft. high on the straight side, and has a conical top and bottom. The slope of the bottom is 50° with the horizontal. The cone-shaped pipe inside the dust-catcher shell is 42 ft. high and is 19 ft. 7 in. in diameter at its bottom lip where it releases the gas in-

Jan 1, 1943

By R. D. Leitch

The work of the United States Bureau of Mines on stream pollution by coal-mine drainage has included a study of seasonal variations in acidity and volume of several streams in Pennsylvania. The acidity of these streams has been determined during the two or three years prior to 1930 and the results may be considered to represent "normal" low water conditions. The summer of 1330, however, was unusually dry and represents what may be termed "extreme low water conditions on these streams. This report is a comparison of the results obtained for extreme low water of 1930 and for other years. The streams investigated were Buffalo Creek in Somerset County, Indian Creek (lower 5 miles) in Westmoreland County, Little Toby Creek in Elk and Jefferson Counties, Daguscohonda Run in Elk County and West Creek in Elk and Cameron Counties. These will be treated separately in the order given. Most of the descriptive matter and physical data pertinent to the streams and drainage basins are taken from published reports of the Pennsylvania State Water Supply Commission, 1917.

Jan 1, 1931

By Leon Orlowski

THE oil-bearing districts of Poland are found on the slopes of the Carpathian Mountains. The oil belt extends from Gorlice southeast to Stanislawow. It is approximately 250 miles long and 30 miles wide, and comprises four geological districts: the western, or Gorlice district; next, to the east, the Krosno district; the Boryslaw district; and, in the extreme southeast, the Stanislawow district. The amount of petroleum produced in Poland from the beginning of the oil industry scarcely totals 26,000,000 metric tons, or 15 per cent. of the estimated supply. Of this amount, 18,000,000 tons have been taken from the fields of Boryslaw within 25 years; and only about 8,000,000 tons from all other fields within a period twice as long, although some of these other fields represent just as good possibilities as did Boryslaw at the beginning of its development. The Polish oil industry was severely stricken by the war. The retreating Russian armies, in 1915, destroyed a large number, of the existing oil wells, nor was the post-war period favorable for the development of this industry;; the money and credit stringency interfered with the expansion of drilling. But since 1921 there has. been a slow steady increase in production and there is now every reason to believe that conditions in the industry will improve. In fact, an increase in new drillings has been reported for the current year. The production of crude oil in Poland, in 1913, amounted to 1,113,668 metric tons. In 1914, the production declined- to 655,600 metric tons. In 1921, the production was 705,596 tons; in 1922, 712,428 tons, and in 1923, 737,182 tons; or more than 5,000,000 bbl. But the fields have a much greater potential output, which could be realized were the capital available for prospecting and new drilling. The principal producing, and at present most exploited, fields are around Boryslaw and Schodnica. These fields were developed rapidly for in the first year of their modern exploitation the wells were gushers of moderate depth. However, as a result of heavy drilling, the shallow folds have been exhausted and oil can be reached now only by deep drilling. Wells of almost 5600 ft. have been drilled in Boryslaw. Because of these drilling conditions, a large number of engineers and workmen specially skilled in deep drilling are to be found in this field.

Jan 3, 1925

By Paul B. Crawford, Gerald N. Pitts

"A new method is introduced for the simulation by computer of the flow of liquid underground. The method has application in simulating, for example, liquid withdrawal systems, injection systems or injection-well systems. The computer simulation of liquid flow permits the utilization of the known properties of the rock in developing a model of the permeable rock mass.The flow properties of the rock at a specific site arc generated statistically using a random number generator. After defining in this manner the rock properties of each element in the computer grid, the streamlines or flow paths of the liquid are traced using the new method. The simulation is designed especially for computers. The meandering character of the liquids paths is displayed clearly as the fluid moves underground, thus providing the technical information required for the control of the movement of liquid."

Jan 1, 2014

By Gerald M. Bandholz

Exxon Minerals Company, a division of Exxon Corporation, has been exploring for base metal deposits in the Precambrian volcanic rocks in northern Wisconsin since 1970. Aerial electromagnetic surveys of the area, conducted in 1974, reported an anomaly, near Crandon, in Forest County. In the summer of 1975, the first diamond drill entered the anomaly, representing the 25th prospect Exxon had drilled in Wisconsin. This first hole revealed significant mineralization containing zinc and copper. Subsequent drilling confirmed the discovery of a sizeable zinc-copper massive sulfide are body. 1.1.2 Location The deposit is located in northeastern Wisconsin within a topographical high called the Northern Highlands region. The deposit lies about 5 miles directly south of Crandon and about 2 miles east of State Highway 55 on Sand Lake Road (see fig. 1). Other local communities include Rhinelander 28 miles west, Antigo 45 miles south, and Iron River and Iron Mountain, in Michigan, 75 and 44 miles east and north of Crandon respectively. In relation to the lakes and streams, the deposit lies 0.25 miles north of Little Sand Lake, and about 1 mile south of Swamp Creek.

Jan 1, 1981

By Martin Rubenstein

CdS crystals have been grown from a number of metallic solvents such as bismuth, tin, lead, and cadmium. Etching studies have shown that plastic deformation occurs if the crystals are not removed from the solvent prior to the solidification of the solvent, on cooling. The deformed crystals show a umique exciton fluorescence as a function of edge dislocation density. If one grows the CdS in the eutectic alloy of the above four metals (commonly called Wood's metal) the crystals can be removed from the solvent with hot water and no plastic deformation occurs. In this paper, the liquidus solubility measurements of CdS, as a function of temperature, are presented. The data were obtained using a high -temperature filtration technique. CADMIUM-SULFIDE crystals have been grown from a number of metallic solvents1 such as cadmium, bismuth, tin, and lead. Liquidus solubilities of CdS in cadmium,2 bismuth,3 and tin4 have already been measured. Crystals of CdS, in all four metals, have been grown by solution growth: 1) by cooling a saturated solution and 2) by a solution transport method.1'"1 CdS crystals grown in these four solvents have a few characteristics in common: 1) 1.8°K photolumines-cent emission consisted mainly of the radiative recombination of the bound exciton commonly known as I,, 2) slip lines which could easily be seen by the naked eye, and 3) edge dislocation densities in the order of l05 per cu cm.1 It was decided that these slip lines and the high edge dislocation densities were caused by a plastic deformation of the CdS crystals. It was felt that this plastic deformation did not occur during the growth of the crystals nor during the cooling of the solution, but did occur when the solvent which was in contact with the crystals froze. If these assumptions were valid, the slip lines and the high number of dislocations could be reduced or eliminated by removing the crystals from the solvent before the solvent froze. Since crystals of CdS had already been grown separately in such solvents as bismuth, lead, tin, and cadmium, it was felt that crystals could be grown in a eutectic mixture of these four metals. In this work a eutectic (or near eutectic) mixture of bismuth, lead, tin and cadmium in the proportion 50, 26.5, 13.5, and 10 wt pct, respectively, was used to grow CdS crystals. Such a mixture has a melting point of about 70°C and is close in composition to the alloy commonly known as Wood's metals. If the crystals could be grown from this mixture of solvents, and if hot water (>75°C) could be used to separate the crystals of CdS from the metallic solvent, it was hoped that CdS crystals could be grown with little or no plastic deformation which had been ob- served when crystals were grown from these solvents uncombined. CdS crystals were grown from this low melting eutectic mixture of bismuth, lead, tin, and cadmium using the solvent transport method. CdS powder and the appropriate amount of metals were sealed in a quartz tube under a pressure of about 5 X 10-6 torr. This ampule was then placed in a vertical position in a furnace. The temperature was raised to about 900°C. The furnace was designed so that the top of the liquid column within the ampule was between 10° to 40°C higher than the bottom of the liquid column. These temperatures were measured on the outside of the quartz ampule. The ampule was maintained at temperature for 7 to 14 days (depending on the temperature at which transport was taking place) and then the furnace temperature was lowered until the temperature was about 125°C. The ampule was then removed from the furnace, placed in water maintained at about 90°C, and opened in this 90°C environment. The crystals could then be removed from this two-phase liquid (Wood's metal and water) by mechanically picking them out. Alternatively, the crystals could be quantitatively removed by adding an excess of mercury to the mixture of metals, crystals, and hot water. The hot solution of metals and the hot water could be evacuated using a small diameter tube connected to a vacuum. Small amounts of mercury and water could be removed by heating the crystals in vacuum. Crystals prepared using this technique showed no evidence of slip. However, some of these crystals did show edge dislocation densities as high as l04 per cu cm. Some few selected crystals showed no dislocations. Single crystals of CdS were grown as large as 5 by 5 by 0.5 mm. The ampules for the growth of these crystals were 13 mm O.D., 11 mm I.D., 150 mm! LIQUIDUS SOLUBILITY MEASUREMENTS The CdS starting materials was G.E. 118-8-2 powder which was fired in H2S at 1000°C, and then a vapor transport technique5 was applied to produce a "sound" mass of CdS. The Wood's metal was prepared by weighing out bismuth, lead, tin, and cadmium in the proportions of 50, 26.5, 13.5, and 10 wt pct, respectively. The bismuth, cadmium, and lead were from the American Smelting and Refining Co. (ASARCO) and all had purities of 99.999+ pct. The tin was 99.9999 pct spectroscopic grade from the Vulcan Materials Co. The appropriate mixture was placed in a quartz tube, evacuated to a pressure of 5 X 10-6 torr, melted to a liquid, cooled to room temperature under this same vacuum. This ingot was then placed in another quartz tube, evacuated to 5 x l0-6 torr, and sealed off under vacuum. The ampule was then horizontally placed in a furnace. The temperature was raised to 600°C, and over a period of several hours the ampule was vigorously shaken several times. The ampule was then removed from the furnace, and the metallic liquid was

Jan 1, 1970