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By C. L. T. Edwards

In the preparation of this paper, the author has drawn upon experience with the operation of a blast furnace on Ioo per cent scrap burden, which he believes was the first operation of its kind in the country. It is the writer's further belief that much of the controversy attending discussions of this subject may be obviated by the presentation of a group of facts that should be known by blast-furnace men and open-hearth men alike. The following question has been raised: "Is iron made with scrap in the blastfurnace charge as good iron as that made without scrap—made with straight ore?" This question may he answered in part by the fact that the open-hearth men of the Bethlehem Steel Co. who used pig iron from a blast furnace that operated on Ioo per cent steel scrap found no difficulty in the processing of such iron other than that to be expected from the known analysis. Operation with ioo PeR Cent Steel Scrap During World War I, there was accumulated at the Bethlehem plant of the Bethlehem Steel Co. some 22,000 tons of alloy-steel turnings and borings. This scrap material was highly corroded and, like alloy-steel turnings of that period, were as a drug on the market. There was also a small tonnage of scale, rich in valuable metal. If this scrap could be worked up into pig iron, it would become readily available for use in the open hearth. In order that the pig iron should contain the maximum percentage of nickel, permission was obtained from the Management to try a Ioo per cent scrap operation. Accordingly, a blast furnace was swung over on July 25, 1919; the percentage of steel scrap increased more or less irregularly until July 29, when Ioo per cent steel turnings were charged. Except for occasional charges of nickel scale as an "cxtra," the operation continued uninterruptedly until Aug. 27, when the furnace was swung back to the regular ore—ore and scrap—operation. During this period, the furnace production ranged from a low of 568.60 tons to a maximum of 766.07 tons. At the swing-over from Ioo per cent scrap to the regular burden, the charge I hung up rather severely. While the latter condition has nothing to do with the object of the paper, a brief discussion of the experience will appear later because of the interest it may have for blast-furnace operators. In Table I, results of the first and last days of the ore charge are shown, July 25 and July 29. The last column shows a summary for the period of maximum scrap ' charge. The furnace employed had a hearth 16 ft. o in., bosh 22 ft. o in., stock line 15 ft. 6 in., bell 11 ft. 6 in., batter in., bosh angle 73' 27' and a Balrer-Neuman top, with gas-engine blowers. Analyses Range of material charged Gravel: SiO2, 64.40 to 70.54 per cent; A1203, 3.52 to 4.58; CaO, 7.27 to 9.49; MgO, 5.09 to 6.14; FeO, 1.67 to 3.34, ignition loss, 9.50 to 13.83. I

Jan 1, 1942

By Kalanadh V. S. Sastry, D. W. Fuerstenau

A locked-cycle balling procedure has been designed to simulate continuous, closed- circuit balling drum operation in the laboratory. By this method, it is possible to simulate the surging in green-ball production rate and circulating load that is experienced in industrial balling circuits. Through an investigation of the effect of feed rate on the stability of the locked-cycle, balling process, it was found that higher feed rates lead to increasing instability in the process. An analysis of the experimental ,results is presented and the utility of the locked-cycle experimental technique for evaluating the stability of an industrial balling drum operation is discussed.

Jan 1, 1976

By D. W. Rudd, D. W. Vose, J. B. Vetrano

In an earlier paper the permeability character of Mo-0.5 pct Ti to hydrogen was described.' It was shown that this alloy is a more effective barrier to the passage of hydrogen than previously studied systems, i.e., copper,2 nickel,3 and several stainless steels.4 The permeability of Hastelloy B to hydrogen was investigated as a material having promising high-temperature structural properties which might have a low permeability to hydrogen. The general theory of permeation has been previously discussed,' and here only a summary of the more important results are given. It is found that except for very thin membranes, at low temperature, permeation of a gas through a metal barrier is determined by the rate of diffusion of the gas through the crystal lattice of the specimen, and that for hydrogen and the common diatomic gases, this passage involves dissociated particles as the diffusing species. The rate of permeation for hydrogen is therefore proportional to the square root of the pressure. It has also been found that the rate of permeation is inversely proportional to the thickness of the barrier. The apparatus used in this investigation was fundamentally the same as that employed in previous studies,' except that several simplifications result in the case of Hastelloy, since oxidation at the temperatures investigated is no longer a problem and welding of the specimen is relatively easy. A cross section of the membrane assembly is shown in Fig. 1. When finished, the assembly is about 5 in. long. The wall thickness is about 6 times the membrane thickness. The membrane (A) can be maintained at

Jan 1, 1963

By A. D. Schwope, L. R. Jackson, A. M. Hall

IN the course of an extensive investigation of the comparative properties of several types of copper, data were obtained on the cold working and subsequent recovery and recrystallization of the copper. In this paper, relations between the degree of cold work and the course of recrystallization are developed. In particular, it is shown that the course of recrystallization over long periods of time and at low temperatures can be predicted with reasonable accuracy from short-time high-temperature recrystallization data. MATERIALS USED IN THE INVESTIGATION Three types of copper were used in this investigation; these were tough pitch, OFHC, and OFHC copper with 15 oz per ton of silver added identified herein as Lots C, D, and F, respectively. The material was supplied by the American Metal Co. Ltd., and processed by the Rome Cable Co. The analyses of the three types of copper are given in Table 1. Originally, it started as wire bars 4 X 4 X 54 in. These bars were heated to 871°C in air and hot rolled to 3/8 in. rod. This rod was cold drawn to 0.204 in. rod (70 pct reduction) in three passes and annealed at 427°C for 4 hrs. A portion of the 3/8 in. rod was saved for more detailed cold-drawing experiments. Starting with the annealed 0.204 in. rod, hard-drawn wires were produced by cold drawing to 0.081 in. wire in 7 passes (84.4 pct reduction in area). Half-hard wires were made by cold drawing the 0.204 in. rod to 0.102 in. wire, (75 pct reduction) in 6 passes and annealing at 427°C for 4 hrs. This annealed wire was then drawn to 0.081 in. wire, (37.1 pct reduction) in 2 passes. Square rod was made by hot rolling wire bars to 9/16 in, rod in 8 passes. This rod was then cold drawn to 0.445 in.-diam rod and annealed for 3 1/2 hrs at 538°C. It was then cold drawn to 0.325 in. rod and again annealed at 538°C for 3 1/2 hrs. Hard square rods were then made by cold rolling this material to 0.257 X 0.257 in. rod, a reduction in area of 20.5 pct. Half-hard square rods were made by cold rolling to 0.268 X 0.268 in. square, annealing for 332 hrs at 538°C and cold rolling to 0.257 X 0.257 in., a reduction of 8.5 pct. Soft wire or rod was made from all types of copper by annealing the hard-drawn material at 343°C for 3 hrs in steam. The grain size of the annealed 0.081 in. wire varied slightly among the three lots: from 0.015-0.025 mm in the silver-bearing OFHC to 0.035-0.045 mm in the OFHC copper. The annealed 0.257 in. wires were more uniform in grain size, averaging about 0.035-0.045 mm. Representative structures are shown in Fig I. EFFECT OF COLD DRAWING AND TENSILE STRAIN ON STRENGTH OF COPPER Conventional tensile tests were performed on the three types of copper in the various degrees of hardness described above. Results of these tests are tabulated in Table 2. The results in Table 2 are

Jan 1, 1947

By R. S. Hendricks

During the past two years, Hecla Mining Co. has used shotcrete for ground support purposes with substantial cost savings. Hecla's experience indicates that shotcrete is an extremely effective ground support material which can be successfully employed in problem areas where various conventional systems would fail. To date, Hecla's use of shotcrete has been limited to openings where long-term high-quality support was required, to specific areas where exceptionally difficult ground conditions were encountered [ ] and, occasionally, to stope support. It is anticipated that when the necessary engineering and procurement of the components of an efficient materials handling system have been accomplished, shotcrete will be used on a routine basis in stoping and development situations. The real future of shotcrete is based, however, on the fact that this form of support offers greater opportunity for mechanization than rock bolt, timber or steel. Unlike all other support operations, which are cyclic, shotcrete is a continuous process, and therein lies its potential for incorporation into an efficient rapid excavation system. Hecla has obtained and operated both wet- and dry-process shotcrete application equipment. The operational characteristics of the two processes are presented and discussed below.

Jan 1, 1970

By J. D. Livingston

THE hardening of alloys by the precipitation of a second phase has long been an important technological process. One approach towards improving our understanding of this phenomenon has been a correlation of mechanical properties with such parameters as particle size and inter par ticle spacing.' Several reviews of such data have appeared.2-4 A major limitation to this approach has been that for most alloys the particles are submicroscopic in size in the range of optimum hardness. Precipitation-hardening copper-cobalt alloys, therefore, are of interest, because the ferromagnetic properties of the precipitate make it possible to measure particle size, number of particles, and so forth, from magnetic measurements alone.5, 6 Livingston and Becker7 have applied these techniques to a study of precipitation hardening in an alloy of 2 pct Co in copper. It was found from magnetic measurements that nearly all the cobalt to be precipitated was out of solution within a few minutes at 600°C, whereas the peak in tensile yield stress was not attained until a much longer aging time. Thus during the first 1000 min of aging time at 600°C the Yield stress was increasing while a constant volume of precipitate was coarsening, i.e., while particle size and interparticle spacing were increasing. Peak yield stress was reached at an average particle radius of about 70A. The earlier study was confined to one alloy at one aging temperature, so that the volume fraction of precipitate was fixed and, therefore, particle size and interparticle spacing could not be independently varied. The work has now been extended to several alloys of varying percentage cobalt in copper, and to aging at various temperatures. It was hoped that such a study might clarify the relative importance to precipitation hardening of particle size, interparticle spacing, and volume fraction of precipitate. EXPERIMENT The alloys studied contained 0.7, 1.3, 2.0, and 3.2 wt pct Co in copper. They were prepared from electrolytic copper and electrolytic cobalt in a vacuum -induction furnace, worked to 3/8-in.-diam rod, and machined into tensile specimens with a gage section 1 1/2 in. long and 3/16 in. in diam. All specimens were given a solution treatment consisting of a 30-min anneal in nitrogen at 1000° C followed by a quench into iced brine. Subsequent aging was done in nitrogen and followed by a water quench. Average grain diameter was approximately 0.01 in.

Jan 1, 1960

By John Griffen, David H. Davis

Much of the ground to be covered by this paper was ably covered by a paper presented by Messrs. Morrow and Jordan1 before a joint meeting of the Iron and Steel Section of the Engineers Society of West-ern Pennsylvania and the A.I.M.E. Pitts-burgh Section at Pittsburgh in the spring of 1940. As that paper was not published, the present authors have availed them-selves of Mr. Morrow's kind permission to use information given therein. Similar figures for the latest years available have been added to many statistics originally presented. It is unfortunate that Mr. Jordan's death removes his stimulating guidance and help, which the authors would have welcomed and have found invaluable in the past. One interested in the Pittsburgh seam should not fail to read the exhaustive and authoritative paper by Eavenson2 presented in 1938. As Allegheny, Fayette, Greene, Washington, and Westmoreland Counties contain practically all the reserves and furnish nearly all of the production from the Pittsburgh seam in Pennsylvania at the present time, this area only is intended when reference is made to the Pittsburgh seam in Pennsylvania. On much of the seam in Greene and Washington Counties, which contain a large proportion of the total reserves, insufficient data are available to determine the detailed characteristics of the seam with any degree of finality. It is hoped that the data presented here will fairly well indicate the probable characteristics. Economic Importance of the Pittsburgh Seam The Pittsburgh seam in Pennsylvania is of primary importance as a coal resource, not only because of its substantial reserves but because it contributes such a large proportion of the coal used in the country and an even larger proportion of that used in the manufacture of coke. Mr. Ashley3 placed the estimated recoverable reserves (1935) of the Pittsburgh coal bed in Pennsylvania at 7,500,000,000 tons.* Although a considerable portion of this tonnage is not now suitable for coking coal, because of its high sulphur content, undoubtedly the supply of coking coal will last for many years and that not suitable for coking will furnish industry with an ample supply of energy. In attempting to assess the contribution of the Pittsburgh seam to total coal production and to that of coal used in making coke, one finds that the statistics published annually by the U. S. Bureau of Mines, Minerals Yearbook, do not give tonnages classified as to seams but only as to districts or states and counties. However, it happens that, at present and during much of the

Jan 1, 1944

By David H. Davis, John Griffen

Much of the ground to be covered by this paper was ably covered by a paper presented by Messrs. Morrow and Jordan1 before a joint meeting of the Iron and Steel Section of the Engineers Society of West-ern Pennsylvania and the A.I.M.E. Pitts-burgh Section at Pittsburgh in the spring of 1940. As that paper was not published, the present authors have availed them-selves of Mr. Morrow's kind permission to use information given therein. Similar figures for the latest years available have been added to many statistics originally presented. It is unfortunate that Mr. Jordan's death removes his stimulating guidance and help, which the authors would have welcomed and have found invaluable in the past. One interested in the Pittsburgh seam should not fail to read the exhaustive and authoritative paper by Eavenson2 presented in 1938. As Allegheny, Fayette, Greene, Washington, and Westmoreland Counties contain practically all the reserves and furnish nearly all of the production from the Pittsburgh seam in Pennsylvania at the present time, this area only is intended when reference is made to the Pittsburgh seam in Pennsylvania. On much of the seam in Greene and Washington Counties, which contain a large proportion of the total reserves, insufficient data are available to determine the detailed characteristics of the seam with any degree of finality. It is hoped that the data presented here will fairly well indicate the probable characteristics. Economic Importance of the Pittsburgh Seam The Pittsburgh seam in Pennsylvania is of primary importance as a coal resource, not only because of its substantial reserves but because it contributes such a large proportion of the coal used in the country and an even larger proportion of that used in the manufacture of coke. Mr. Ashley3 placed the estimated recoverable reserves (1935) of the Pittsburgh coal bed in Pennsylvania at 7,500,000,000 tons.* Although a considerable portion of this tonnage is not now suitable for coking coal, because of its high sulphur content, undoubtedly the supply of coking coal will last for many years and that not suitable for coking will furnish industry with an ample supply of energy. In attempting to assess the contribution of the Pittsburgh seam to total coal production and to that of coal used in making coke, one finds that the statistics published annually by the U. S. Bureau of Mines, Minerals Yearbook, do not give tonnages classified as to seams but only as to districts or states and counties. However, it happens that, at present and during much of the

Jan 1, 1944

By Hermann Wedding

I ASK your permission to speak about a matter which is not of a specifically scientific nature, but more of a general-I might even say of an international-nature, and the international character which this city now presents must be my justification for introducing it. The Germans, very often, are thought to be an exceedingly warlike people, but I come to-day in the capacity of a peacemaker. Our German language is an original language; it is, therefore, a language in which it is impossible to change the meaning of a word at will. It may be, perhaps, easier in a combined language, as the English, to associate and to exchange meanings. Now, a word which we hear a great deal at the present day, is "Stahl," in English, "steel." This word means, in the German language, a substance which can be hardened. As the German literature, in relation to metallurgy, is the oldest of the modern world, this circumstance may give the German a right to ask for consideration. But I think, now, when the four languages, German, Swedish, French, and English, compete in rich metallurgical literature, it is very necessary to have uniformity in the nomenclature of iron, which would prove not only useful for science, but equally so for trade. For that purpose I propose to make the divisions of iron so that the word steel shall comprise a subdivision and not a primary division as formerly. Nature furnishes us iron mostly in the state of oxides, and if in any other condition, we must convert the ore into oxide before we can make iron. The oxides are always mixed with certain earthy substances called rock or gangue. The extraction of iron involves, therefore, the twofold process of the reduction of the iron, and im¬parting to it the amount of carbon necessary for technical purposes, and the separation of the reduced and carburized iron from the gangue. The reduction is always effected by carbon or carbonaceous substances (coke, anthracite, carbonic oxide, etc.), and the result is, according to the degree of heat employed, either malleable iron or a non-malleable iron. The process of making malleable iron in this way is called, generally, the direct process-in German, Rennarbeil. It produces the iron in a solid state with a fluid cinder. By this process our ancestors made all their iron, and it has been revived in various ways in modern times up to the process of Mr. Blair, so far as I know, always without commercial success. The

Jan 1, 1877

This excellent paper by Dr. Colombo parallels quite closely the bench and pilot work done by the Hanna Research Laboratory on the Mesabi oxidized taconites. Because of the vast reserves and future ore requirements the need to perfect the selective flocculation-flotation process becomes very necessary. The selective flocculation process is a very efficient method of desliming, leaving a fairly clean, upgraded product for flotation. However, one of the problems that we have encountered in this process was some very fine, -2 micron liberated goethite in the slimes that did not flocculate. The complete slime removal is not necessary. We remove slimes to the extent of about 5% of the iron units. However, on difficult treating ores we would remove more slimes. The reclaimed water from our pilot plant has a turbidity of about 1000-3000 ppm. We can obtain lower turbidity water but to do this would involve additional lime as a tailing flocculant and we would run the risk of flocculating the entire ground pulp in the selective flocculation process because of the increased Ca level in the water. We have about seven different geological ore types out of 17 recognizable ore types that are treatable. All of these ore types require different degrees of dispersion and grinding which is a problem. The use of acrylic acid polymers as a selective flocculant has been patented by the American Cyanamid Co. This will-have to be

Jan 1, 1979

By Wm. Reuben Webster

BRASS is an alloy of copper and zinc. The brasses (using this term to denote all useful proportions of the two constituents) are the most valuable and widely employed of all [ ] nonferrous alloys, because of their high resistance to ordinary corrosive agencies and the very wide range of properties that may be imparted to them by variations in the proportions of the constituents and by variations in mechanical treatment and heat-treatment. Fig. I shows the normal physical properties, as determined by standard tensile tests, of the series when in the annealed condition. Fig. 2 shows the effect of varying amounts of cold-working on an almost pure brass containing 70 per cent copper and 30 per cent zinc. Fig. 3 shows the effect of annealing at various temperatures on the same alloy. This effect is somewhat modi [ ] fled by the degree of cold-working to which a brass has been subjected, as shown by Fig. 4. A fourth test, which is empirical, has been found useful because of its simplicity -the hot hammer test. Samples Y2 in. in diameter and ¾ in. long are placed in a suitable furnace. These are withdrawn one at a time at successively higher tempera¬tures and are subjected to the blow of a drop hammer weighing 50 lb. with a drop of 4 ft. The percentages of' reduction in length of the cylinders are plotted against temperatures and give a comparative measure of plasticity at different temperatures. The results of this test on several

Jan 1, 1942

By R. L. Fleischer, B. Chalmers

In order to observe size effects associated with a grain boundary, aluminum single crystals and bicrystals of various cross-sectional dimensions were deformed in tension. Typical stress-strain curves are presented in conjunction with measurements of the effects of changes in crystal dimensions. Some effects of the growth rate used in preparation of crystals are also described. It is indicated that the macroscopic constraints at a grain boundary are responsible for the most prominent grain-boundary effect, the production of multiple slip. Two measurements of the width of the region of double slip are in agreement. It is concluded that the yield stress of aluminum is affected markedly by the inherent oxide coating. THE general problem to be examined is that of dimensional effects in the plastic deformation of metal crystals. These effects will be termed "size effects" and are here defined as follows: A size effect occurs in a series of crystals if their plastic-deformation properties are a function of crystal dimensions. Clearly then size effects depend on the nature of the boundary conditions imposed on the crystal. Crystal boundaries can be of three types: interphase, inter-crystalline, and free surface. Such deformation effects as are caused by distribution of phases, grain size, lineage structure, and single crystal external geometry are specific types of size effects. This discussion will be confined primarily to grain-boundary and single-crystal size effects, though in practice most "single crystals" not only have a number of small angle boundaries but also have one or more surface phases, so that the boundary conditions appropriate to a free surface do not necessarily apply. Hence, to this extent interphase size effects will be considered. The question of size effects associated with grain boundaries (called here intercrystalline size effects)

Jan 1, 1959

By Arthur A. Center

World production of electrolytic zinc has shown an increase for each year since 1932. Production up to 1936 was summarized in my earlier paper [Trans. A.I.M.E. (1936) 121, 453-4641, and this present paper carries the subject through 1943. During this time of increase, it is safe to say that the average purity has been raised more or less continuously, and the amount of four-nines metal has been in- creased. While the period reflects preparations for and the carrying on of the present war, electrolytic zinc proved its value in many industries as a peacetime metal in the years from 1919 to 1940. World production (Table I) increased from about 594,000 tons in 1936 to around 858,000 tons in 1943; United States production increased from 127,171 tons to 329,903 tons for the same years. Total production of primary zinc in the United States is given in the first column of Table I; retort production of primary zinc, obtained by difference, in the last column. The curves drawn from these figures are shown in Fig. I. They represent continuations of the curves in the earlier paper that cover commercial production of electrolytic zinc from its inception in 1915 to 1935. The earlier paper gave data for total world production and foreign retort production (calculated therefrom) and showed curves of electrolytic vs. retort production

Jan 1, 1944

SHELBY M. HARRISON,* New York, N. Y. (written discussion ?).¬Your secretary requested a brief description of the Russell Sage Foundation, in order that members of the Institute, if they should desire to avail themselves of it, would know what type of service is offered to them through our institution. The foundation was established in 1907 by the gift of Mrs. Russell Sage of $10,000,000 as a capital fund, the income of which is to be spent for the improvement of social and living conditions in the United States. One of the lines of activity which the foundation has felt would lead toward this end is the development and promotion of community surveys; and because the scope and methods followed in these surveys are very similar to the scope and method of much of the institution's work in general, an idea of its main activities can perhaps be given best by describing one of our surveys. Incidentally, it may be pointed out that antecedent to the survey stand at least two important facts: first, the recognition. that communities are active, not static forces, that they develop, that changes in. material and human relationships occur continuously, and that with them come new social and civic problems which must, in many cases, be diagnosed and prescribed for anew; and second, the reality of scientific advances along lines which make possible at least some measure of solution of the problems. Evidences of these changes are abundant; many of them are found in the rapid growth of cities in the last few decades. Villages in agricultural districts, places where everybody knew everybody else, where the pulpit had been long the chief or only influence molding public opinion, where the air was unclouded by the smoke from factory stacks, where the water supply was not affected by pollution, where sunlight and building

Jan 5, 1918

By J. H. Bechtold

Tensile properties of annealed molybdenum were investigated from 1000" to—200°C. In the vicinity of room temperature a well-defined transition in tensile properties occurs. Reduction in area decreases from over 80 pct to 0 pct and, simultaneously, the yield strength increases about 60,000 psi. MOLYBDENUM, tungsten, iron, and many other metals and alloys with the body-centered cubic and hexagonal close-packed crystal structures change from ductile to brittle behavior over some relatively narrow temperature range. The temperature at which this transition in ductility occurs depends on chemical composition, microstructure, and method of testing. When fine grained, completely recrystallized molybdenum of commercial purity is tested in uniaxial tension at a slow strain rate, the transition occurs at slightly below room temperature.' Iron2 and tungsten3 tested under similar conditions become brittle at temperatures close to the boiling point of nitrogen, — 195°C and at about 200°C, respectively. A sharp change in ductility is uncommon in metals with the face-centered cubic crystal structure, however, a relatively sharp transi- tion in notched bar impact properties has been observed below room temperature in a face-centered cubic copper-antimony alloy.4 A transition from ductile to brittle behavior is usually explained by the concepts originally developed by Ludwik,5 and discussed and elaborated on by others including Orowan,6 Hollomon and Jaffe,7 and Gensamer8 In brief, there are two aspects to strength, first the resistance to flow and second the resistance to fracture. Both are functions of temperature, strain, strain rate, stress system, composition, and microstructure. With decreased test temperature the flow stress required to initiate plastic deformation increases more rapidly than the fracture strength and brittle fracture occurs at that temperature where the yield strength equals or exceeds a brittle fracture strength. This investigation was conducted to determine the effects of temperature, strain, and rate of straining on the flow and fracture strengths of molybdenum above, through, and below the ductile-to-brittle transition. Other variables were held constant during testing. This information is believed to show

Jan 1, 1954

By J. L. Bray, S. T. Ross

The paper provides electrometallurgical data on the problem of germanium removal from zinc sulphate solutions. Germanium traces have caused much concern to the zinc refiner. Confirmatory evidence of interaction between germanium and cadmium is presented. Statistical analysis of data expands its significance and enhances its value. Further research is outlined. THE literature contains many references to the effects of trace amounts of germanium in the production of electrolytic zinc. One of the authors had experience with this troublesome element as early as 1917 at Trail, B. C. In 1929, Tainton and Clayton' reported that concentrations of as little as one part per million of germanium were sufficient to cause serious losses in current efficiency. Liddell2 reported that trace amounts of germanium cause marked lowering of the hydrogen overvoltage of electrolytic zinc cells, so that commercial production was impaired. Bray3 recorded the history of germanium in relation to electrolytic zinc production, noting that concentrations below 10 ppm have been found to yield low current efficiencies and copious hydrogen evolution. Koehler' stated that germanium "when present to the extent of a small fraction of one part per million per liter, causes serious evolution of hydrogen with a corresponding reduction in current efficiency." Recently, however, S. W. Ross" reported, from Risdon, Tasmania, that "in the course of leaching . .. dissolved traces of germanium... if not removed almost completely ... increase the reversion of cadmium during the filtration of the copper-cadmium precipitate and reduce the current efficiency during subsequent analysis." The copper-cadmium precipitate referred to is the residue from the zinc-dusting purification of zinc sulphate leach solutions. In the face of such conflicting testimony and with the increasing industrial importance of pure germanium and zinc it was decided to investigate the relationship between cadmium and germanium. Furthermore, other work by the authors showed certain discrepancies to exist in the theories of Tainton, et al. In the laboratory, without marked efficiency decreases, the authors have deposited zinc successfully from solutions containing as high as 1 g per liter of germanium. This could be done only when there was no cadmium present. Preliminary investigations of the suspected rela- tionships were carried out by means of emission spectrographic analysis using a beryllium internal standard. Several solutions containing 100 g per liter of zinc, as zinc sulphate, and 1 g per liter of cadmium, as cadmium chloride, were prepared. These concentrations were on the order of those obtained during a commercial low-acid leaching process. Varying concentrations of germanium were added to these solutions so that the range of 0.0000 to 0.5000 g per liter of germanium was covered. A 250 ml sample of each solution was agitated with 2.5 g of zinc dust for 30 min, filtered, and the filtrates were examined spectroscopically. Qualitative evidences of cadmium traces were found in those filtrates which originally contained above 10 ppm of germanium. Reliability of the analytical method did not permit quantitative investigations since cad-Table I. Current Efficiencies Obtained at 0.0000 and 1.5000 G per Liter Cadmium Concentrations Ge Concentrastion,* Cd Concentration,* EtBclenoy, G per Liter G per Llter Pot 0.0000 0.0000 84.270 0.0010 0.0000 94.849 0.0050 0.0000 92.649 0.0075 0.0000 94.039 0.0100 0.0000 96.084 0.0000 1.5000 93.460 0.0010 1.5000 95.158 0.0050 1.5000 92.148 0.0075 1.5000 91.260 0.0100 1.5000 84.546 • Cd and Ge concentrations shown are those existing before zinc-dust purification. mium determination in the concentrations present in zinc-dusted solutions lacks sufficient sensitivity for reproducible results. As a consequence of the inability of the investigators to obtain acceptable results through direct quantitative analysis, an indirect approach was devised. This indirect method involved a study of the current efficiency, in a model zinc cell, as a function of the concentrations of cadmium and germanium. Variables such as cell temperature, voltage, current density, anode spacing, relative electrode area, degree of agitation, cathode preparation technique, time, acid concentration, and solution volume were held constant. Fig. 1 shows the cell used. The current was fur-

Jan 1, 1952

By Tell Ertl, Will Mitchell

THE Mineral Industry Education Division made the headlines when Columbia's President, Nicholas Murray Butler, welcomed it in a provocative address made before a record crowd of over 100 members attending the opening Sunday session in the Columbia Men's Faculty Club. Arthur F. Greaves- Walker, Chairman of the Division, who was presented by H. R. Hanley, told of the excellent job of war research being carried on in the colleges. E. A. Holbrook led a discussion on the unionization of engineers, stating that he had learned that professional engineers were being forced into unions by subprofessionals. This might become a serious problem if the professional engineering organizations are lax in combating the

Jan 1, 1944

By Robert H. Richards, E. E. Bugbee

Friends often ask how accurate the work of our little stamp mill is, or express the opinion that a little mill cannot do good work. As a reply we would like to place on record the results of a few tests. There are two periods of work in our laboratory; the fall term, when the class collectively goes through all our chief laboratory-processes, and the spring term, when the students work up their theses, each electing some one process or investigation and devoting himself wholly, or almost wholly, to that. Some of the tests, the results of which are recorded in this paper, were made in the fall term; the preparation of the apparatus, the sampling and the assaying being done largely by assistants, with the aid of the students. Others were made in the spring term as thesis-work, and the results are due wholly to. the students. The complete " tree " of our process is patterned after the-

Jan 1, 1904

By J. Gordon Parr, G. R. Purdy

The phase boundaries of "TiNi" have been accurately determined by high-tewperature X-ray diffraction and metallo-graphic techniques. The phase (centered at 51 pct Ni) has a restricted range of homogeneity at 500°C, and a much greater range at 800°C. "TiNi" in all alloys containing less than 51 pct Ni decomposes rapidly and reversibly at 36°C to form a previously unreported phase. ThE region of the titanium nickel system corresponding to the phase "TiNi" has been the subject of several investigations.1,2,4-7 Laves and wallbaum1 reported "TiNi" as a body-centered cubic (a2) Phase, and Duwez and Taylor2 determined its para- meter to be 2.986. Duwez and Taylor also reported that "TiNi" decomposed into "Ti2Ni" and "TiNi3" on prolonged heating at 650" and 800°C, which led McQuillan3 to suggest a sluggish eutectoid reaction between "TiNis" and "Ti2Ni". Margolin, Ence, and Nielsen,' working with higher purity alloys, found no evidence of this decomposition. They showed the "TiNi" phase region extending from 49 to 54 pct*

Jan 1, 1962

By W. D. Potter, E. T. Peters

Single-crystal films of boron have been prepared by thermal reduction of purified BCl3 with subsequent deposition of boron onto oriented silicon substrates. The structural properties of films prepared under various experimental conditions have been determined by light microscopy and "grazing-" angle electron-diffraction analysis. An orientation relationship is proposed for silicon and a-rhombo-heclral boron which can be described as: (111)Si (112)B; [110]Si [110]B ElEMENTAL boron is known to have a high energy gap* and consequently has potential value as a high- *Energy gaps of 1.35 to 1.55 ev1-3 and 2.0 ev4 are reported for ß-rhombohedra1 and a-rhombohedra1 boron, respectively. temperature semiconductor.5 Exploitation of this property, however, has been hampered by the unavailability of pure, single-crystal boron. Two recent symposia6,7 have treated the subjects of purification, crystallization, crystal structure, and properties of boron and provide a foundation for further investigation in these areas. The structure, lattice constants, and observed ranges of stability for four reported polymorphs of boron8°12 are listed in Table I. The rhombohedral structures are generally accepted as true polymorphs whereas the tetragonal structures are believed to be transient. Most currently available single crystals of boron are grown by Czochralski and floating-zone methods. Unfortunately, these crystals generally contain numerous defects and are highly strained as a result of the polymorphic transformations and thermal contractions which accompany cooling. Recently, Armington, Potter, and Tanner13 have reported the formation of single-crystal films of boron on silicon single-crystal substrates through thermal reduction of BC13 by hydrogen. Boron E. T. PETERS, Junior Member AIME, is Senior Scientist, ManLabs, Inc., Cambridge, Mass., and W. D. POTTER is Research Chemist, Air Force Cambridge Research Loboratories, L. G. Hanscom Field, Bedford, Mass. formed at temperatures near 1000°C was identified as the a-rhombohedra1 form, consistent with expectation. The present paper describes a continuation of this work with specific reference to characterization of the structural features of the deposited boron films. The ultimate goal of this program is to produce large-area single-crystal films of a-rhombohedra1 boron to be used for electrical and optical studies by other workers. PREPARATION OF BORON FILMS The experimental procedure of preparing thin films is similar to that described by Theuerer14 for the epitaxial growth of silicon by thermal reduction of SiC14 and has already been described as applied to the preparation of boron thin films.13 Briefly, a mixture of BCl3 vapor and dry hydrogen is passed over a heated silicon substrate. Thermal reduction of the BC13 allows deposition of boron on the substrate. The substrates were {111}-oriented, single-crystal silicon. Square specimens 0.63 cm on an edge by 0.1 to 3.0 mm thickness were prepared by

Jan 1, 1965