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By E. C. Truesdale

A FEW years ago H. M. Cyr, working in the Research Laboratories of The New Jersey Zinc Co., produced a few pounds of zinc1 of such purity that no other elements were detected in it by spectrographic analysis, using the facilities then available. This zinc contained less than one ten-thousandth of one per cent of metallic impurities.2 During the decade that followed upon the laboratory production of this "spectro-graphically pure" zinc, commercial developments brought about the production of large tonnages of zinc of purity exceeding 99.99 per cent, and today zinc of 99.999 per cent purity is produced and marketed as "chemically pure" zinc. Typical analyses of present supplies of high-purity zinc are given in Table 1. TABLE 1.-Typical Analyses Percentage by Weight Sum of Zinc Pb, Fe, Pb Fe Cd Al Cd Special High Grades 0.007b 0.005b 0.0056 none 0.0106 C.P. (chemically pure) <0.0002 0.0005° 0.000052 S.P. (spectrographically pure).. <0.0002d <0.00005d a A.S.T.M. Standard Specification for Special High Grade Slab Zinc (A.S.T.M. Designation: B 6-37). b Maximum. c Fe chemically determined. Pb and Cd are spectrographically determined. d Differences between composition of C.P. and S.P. zinc are discussed later in this paper. The availability of commercial tonnages of special high-grade zinc has been the basis for the development of the zinc-base die-casting alloy industry which, in the year 1936, consumed one-eighth of the zinc used in the United States for all purposes. This and the C.P. and S.P. grades have given impetus to scientific investigations into the properties of pure

Jan 1, 1939

By D. M. Dunbar, H. C. SCHLILTZ

HE Chile Exploration Co.&apos;s mine and reduction plant are at Chuquicamata, Chile, on the eastern edge of the Atacama Desert, 163 miles northeast of Antofagasta, 80 miles from the Pacific Ocean, and 70 miles from the Bolivian border and at an altitude of 10,000 ft. Guggenheim Brothers started prospecting in -4pri1, 1912, and purchased the main property, in October of that year; the property is now controlled by the Anaconda Copper Mining Co., which acquired it in January, 1923. The orebody strikes north 10" east, and has a dip of about 64" west. The length, as far as developed, is approximately 1% miles; the width averages sightless than mile.

Jan 1, 1925

By George Krauss, Seth R. Thomas

One complete cycle, allstenite to martensite to aus-tenite, of Martensitic transformation was induced in a commercial 18 Cr-8 Ni stainless steel. Transmission electron microscopy showed that the reverse transfarmation, martensite to austenite, perpetuated the dense defect substructure of the martensite produced by the direct transformation, austenite to &apos;martensite, and reproduced the retained austenite matrix orientation. A general precipitation of lathlike M,,C, particles was noted to be present in, and is suggested as cause for, regions of martensite that Izad formed after a complete cycle of transformation. The habit plane of the precipitate particles was found to be within 5 a plane previously established as the habit of nitride precipitates of similar morphology in bcc iron. The direct transformation of austenite (y) to martensite (a) in metastable 300 series stainless steels has received considerable attention in the past,&apos;-8 and the martensite product given special emphasis in recent years,9"*u but little information has been published about the reverse martensitic transformation during which bcc a martensite is converted to fcc y austenite."-" The reversal mechanism and the resulting crystallographic relationship between parent and product austenite are of fundamental concern. The reversal product, fully austenitic, and hereafter referred to as reversed austenite, exhibits a defect structure far different from its virgin counterpart. Some studies have been reported in which the structure of reversed austenite in iron nickel alloys is compared to annealed austenite with respect to austenite strengtheningM and Stabilization.&apos; The martensite in these Fe-Ni alloys, however, shows a basic difference from that produced in stainless steels. Structurally, the Fe-Ni martensite is profusely twinned," while the (low-carbon) Fe-Cr-Ni martensite contains a high density of tangled dislocations and is apparently twin-free.I0 reediis" has recently shown in an Fe-16 Cr-12 Ni stainless alloy that this typical martensitic defect structure and the reverse transformation directly influence the structure of the reversal product. He found that much of the reversed austenite had returned to the orientation of the virgin austenite and that fine twins were formed in the austenite after the reverse transformation. This investigation was undertaken in order to describe as completely as possible the structural changes produced by a cycle of transformation in a typical 18-8 stainless steel. EXPERIMENTAL PROCEDURE The 301 stainless steel under investigation (17.44 Cr, 7.75 Ni, 0.80 Mn, 0.60 Si, 0.40 Mo, 0.40 Cu, 0.08 C, 0.03 N, bal Fe)was received as 0.060-in.-thick

Jan 1, 1968

By Fred W. Stiefel

To open the Fisher Hill mine of the Republic Steel Corporation, it was necessary to sink an inclined shaft into the rock and excavate stations, drifts, and ore pockets. This inclined shaft, or slope, q ft. 8 in. high by 28 ft. 2 in. wide, has compartments for two 5-ft. gauge ore-skip tracks of 120-lb. rail, one 5-ft. gauge man-skip track of 60-lb. rail, a concrete stairway, and service pipes consisting of a 12-in. compressed-air line, an 8-in. pump-discharge line, and a 4-in. water-supply line. When we were requested to investigate the work, the progress being made (by another organization) amounted to only 2 ½ ft. advance in 24 hr. We reported that progress of at least 6 ft. per day could be made. As a result, the Defense Plant Corporation, through the Republic Steel [ ] Corporation, entered into a contract with us to sink the shaft. The contract contained a penalty and bonus clause predicated upon an advance of 150 ft. per month. The average advance was 7.8 ft. per day; that in the best six-day week was 60 ft. and that in the best month, 215.5 ft. in 25 working days. The drilling was performed by 3 ½ -in. wet drifter drills mounted on five 8-ft. columns (see accompanying illustration). Even though a full-face drilling and mucking operation is customarily desirable, the steep slope, with the accumulation of water and fine debris at the face, made a modified heading and bench operation preferable. The heading and bench were of equal height. The five columns, instead

Jan 1, 1945

By J. A. Bownocker

THE Pittsburgh is one of the most important coal beds of Ohio. It was the last of the great coal beds to be worked extensively in that State, has the largest area of virgin coal, and will in all probability be the last of the great deposits to be exhausted. The line of outcrop sweeps nearly southwest in a sinuous line from Jefferson County on the north to Lawrence on the south, a distance on a bee-line of at least 150 miles. (Fig. 1.) The maximum width of the area under which this coal is due is about 55 miles, but in most places it is less than half that and in the two southern counties it is in places restricted to narrow ridges. Here as elsewhere the Pittsburgh coal forms the base of the Monongahela formation, and the following section taken from Condit shows the position of this bed with reference to certain higher ones in this field:1 FEET INCHES Shales and thin beds of limestone 24 5 Coal, Meigs Creek, No. 9 4 0 Shale, sandy 11 0 Coal 0 8 Shale, clayey 6 0 Coal, Lower Meigs Creek 3 0 Shales,clayey 2 0 Limestones and thin layers of clay 25 0 Unseen 11 0 Coal, Redstone 2 0 Unseen 11 0 Coal, Pittsburgh, No. 8 8 0 Clay 5 0 Limestone 4 0 From the standpoint of continuity the Pittsburgh coal of Ohio must be classed with the patchy type. As the map shows, the coal is thin or wanting along many miles of the line of outcrop. The large deposits form three separate areas, which, in order of their importance, are generally known as (1) the Belmont, (2) the Federal Creek, and (3) the Gallia fields.

Jan 10, 1926

By Clinton H. Crane

IN October, 1925, J. R. Finlay delivered an address entitled, "The Future Price of Lead." Lead was then selling at 8.85c. and Mr. Finlay and most of the rest of us were concerned about the shortage. Now, a little more than six years after, lead is selling for 3.55c., and nobody is worrying about the difficulty of getting plenty of it. For 1931 the U. S. G. S. reports United States produc¬tion as 390,000 tons of recoverable lead in ore. Our estimate is slightly higher than this; nearer 400,000 tons. This is the smallest production since 1911 and 1912, but in spite of this, stocks for the year-have increased nearly 50,000 tons. Our estimate for the production outside the United States is 1,120,000 tons, or more than double the production of either 1920 or 1921, and 30 per cent more than in 1913. Stocks abroad probably have not increased more than stocks in the United States. In other words, foreign consumption is double what it was in 1.920-21, whereas domestic consumption is substantially less. It looks as if Mr. Krueger, president of the Swedish match trust, was right when he said that "This country had better stop worrying about Europe and think a little bit more about its own affairs."

Jan 1, 1932

By J. R. FINLA

THE three great war periods of recent times involving the-chief industrial, commercial, and military nations of the world have been the following: 1. Wars centering around the French Republic and Napoleon Bonaparte, .1791-1815;. involving every nation in Europe, parts of Asia Minor and *North Africa., and the United States of America. 2. Wars in Europe, Asia, and North -America beginning with the Crimean War, 1854-56, the British Empire, France, Sardinia, and Turkey against Russia; the Sepoy rebellion in India, -1857; -war of France . and Sardinia against ..Austria in Italy, .185.9; :the Taiping rebellion in China, 1861; Civil War in , America, 1861-65; French. occupation .of .M Mexico, .1863; Prussian war against :Denmark, :1864; (Prussia and Italy against Austria sand various -south German : states, 1866; :the Franco-German War, 1870.7,1.

Jan 1, 1931

By F. H. Daniels

IN this, paper it is my intention to, call your attention to* a few of the many producers using blast, now, in common use in Sweden, and also those constructed by the Washburn & Moen Manufacturing Company at their Quinsigamond Works. During a prolonged stay in Sweden the writer had an opportunity

Jan 1, 1881

T.B.King (Depaytment of Metallurgy, Massachusetts Institute of Technology)— A valuable contribution of the authors is in the factual information which they have been able to gather; this type of information is quite difficult to obtain. In many respects, however, it would have been better if they had not subsequently embarked on a discussion of the chemistry of the converter process. It seems inconceivable that the authors do not refer to the papers of Schuhmann and his associates14 which have set the thermodynamic foundation for the whole copper smelting operation. In addition, a very useful review on the physical chemistry of copper smelting by Ruddle 5 appeared as long ago as 1953. An examination of this literature would have convinced the authors that there is no cause to be surprised at a correlation between the magnetic content and the silica content of converter slags, though they rightly point out that one should distinguish between the total magnetite content of the slag and the amount of magnetite which may be considered to be in solution. It is not true that the lowest melting converter slag is that corresponding to the eutectic between ferrous oxide and silica. The simplest slag system which can be considered is a three-component system, since both ferric and ferrous iron are present. As Schuhmann, Powell, and Michal have shown, there are lower melting compositions than this eutectic in the ternary system. The most unfortunate impression given by this paper is that the driving force for chemical reaction is determined by the heat of reaction: of course the entropy change must be taken into account. It would have been more correct to list, in Table VI, values for free energies of formation. Nor can it be said that the data in Table VI represent the "best available data." They do not corregtond with any of the recent, acknowledged sources. F. E. Lathe and L. Hodnett(author&apos;s reply)— We are pleased that Dr. King finds the factual information in our uawer of some interest. Dr. King suggests that it would have been better if our analysis and discussion of the data had been omitted, largely because our list of references is so. incomplete. If he will carefully read our introduction, he will see that the questionnaire was sent out in the hope of obtaining data which would throw light on certain questions relating to the use of converter refractories. We did not attempt (nor would the AIME have published!) a complete review of the literature on copper converting, as Dr. King has apparently assumed, nor indeed a complete analysis of the data submitted, but tried only to find a sound basis for the choice of refractories, taking into consideration common variations in converter practice. We hope our paper indicates that, by raising the silica content of the converter slag and operating at a higher temperature, the normal circulating load of magnetite can be greatly reduced, and the whole reverberatory-converter operation improved to a major degree, with resultant important savings. Under such operating conditions, chrome-magnesite brick may be expected to stand up better than those of straight magnesite. Regardless of the choice as between these brick types, however, we find the cost of converter refractories to be so low in comparison with other converter costs as to justify operation under the more severe conditions suggested. Valuable as are the papers by Schuhmann and associates and the book by Ruddle, we make no apology for omitting reference to them, nor for using heats of reaction without mention of entropy changes or free energies of formation. Our primary object was to interest the practicing copper metallurgist, with whose language we may claim to be fairly familiar; we think it would have been unwise to include the highly theoretical phases of the subject which Dr. King suggests. The interest shown in our preliminary paper presented at the New York meeting in 1956, and the trends in practice whtat we have observed since that time, suggest that we did not wholly miss the target. In conclusion, we sincerely hope that Professors King and Schuhmann will independently review the data obtained in our questionnaire and submit a paper giving their own recommendations as to the choice of refractories and the particular converter operating conditions which will result in the lowest overall cost of copper smelting and converting.

Jan 1, 1960

By R. J. Brison, O. F. Tangel

The development of a new method of mineral separation was sponsored by the International Salt Company, which requested Battelle Institute to investigate means for improving the quality and appearance of rock salt from the Company&apos;s Detroit mine. Although developed specifically for removing impurities from rock salt, the general method may be applicable to other separation problems. The principal impurities in rock salt from the Detroit mine are dolomite and anhydrite which represent 2 to 5 pct of the weight of the mined salt. In the size range from 114 to 112 in. (the range of primary interest in this project) the impurities are only partially liberated from the halite in normal production. Further size reduction to improve the liberation of impurities is not practicable in view of the market requirements for the coarse grades of rock salt. Laboratory separations in heavy liquids showed that, to improve the quality and appearance of the rock salt substantially, it would be necessary to remove not only free gangue particles but also a large proportion of the locked-in particles.

Jan 8, 1960

By J. S. Aronofsky, A. S. Lee

Results and experimental procedures are presented covering a preliminary laboratory investigation of the compaction of reservoir rocks and its effect on porosity and permeability. "Egective" compressibility was measured by subjecting core material to an overburden load and reducing pore pressure. Preliminary results showed relatively high effective compressibilities which varied from 1.8 X 10-&apos; pore volume/pore volume /lb / in.~ for limestones to 7.7 X 10-6 pore volume/pore volume/lb/in.&apos; and even higher for sandstone reservoirs conmining large amounts of fine clay material. It appeared from the initiol results that the effective compressibility of the material could not be correlated directly with porosity and that other factors, such as the amount of clay material present might have to be taken into account. The work to date has indicated that effective compressibility factors will have to be measured for the particular reservoirs heing studied. Oil permeability of core materid was measured under various effective overburden loads from 0 to 8,000 psi. It has been found than reduction of permeability in clean sands was relatively small and the results agreed with published data. For sandstones containing large amounts of clay, preliminary tests indicated very large reductions in permeability with increasing effective overburden pressures. It is planned to continue laboratory work on this phase because of its importance in low-permeability reservoirs. INTRODUCTION During the past few years increasing interest has been shown in the differences obtained between conventional laboratory measurements on cores at atmospheric pressure and those when reservoir conditions are simulated. Since these data are used as the basis for calculations and the prediction of reservoir behavior, their evaluation under reservoir conditions is most important. The effect of the compressibility of the rock upon the reservoir behavior, as fluid pressure declines, is an important subject which has been insufficiently studied. The total pressure on any plane through a reservoir is the result of the grain-to-grain rock pressure due to the overburden and the pressure of the interstitial fluid on the plane. As reservoir fluid pressure declines, the net load on the rock phase must increase, and the result is the compaction of the rock structure which produces a decrease in pore volume. Simultaneously, the rock grains expand into the pore space as the fluid pressure declines. The result of these two effects is defined as the effective compressibility of the rock and is expressed in units of pore volume/original pore volume/psi. Work was started by Imperial in 1954 on the effects of pressure on the porosity of reservoir rock. These studies established effective compressibility factors for some limestones and dolomites. Since that time effective compressibilities have been obtained for other Canadian and some U. S. reservoir rocks. In conjunction with the study of porosity, an investigation has also been initiated to determine the effects of pressure on permeability. One outcrop and several reservoir sandstone cores have been tested to date. ROCK COMPRESSIBILITY Apparatus anD Procedure A diagram of the apparatus used in these studies is shown in Fig. 1. The equipment was constructed so that a uniform pressure, equivalent to the reservoir overburden, could be applied by the oil pump and transmitted on all sides of the core through the Lucite sheath. The sample was completely saturated by circulating brine through the mounted core. Pressure in

By Don Simon

In the late 1960s the mining industry was in an apparent slump due to a combination of factors. Enrollment dropped significantly at schools offering mining engineering degrees, resulting in a shortage today of experienced mining graduates to staff middle management positions. How has this limited supply affected salaries? Does the shortage impair the mining industry&apos;s ability to respond to national energy needs?

Jan 12, 1979

By W. C. Hagel, J. H. Westbrook

Usittg a sectioning technique with Agl10 as the tracer, the diffusion of silver in silver-excess (45.8 at. pct Mg), near-stoichiometric (49.8 at. pct Mg), and magnesium-excess (52.0 at. pct Mg) cylinders of CsCl-type AgMg was determined from 500" to 700°C. Diffusion coefficients conform to the expression D = Do exp (-q/RT) where the respective Do values are 1.53, 0.280, and 0.134 sq cm sec-I and the Q values are 41.3, 40.6, and 38.0 kcal g-atom-&apos;. Lnttice-parameter and density measurements were performed on a more numerous assortment and wider range of compositions. Substitutional defects were found on both sides of stoichiometry. Activation energies for other rate processes in these alloys show related trends with changing composition, although silver may not be the rate-detemining species. KNOWLEDGE of diffusion coefficients is necessary for a quantitative understanding of the many rate processes (e.g., grain growth, precipitation, sintering, oxidation, or mechanical deformation) occurring in solids. Although these data are available for most metals and common alloys, they are quite limited for intermetallic compounds—a group of materials whose unique physical and mechanical properties are presently attracting great interest. From a fundamental viewpoint, diffusion in intermetallic compounds also offers several engaging aspects owing to: their ordering, the possibility of introducing large, stable concentrations of lattice defects, and the variety of bonding types and crystal structures which can be found. In the case of CsC1-type compounds, some previous work has been directed at examining the role of vacancy defects by changing their concentration compositionally. The diffusion of Co60 was measured in 0 NiAl1- and in P COA., Except for the results of Smoluchowski and Burgess, isothermal diffusion coefficients were found to pass through a minimum at the stoichiometric composi- they decreased sharply on what was reported by Bradley and co-wrkers&apos; to be the vacancy-rich (aluminum excess) side of stoichiometry. This investigation of the diffusion of Agl110 in AgMg was undertaken both as an adjunct to a concurrent study of its deformation behavior and for the purpose of obtaining information on the influence of lattice defects and temperature on diffusion in another CsC1-type intermetallic compound. Bcc AgMg remains ordered up to and melts congruently at 820°C. Solubility limits at 300°C are about 41 at. pct Mg and 53 at. pct Mg. It is one of the Hume-Rothery electron compounds with a 3/2 electron-atom ratio. Previous investigations of its properties include hardress,&apos; tenile,&apos;-&apos; electrical reistivity, and thermodyna-mic1&apos;,14 studies. Indications of a high bonding strength may be found in the large heat of mixing1&apos; and in the 6-pct vol contraction on compound formaticp, as calculated using atomic radii of l.40 and l.55a for Ag and Mg. EXPERIMENTAL PROCEDURE Alloys were prepared by the induction melting of selected fine silver (99.95) and low-iron magnesium (99.95) in magnesia crucibles under 1 atm of A. Supplied by the Handy and Harmon and Dow Chemical Cos., respectivelv. Melts were poured under argon into graphite molds providing 1 1/8-in.-diarn. by 4-in.-long ingots. These were homogenized in evacuated and argon-filled fused-silica capsules by heating for 16 hr at 750&apos;. Three 1 in.-diam. by 3/4-in.-long cylinders were machined from the mid-portion of each ingot for diffusion measurements. Three alloys, analyzing 45.8, 49.8, and 52.0 at. pct Mg were taken as representing the extremes of interest, with 49.8 at. pct Mg being very close to the stoichiometric composition of 50.0 at. pct Mg.

Jan 1, 1962

By Edward Thomas

THE late George S. Rice was active in the investigation of bumps, particularly in the last ten years of his career as chief mining engineer of the U. S. Bureau of Mines. Since most of his investigation was carried out in Great Britain, continental Europe, and-to a lesser extent-Canada, his thinking on prevention was influenced considerably by the experience of those countries. It is not surprising, therefore, that when he was called upon a few years before his retirement to investigate bumps in the U. S. and suggest ways to prevent them, he turned to longwall mining. A longwall method had been most successful in combating the bump hazard in mining coal under deep cover, especially in Great Britain, but the prevailing method there at the time was advancing longwall mining, which he knew was uneconomical under U. S. mining conditions. For this reason he proposed a modified retreating longwall system that he believed included the best features of the advancing method. As brought out by Rice,1 if the cover is 2000 ft and 50 pct of the coal is extracted, the static load on the remaining pillars will be about 4000 psi, which exceeds the ultimate crushing strength2 in most instances. If the pillar coal is overloaded before a pillar line is established, then the abutment zone preceding a line of extraction is no place to split pillars or extract them by any method other than an open-end system. Rice therefore advocated open-end mining, preferably by longwall, but he was willing to compromise with long-face mining if the longwall method was not acceptable.

Jan 8, 1958

Jan 1, 1943

By J. W. Dougherty, J. M. Douglas

THE Hollinger gold mine is in the Porcupine mining division, District of Cochrane, in the northern part of the Province of Ontario. The adjacent town of Timmins, with a population of 25,119, lies 490 miles by railway north of the city of Toronto. GEOLOGY The property is situated on the northwest limb of a major syncline, which pitches northeast at approximately 50°. The principal rocks of the Hollinger area are of pre-Cambrian age and consist of altered, schistose, Keewatin lava flows intruded by stocks of schistose, quartzfeldspar porphyry generally assigned to the Algoman period. The structure of the Keewatin series is extremely complex as a result of close folding and some faulting. The schistosity, trending north 70° east and dipping steeply to the southeast, is most highly developed along a subsidiary anticline in which the major porphyry bodies occur. The ore bodies, which exhibit three principal structures, consist of quartz veins and associated pyritized wall rock. Some lodes are composed of en echelon veins, others exhibit a main quartz body with branching stringers and a third consists of a single definite lead. Gold, in a coarse visible form, may be confined to quartz in some ore bodies but in others it is finely divided and is found not only in quartz but also associated with pyrite in the adjacent wall rock. In many veins the distribution of gold is such that there are several ore sections, separated by areas of low-grade material, in the same vein although its physical appearance remains unchanged. The veins form a very complex pattern in an ore zone which in places attains a length of 6000 ft. and a width of 4000 ft. They are most abundant in the Keewatin lavas in the neighborhood of the porphyry bodies. Few of the veins are persistent for long distances, though some

Jan 1, 1940

Jan 1, 1943

By James A. Lewis

It is the purpose of this paper to show the importance of sand characteristics, when combined with other physical data, in evaluating production obtained by secondary recovery operations, and to indicate the benefits to be gained from the application of these principles to primary production.

Jan 1, 1942

By T. Watanabe, S. Karashima, H. Oikawa

Creep tests of a! iron and its solid-solution Fe-Mo, Fe-Co, and Fe-Si alloys with bcc structure were conducted under constant stresses in ferromagnetic and paramagnetic temperature regions above 0.5T,(T, is the absolute melting temperature). It was found their high-temperature creep behavior changed in the vicinity of the magnetic transformation temperature, that is Curie temperature, TC. In the ferromagnetic region below the steady-state creep rates were lower than those expected from the extrapolation of the data in the paramagnetic region, the amount of decrease being affected by solute addition. Also, activation energies for steady-state creep were different in the two temperature regions. The observed changes were concluded to be due to the effect of ferromagnetism on diffusion. It is well-known that plastic deformation of metals and alloys in the temperature region where mobility of atoms becomes high enough is controlled by atomic diffusion." Many experimental results394 on fcc and hcp materials have been reported to confirm this view. In bcc metals and alloys, not much basic investigation of creep deformation has been performed. In particular, experimental work on iron5-&apos; and its alloys, covering a quite wide temperature range is extremely scarce. On the other hand, the effect of ferromagnetism on diffusion has recently been demonstrated in a iron and its alloys;&apos; it has been made clear that diffusion rates in ferromagnetic temperatur~e region are significantly lower than those expected from diffusion measurement in the paramagnetic region. Therefore, it is concluded that the magnetic effect influences the high-temperature creep behavior in a! iron and in its alloys. The present authors have conducted creep experiments on a iron and its solid-solution alloys over a very wide temperature range, and have demonstrated the magnetic effect. A part of the result has already been reported elsewhere.26 In this paper, the experimental results will be described in detail. While the manuscript was in preparation, a similar magnetic effect on creep deformation of a iron was reported by Ishida . Though their experiments covered an extremely wide temperature range, the creep stresses varied from several thousand psi to several ten thousand psi with decreasing temperature. Consequently, it may be said that there remain some questions concerning their results. I) EXPERIMENTAL PROCEDURE The materials used in the experiments were pure iron and its alloys; they were prepared by vacuum melting (10"" mm Hg) electrolytic iron (99.9 pct), molybdenum powder (99.9 pct), ultrapure silicon, and cobalt pellet (99.5 pct) in alumina crucibles. The ingots were hot-forged to plates 10 mm thick and 50 mm wide, and then were hot-rolled at about 700°C into sheets 1 mm thick. Creep specimens, 5 mm in width and 15 mm in gage length, were machined from the sheets. They were annealed at temperatures which were well above their respective recrystallization temperatures. The chemical compositions of the metal and alloys are shown in Table I together with their heat treatments. High-temperature creep tests by the use of a lever-type creep testing machine were carried out in argon atmosphere under constant tensile stress. In order to keep &eep stress constant within about *0.5 pct, stress change due to specimen elongation was compensated by tensile force of a stainless-steel bellows which was inserted between the loading lever and lower specimen grip with the assumptions of a linear relationship between change in cross section and strain and uniform strain along the section. Beyond the limit of compensation by the bellows, small amounts of load were removed after appropriate strains. The testing temperatures were maintained to within i2"C of the reported values. Creep deformation was auto-graphically recorded at the upper (moving) specimen grip using a linear differential transformer which was held by a stainless-steel rod mechanically connected to the lower specimen grip. It was also directly measured with a dial-gage reading to -& mm. 11) EXPERIMENTAL RESULTS AND DISCUSSION 1) Creep Curves of a Iron and Its Alloys. Creep curves of a! iron, Fe-Si, Fe-Co, and Fe-Mo (<2 at. pct Mo) alloys usually consisted of three stages, that is transient (primary), steady-state (secondary), and accelerating (tertiary) stages. An example is illustrated in Fig. 1 for a! iron. However, in Fe-Mo alloys with more than 2 at. pct Mo, an inverse transient creepZ8 was observed as indicated in Fig. 2. The inverse behavior, which varied with the amount of molybdenum, may be due to the substructure* in the annealed specimen as was sug-

Jan 1, 1969

By F. P. Bullen

Empirical relationships between fracture stress, orientation angle, and diameter of crystal have been determined at 77°K. Orientation ranges of markedly different behavior were found—a law of constant normal stress&apos; of value a (diameter)-1/2 for the fracture of ductile crystals, and a condition of shear stress (or strain) for more brittle crystals. The observations are not consistent with current theories. An interpretation is advanced which is also applicable to observations on the effect of prestrain at room temperature on the subsequent fracture stress at 77°K and to the effect of cyclic stressing on the cleavage strength.&apos;&apos; The law of constunt normal stress&apos; and the brittle ductile transition are also explained. The interpretation is more consistent with the initiation of cracks by intersecting dislocations than with theories based on stress -concentration by dislocation arrays. ZINC single crystals are particularly suited to the study of cleavage because fracture occurs on the basal plane over a wide range of crystal orientations. Analysis of the conditions of stress and strain at fracture in crystals of different orientations should indicate which parameters control the cleavage process. Unfortunately, controversy has arisen over the correct empirical relationship between tensile fracture stress and orientation. Schmid&apos;s observations1,2 favored a &apos;law of constant normal stress&apos;, as observed in other materials.2 For zinc, however, the observed values are far below the theoretical strength and cannot represent the true limit of cohesion between neighboring atomic planes. Hence, the interpretation of such a &apos;law&apos; is not straightforward. Deruyttere and Greenough3,4 found a complex variation between tensile fracture stress and orientation; this variation did not agree with a &apos;law of constant normal stress&apos;. Two theories have been advanced to account for their observations: a) the propagation of cracks from low-angle boundaries,5 and b) the release of energy from piled-up dislocations during crack-propagation.4 The present work resolves the apparent discrepancy between the observations and shows that neither of the above theories are applicable to the tensile fracture of zinc single crystals. A phenomenological explanation, along the lines suggested by Gilman,&apos; is advanced and successfully applied to previously unexplained effects. EXPERIMENTAL DETAILS &apos;Crown Special&apos; redistilled zinc was used, except for one comparison series op tests using &apos;Tadanac&apos; electrolytic zinc. Crystals of 1 mm diam, subsequently called &apos;1 mm crystals&apos;, were grown from the melt in vacuo in precision-bore Pyrex tubes internally coated with graphite. Several specimens 1 in. long were cut from each crystal and chemically polished. Jigs were used to minimize handling strains, and crystals were mounted in the Polanyi machine the day prior to testing to allow recovery from any such strains. One-mm crystals were chemically polished for long periods to obtain 0.1 mm (approx) crystals. One-mm crystals were cemented into miniature gimbals by &apos;Araldite&apos; casting resin. The Appendix gives the reasons for using gimbals and the results obtained by other methods. More complete details of all techniques are given elsewhere.7 The symbols and terminology used are as follows: X = orientation angle (angle between tensile axis and line of greatest slope in the basal plane). T = tensile stress (on true cross-section) S,N = shear and normal stress (components of T with respect to the basal plane) ? = shear strain D = crystal diameter. The subscript &apos;f&apos; will be used to denote values at fracture. PART I-ANNEALED CRYSTALS EXPERIMENTAL OBSERVATIONS One-mm crystals were used to establish the variation of fracture stress at 77°K with orientation at fracture (Xf), Fig. 1. For 18 deg = Xf = 55 deg, a &apos;law of constant normal stress&apos; was observed. For Xf > 55 deg, the fracture condition approximated to a constant shear stress. At Xf< 18 deg, twinning occurred before fracture so that the results were not typical of homogeneous single crystals,4,8— such specimens will not be considered herein. The dependences of fracture stress upon Xf were of similar type for 6 mm,* 1 mm, and 0.1 mm crystals,

Jan 1, 1963