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By P. B. Bucky, R. V. Taborelli

This investigation was carried on by means of models and the application of the principles of similitude to determine the effects of props, props and cribs and sand filling in longwall mining. The geologic structure and rate of face retreat were kept constant and the only change introduced was in the method of support. It is not felt necessary to repeat a description of apparatus, or to explain the fact that a scalar model made in all parts of the same material as the prototype will behave similarly to the prototype when rotated at speeds such that the centrifugal force is as many times the gravitational force as the prototype dimension is a similar linear model dimension. The reader is referred to earlier papers1,2 for further information regarding these statements. All models were made of sandstone and were as in Fig. 6. They are composed of a 3/16-in. ore body bed A, overlain by a 3/16-in. bed B, a ?-in. bed C and two ?-in. beds D and E. The model was rotated at + 2350 r.p.m. equivalent to a model ratio of 1268. It was worked back ¼ in. at a time before being replaced in the centrifuge and again rotated. Table 1 gives model and prototype dimensions occurring in this discussion, the prototype dimensions being 1268 times the model dimensions. Figs. 1, 2, 3 and 4 were taken while the model was rotating at 2350 r.p.m. One was taken for each face retreat of 26.4 ft., but for obvious reasons all are not presented. Fig. 1 (A-E) shows the behavior of this type of structure with face retreats of 26.4 ft. and no artificial support. Fig. 2(A-E) shows the behavior of this type of structure where breaker and face props were used. The props were exceptionally strong, being of steel ? in. square in cross section, and capped with 1/16 in. ± of soft wood and paper, to allow for roof deflection. The face props were

Jan 1, 1940

By J. C. Uy, T. E. Davidson, A. P. Lee

The effects of hydrostatic pressures to 26 kbars on the micro structure of poly crystalline Cd, Zn, Bi, Sn, Zr, Mg, Cu, and Fe were examined. Pressure-induced microscopic plastic flow in the form of boundary migration, slip, multiple slip, or twinning has been observed either singly or in combination in cadmium, zinc, bismuth, and tin. No deformation was observed in zirconium, magnesium, copper, and iron. The occurrence of such deformation, in terms of its intensity and initiation pressure, relates directly to the degree of anisotropy in the linear compressibility. Pressure cycling does not significantly affect the residual tensile properties of a zinc alloy which exhibits pressure-induced deformation similar to that of Pure zinc. CLASSICAL elastic theory predicts that a superim-posed hydrostatic pressure will not induce shear stresses in an ideal material. Thus, in the case of homogeneous and isotropic materials plastic flow will not occur as a result of pressure exposure, regardless of the magnitude of the pressure, unless some form of phase transformation or permanent density change takes place. However, real materials, such as metals, often vary considerably from the condition of homogeneity and isotropy. For this reason, Vu and johannin' examined and observed hydrostatic pressure-induced microscopic deformation in polycrystalline cadmium and, zinc, but not in aluminum, to pressures of 9 kbars and indicated that its occurrence is related to anisotropy in the linear compressibility. In addition, Davidson and omaan' have reported pressure-induced deformation in polycrystalline bismuth below the 1-11 transformation pressure. It becomes apparent then that under certain conditions hydrostatic pressure can induce localized internal shear stresses in some metals of sufficient magnitude to cause plastic flow. In this work, eight pure single-phase metals of different lattice structures and degrees of elastic anisotropy were examined after pressure exposures of up to 26 kbars in order to establish the conditions under which such deformation occurs and the type of deformation as a function of pressure. The effects of pressure cycling on the mechanical proper-

Jan 1, 1965

By W. C. Maurer

A study of the mechanics of shear failure of rock under pressure has been made. The transition from brittle to ductile failure occurs when the friction along the fracture surfaces exceeds the shear strength of the rock. A machine has been developed for measuring both the shear strength of rock and the friction along rock fracture surfaces. In this shear machine, the fractures are forced along definite planes; as a result, the rock is stronger than in compression tests where the fractures choose the weakest paths through the specimens. Friction is composed of several forces: (1) the forces to slide irregulurities on surfaces over each other; (2) forces to shear some of these irregularities; (3) molecular attractions across the fractures; and (4) forces required to break bonds resulting from melting and welding at the tips of irregularities on the surfaces. Friction along rock fracture surfaces is not proportional to contact pressure as usually assumed; instead, it increases as the contact pressure raised to the 0.4 to 0.8 power. INTRODUCTION It is difficult to produce tensile stresses under the high compressive stresses present in the earth; therefore, in deep drilling and geological faulting, shear failure predominates. This shear failure mechanism is complicated because rock is a heterogeneous material containing pore spaces, microfractures, elastic discontinuities and other imperfections. A study of shear failure of rock under pressure has been made to obtain a better understanding of this complex mechanism. A machine has been developed and used to measure the shear strength of rock and friction along sheared surfaces. This machine has certain advantages over the compression test — shear properties can be measured under low normal stresses and shear stress and normal stress can be varied independently. The first part of this paper is a description of shear failure of rock under pressure. The role of shear strength and friction along fracture surfaces in the shear failure mechanism will be discussed. The second part consists of a description of the shear machine and a discussion of the shear strength and friction data obtained using this machine. It will be shown that shear strength depends upon the size of the stressed zone, and that friction does not increase linearly with contact pressure as usually assumed. Attempts are made to relate some of the new concepts to tectonic failure and to dril ling. SHEAR FAILURE IN ROCK TRIAXIAL TESTS The shear failure mechanism is illustrated by the triaxial test shown in Fig. 1. In this test, a cylindrical rock specimen is subjected to a confining pressure, PC, and an axial pressure, pa. These external pressures produce normal a and shear T stresses on inclined planes within the specimen equal to1 where 0 is the angle between the specimen axis and a normal to the inclined plane. Fig. 2 shows how triaxial specimens deform as the axial pressure is increased. The pressure is

Jan 1, 1966

Edward Keller, Baltimore, Md. (communicatioin to the Secretary*):—It is pleasing to note the increasing amount of work on metallurgical problems that is being carried on by exact scientific methods, and the results of such labor issued by the laboratories of our universities. Without doubt, Mr. Bolles's paper will be welcomed by all progressive practitioners. Many of the results which Mr. Bolles presents to as are new; and I take exceptioil to a few minor points only. The first of his concluding remarks is as follows: "Mattes are not homogeneous, but are composed of distinct mineral entitier, and may be likened to igneous rocks, in which the mineral constituents fall out upon the lowering of the temperature and ensuing solidification." He quotes an introductory remark to a paper1 of mine, as follows: "The true chemical character of copper-mattes does not yet seem to have been definitely determined, i.e, it is still more or less of an open question whether they are true chemical compounds, or mixtures, such as igneous rocks." This quotation, taken alone, would convey the impression that Mr. Bolles's conclusion is entirely new. Had he quoted also another paragraph from my paper in question, it would be clear that he was, to a certain extent at least, anticipated. I take the liberty, therefore, to state the substance of my own work. In the paper referred to, I showed the existence of the phenomenon of liquation in mattes, and, continuing, said: " A more direct method to test whether a matte is a compound sulphide or a mixture of individual sulphides was attempted by applying hydraulic separation. A clean piece of matte was selected containing practically no magnetic oxide and of the following composition: Cu, 37.96; S, 24.45; Fe, 33.63; Zn, 1.25; Pb, 1.02 ; Sb, 0.26 ; As, 0.065 ; insoluble, 1.15 per cent. ; Ag, 26.7 ; Au, 0.04 oz. per ton. For such a test it is essential to select a chemically uniform piece, other-

Jan 1, 1905

By H. De Cizancourt

The Pechelbronn (Alsace) field is the only important French producing field. During 1934, development was carried on as in previous years. The total output of this field reached 553,575 bbl. in 1934, showing a slight decrease from the 1933 figures. Of the total, 315,000 bbl. (56 per cent) was extracted by drilling, while 238,875 bbl. (46 per cent) was obtained by means of shafts and galleries. Exploration of deep Jurassic and Triassic horizons was still in progress at the end of 1934. A deep well reached the Upper Triassic at a depth of 34 m. (2736 ft.). (Information kindly supplied by M. S. Mena, Directeur Technique.) As mentioned before, the small Gabian field (Herault) is gradually being exhausted. No drilling operations were undertaken in 1934, the small production being restricted to the pumping of old wells. Two exploration wells, noted as "drilling" at the end of 1933, were completed in 1934; viz., Lavelanet (Ariége) at 3785 ft. and Santenay (Niévre) at 2578 feet. French Possessions Algeria.—No drilling at Tliouanet. Out of a total of 100 wells drilled in the area, only 8 are still producing. No exploration work is reported during 1934 in Algeria. Tunisia.—Two wells completed; one well drilling at the end of 1934. A total of 11 wells is reported to have been drilled before the beginning of 1935; out of these, 8 were completed before the present program was begun. Morocco.—Exploration work progressed actively last year. The outstanding event was the coming in of Ts. 26 well at 1243 ft. This well took fire, therefore great difficulties were encountered in the accurate measurement of initial production; the figure of 1500 bbl. of oil given here is a near estimate. Oil flowed accompanied by a great amount of water. The apparent decrease of drilling operations in 1934 is explained by the increase in field activities after the results of Ts. 26 were known;

Jan 1, 1935

By C. F., Christopher

The purpose of any steel-making process is to convert the two raw materials iron and scrap into steel. The chemical analysis of the steel is set within certain limits which involve the physical proper- ties desired by the consumer. In addition to tensile properties a large number of other properties are at the present time desired, such as impact resistance, grain size regulation, specific degrees of hardenability, resistance to creep at high temperatures, resistance to expansion on heat treatment, the ability of the product to undergo extreme amounts of cold deformation without failure, and many other properties which are not directly related to the specified chemical analysis. Variations in many of the properties of plain-carbon steels are due to elements and compounds not included in the ordinary "five element"§ composition. Such variations result primarily from variations in oxidation of the metal in the furnace and from the deoxidation method employed. The steel-making problem therefore resolves itself into two distinct sections: (I) the elimination of certain elements from the charge (the iron and scrap entering the furnace) and the addition of materials to meet the chemical specifications for the heat; (2) the manipulation of the slag and metal and the process of deoxidation to give certain desired properties in the steel entirely apart from the chemical analysis specified. Each of 'these two ends must be attained

Jan 1, 1957

By AIME AIME

Award of a Gold Medal : to the Institute. The Jury of Awards of the Jamestown Ter-Centennial Exposition has conferred a gold medal, the highest distinction within its power,. on the American Institute of Mining Engineers for the excellence of its publications during the past decade. ; A half-tone photographic reproduction of both sides of the medal is given in the accompanying illustration.

Jan 7, 1908

By Oscar H. Hershey

COMPLAINT has been made that in the literature of economic geology the work of the "company or practical" mining geologists does not get enough attention. I propose to attempt to overcome this com¬plaint in reference to one important lead-mining district, that of the Coeur d'Alene in northern Idaho. Furthermore, I will assume that the reader is not so much interested in the geology of the district as in the methods of application used and incidents that have arisen in the work. All the important discoveries of ore in the Coeur d'Alene were made without benefit of geology. Certainly I would not claim the reputed discoverer of the Bunker Hill mine as a fellow geologist. It appears also that the mines were operated quite successfully for many years without geological specialists, though doubtless certain properties were visited at long intervals by such men as Waldemar Lindgren. It was known that the ores occur in quartzite, graywackes and slates as stated by J. R. Finlay in 1903. (TRANS., VOL. 33.) He described the ore as occurring in typical fissure veins that occupy fault-planes of indeterminate displacement. The Bunker Hill lode was based on a definite fissure with the mineralization all on the hanging-wall side, extending as far as 300 ft. from the fissure.

Jan 1, 1933

By AIME AIME

ON MAY 22 the American Institute of Mining and Metallurgical Engineers will commemorate the sixtieth anniversary of its founding at Wilkes- Barre, Pa., in May, 1871. The Directors have transferred the May meeting of the Board to Wilkes-Barre, and the Pennsylvania Anthracite Section has invited as many members of the Institute as can to be present at this time and to join with their fellow-engineers at Wilkes-Barre in the inspection trip through a portion of the anthracite district that has been planned. Ac- cess to Wilkes-Barre is easy, from nearby points, over excellent automobile roads, or by train. The distance from New York is only about 140 miles. , It is hoped to engage a special car for those travelling by train from New York, which will leave the Pennsylvania Station over the Lehigh Valley Railroad at 11:50 p.m., arriving in Wilkes-Barre the next morning. Return can be made from Wilkes-Barre by sleeper the same evening, arriving in New York Saturday morning. Other trains are available for those who prefer a daylight journey.

Jan 1, 1931

By H. Kazemi, G. W. Thomas, M. S. Seth

The double-porosity model of Warren and Root7 for examining pressure drawdown and buildup phenomena in naturally fractured reservoirs has been extended to intetpret interference test results. Both analytical and numerical solutions are presented. The practicality of some of the assumptions in the Warren-Root model was also investigated. The standard procedure for interpreting interference tests in naturally fractured reservoirs beretofore employed an equivalent homogeneous reservoir model. A comparison of our results with the equivalent homogeneous model indicates the latter is inadequate for early time responses. For late time responses, however, the simpler equivalent homogeneous model yields favorable results. Finally, the effects of well spacing and the magnitude of the interporosity flow parameter are briefly cited. INTRODUCTION Interference tests can be used to provide reservoir information not obtainable from conventional pressure drawdown and buildup tests. The technique involves measuring the response in one or more wells arising from a pressure perturbation introduced into another well. It has been. successfully applied to single-layer, homogeneous, unfractured, isotropic and anisotropic formations to arrive at values of well storage capacity and a measure of directional permeability.l The techniques of interference testing usually can be extended to heterogeneous systems, provided the permeability contrast between any existing rock layers is not excessive.9 In such cases, the practical interference effects in an observation well of an interconnecting heterogeneous reservoir can be predicted using an equivalent homogeneous model. The calculated properties are then average values. Russell and Prats2 have demonstrated the utility of this approach for a single-phase, two-layer system. For naturally fractured reservoirs, some different approaches usually are necessary. The major departure from homogeneous or nearly homogeneous reservoir treatment is to characterize the fractured system as an entity having "double-porosity"; namely, we suppose the existence of both primary and secondary porosity, where the former is contained within a systematic array of identical rectangular matrix blocks and the latter is contained within an orthogonal system of continuous, uniform fractures (see Fig. 1). It is sufficient to assume that the permeability of the rock matrix is so small that movement of reservoir fluids to the producing wells is entirely through the fracture network. This assumption has been validated by Barenblatt3 and .employed by others?-7 Warren and Root7 used the double-porosity model to develop an interpretation of pressure drawdown and pressure buildup tests in naturally fractured

Jan 1, 1970

By AIME AIME

THE climax of the various programs and entertainments in connection with the holding of the World Engineering Congress* in Tokyo in October was the complimentary dinner given by the visiting members of the Institute to our members in Japan. At the same time President Bradley conferred an honorary membership on Baron Takuma Dan, the vice-president of the World Engineering Congress.

Jan 1, 1930

[Executive J. V. W. REYNDERS, Chairman WILLIAM H. BASSETT E. DEGOLYER I-I. C. BELLINGER RICHARD PETERS, JR. Finance GEORGE OTIS SMITH, Chairman H. A. GUESS F. JULIUS FOHS Admissions GEORGE D. BARRON, Chairman DAVID LEVINGER P. A. MOSMAN H. K. MASTERS J. A, SINGMASTER Alternates F. G. BREYER C. W. HAMILTON F. E. PIERCE]

Jan 1, 1928

By H.A. Bedworth

AlloTs of copper and silicon have been known for one hundred years or more but the commercial development of this type of alloy has taken place during the past few years. In 1905, Sperry l proposed the use of copper-silicon alloys for springs and other purposes for which copper-tin bronzes were used. Some attention was given to this proposal at the time but no one succeeded in producing a practical alloy containing more than a fraction of a per cent. of silicon. The equilibrium relations of the copper-silicon system were studied first by Rudolfi2 and later by Sanfourche 3 and Corson. 4 The constitution of the system has also been recently investigated by Matuyama, 5 and in the laboratories of the American Brass Co. by Smith. 6 Some of the physical properties of the copper-silicon alloys have been investigated by Norbury7 and by Geiss and Van Liempt.8 Summarizing the results of various investigators of the constitution of copper-silicon alloys, the solubility reaches its maximium value, 6.7 per cent. silicon, between 721" and '782" C. At 852" (1. the solubility is 5.25 per cent., while at 400" C. it is only 4.1 per cent. silicon. The copper-silicon alloy begins to get so hard at about 3 per cent, silicon that it is difficult to manage. It was found by Jacobs that the addition of manganese to this alloy considerably improved the working

Jan 1, 1929

By H. A. Bedworth

AlloTs of copper and silicon have been known for one hundred years or more but the commercial development of this type of alloy has taken place during the past few years. In 1905, Sperry l proposed the use of copper-silicon alloys for springs and other purposes for which copper-tin bronzes were used. Some attention was given to this proposal at the time but no one succeeded in producing a practical alloy containing more than a fraction of a per cent. of silicon. The equilibrium relations of the copper-silicon system were studied first by Rudolfi2 and later by Sanfourche 3 and Corson. 4 The constitution of the system has also been recently investigated by Matuyama, 5 and in the laboratories of the American Brass Co. by Smith. 6 Some of the physical properties of the copper-silicon alloys have been investigated by Norbury7 and by Geiss and Van Liempt.8 Summarizing the results of various investigators of the constitution of copper-silicon alloys, the solubility reaches its maximium value, 6.7 per cent. silicon, between 721" and '782" C. At 852" (1. the solubility is 5.25 per cent., while at 400" C. it is only 4.1 per cent. silicon. The copper-silicon alloy begins to get so hard at about 3 per cent, silicon that it is difficult to manage. It was found by Jacobs that the addition of manganese to this alloy considerably improved the working

Jan 1, 1929

By C. M. Smith

DELEGATES from 26 Local Sections and- Divisions of the Institute had three stimulating sessions during the Annual Meeting, a few topics still remaining to be discussed after the two Monday sessions.. The final session was held on Thursday morning. An abstract of the discussion will be transmitted to each delegate present. The topics included: Student relations. Section operation, membership, employment, MINING AND METALLURGY, a new nonmetallic minerals Division. licensing of engineers, and increased allotments of money to Local Sections. Some of the Sections felt that the present limit of $250 allotted to them - from the national treasury was insufficient to carry on their activities, and that this maximum should he increased. A resolution to this effect was passed for transmission to the Board of Directors.

Jan 1, 1935

By F. E. Lathe, L. Hodnett

This paper summarizes extensive data supplied by 40 copper converter plants in 18 countries, and includes a partial analysis and comments on the effect of converter slag composition and temperature on the fomzation and elimination of magnetite and the life of basic and neutral refractories. APRELIMINARY draft of this paper, including data from 26 companies which had submitted replies to a questionnaire, was presented at the Annual Meeting of the AIME held in New York in February, 1956. Publication was delayed in the expectation that additional replies would be received, and justification for the subsequent delay may be found in the fact that the present revised paper contains data from 40 converter plants situated in 18 different countries. The suggestion that a questionnaire be sent to the major copper and copper-nickel plants outside the U.S.S.R. and associated countries arose at the Los Angeles Annual Meeting in February, 1953, where several papers dealing with converter construction and operation were presented. In private discussions which followed, a group of metallurgists and refractories engineers raised the question why practices varied so much at different plants. Why did magnesite brick give superior service to chrome-magnesite in some plants but chrome-magnesite prove superior in others? Would metallurgical studies point the way to the development of still better refractories? Could magnetite formation be prevented in converter slags and reverber-atory furnace mattes? If this was feasible, why was a heavy circulating load of magnetite tolerated, when, in all probability, it increased copper losses in the reverberatory slags and, in some cases, made it necessary to shut down the furnaces periodically to clean out the accumulated magnetite? Was the sole purpose of coating brick with magnetite that of

Jan 1, 1959

Who's Who in Mineral Engineering - The 1979 Directory of the Society of Mining Engineers of AIME

Jan 7, 1979

Division of Geology, State of Tennessee, 401 Seventh Ave, North, Nashville, Tenn. Walter F. Pond, State Geologist A selected list of Bulletins available: Bulletin 1(B), Bibliography of Tennessee geology (1911); 2(A) Outline introduction to mineral resources (1910), 2(D) Marbles (1911); 2(G) Zinc deposits (1910), 16, Red iron ores of east Tennessee (1913), 22, Geology and natural resources of Rutherford County (1920), 24(A) Geology and oil possibilities of parts of Overton, Clay, Pickett and Fentress counties (1920); 24(B) Oil and gas resources of northeastern Sumner County (1920), 26, Mineral resources of Waynesboro Quadrangle (1921); 28, Marble deposits of East Tennessee (1923), 29, Magnetic iron ores of east Tennessee (1923), 31, Zinc deposits of east Tennessee (1923), 33, Tennessee coal fields, 37, Geology and mineral resources of Hardin County, 38, Stratigraphy of the Central Basin (in press), 39, Brown iron ores of the Eastern Highland Rim (in press) From 1911 to 1919, inclusive, volumes were issued annually on The Resources of Tennessee Only a few of the separate papers contained in those volumes are now available Vol. 2 (1911): No 1, Explosions of coal dust in mines, and other papers, No. 4, Lignite and lignitic clays in west Tennessee, and other papers; 5, The growth of knowledge of Tennessee geol¬ogy; 9, The valley and mountain iron ores of east Tennessee, 10, The iron industry of Lawrence and Wayne counties, and other papers; 11, Barite deposits in the Sweetwater district, and other papers, 12, The iron ore deposits in the Tuckalioe district, and another paper Various oil maps (15 to 40 cents each) and traverse maps of counties (25 cents and 31 each) can be had, as well as pertinent U. S topographic maps.

Jan 1, 1933

By P. Somasundaran, D. W. Fuerstenau

This article presents the results of an analysis of grinding of 1:1 mixtures of 4x8-mesh quartz and limestone in laboratory ball and rod mills. From these experiments, the amount of energy consumed in grinding each component of the mixture was determined. In the ball mill, limestone consumes slightly more energy than quartz in the initial stages of grinding, but as the grinding proceeds quartz begins to consume a slightly greater fraction of the energy. The postulate that the fraction of energy consumed by any material in a ball mill is proportional to its volume fraction has been shown to be approximately true. On the other hand, in a rod mill energy consumption by quartz and limestone is equal only in the initial stages of grinding, with energy consumption by quartz greatly exceeding that by limestone as rod milling proceeds. Preferential energy consumption in tumbling mills has been discussed in a number of papers. For example, from an analysis of the kinetics of comminu- tion in ball mills, Arbiter and Bhrany' obtained rate equations based on the postulate that only coarse particles are ground, indicating that fine particles are protected from the action of the balls by coarser particles. In rod mills this protective action is much more pronounced than in ball mills. Recent studies on the rod milling of limestone-quartz mixtures have shown that this protective action causes the mineral with the lowest grindability (quartz in this instance) to consume the greater fraction of energy. 2 However, in the ball milling of mixtures it has been postulated that the consumption of energy by one of the constituents is determined by its volume fraction within the mill. 3 Possibly this hypothesis may be a simplification of the ball milling of mixtures since the protective action suggested by Arbiter and Bhrany may result in some preferential energy consumption by one of the constituents of a mixture. The objective of this study has been to determine preferential energy consumption in laboratory ball and rod mills by analyzing size distributions of each material in the products obtained from grinding 1:l mixtures of quartz and limestone. MATERIALS AND METHOD The procedure for carrying out the tests on wet grinding quartz-limestone mixtures has already been described.'r3 In the present investigation, 1:l mix-

Jan 1, 1963

By B. A. Kulp, R. R. Reeber

Lattice parameters for the wurtzite form of' CdS mere measured by powder X-ray diffraction techniques over the temperature range 26° to 1000 K'. A negative thermal -expansion coefficient was determined parallel and perpendicular to the c axis below 13.5°K. Near 808°K, the curves of the a, parameter, the differential thermal expansion, and the resistivitv vs absolute temperature exhibited a reversible discontinuity. j\. direct determination of the lattice parameters of CdS over an extended temperature range is of particular use in interpretation of the effects of high pressure on the band structure of semiconductor materials. For example, Langer' has studied the effects of pressure on the absorption edge of CdS from 77°K to room temperature. In order to properly interpret his results it is necessary to know the change in lattice constants as a function of temperature for the wurtzite, zincblende, and rocksalt2 modifications of this material. Thermal-expansion measurements for CdS, wurtzite phase, have previously been determined over a limited temperature range.s74'5 The zincblende phases, of other compounds with similar bonding, have been investigated by Novikova et a! .'' Previous thermal-expansion measurements for metals with hexagonal symmetry have for the most part used bulk sample techniques for low-temperature result. Most X-ray measurements at low temperature have been on materials with cubic symmetry.'jQ The use of X-ray powder-diffraction techniques offers a convenient and accurate method of measurement over a wide temperature range. The X-ray method, besides measuring unit cell size, also provides information about change in structure type and the nature of some of the stacking defects present. I) EXPERIMENTAL PROCEDURE The thermal expansion was measured by X-ray powder-diffraction techniques. Lattice parameters for the range 300" to 1000°K were determined in a 19-cm Unicam camera. From 26" to 300°K a 34-cm back-reflection camera with the Van Arkel" film arrangement was used. The sample was bonded to a copper cold finger below a helium, hydrogen, nitrogen, oxygen, dry ice, or ice brine bath in a metal cryistat. che inner bath was surrounded by another one for radiation shielding. Nitrogen was used in this outer bath for the very low-temperature runs while dry ice and acetone was used for the 195°K point. CuKa X-rays, filtered with a nickel foil, entered the cryostat through a 0.001-in.-thick aluminum window. During a typical 9-hr exposure the sample was continuously rotated through a 30-deg arc. Heat losses from the sample holder limited the minimum temperature attained to 26°K with helium in the inner dewar. Temperature calibration between 25" and 125°K was determined with an Allen Bradley 300-ohm carbon resistor. The resistor was attached to the back of the copper finger with a thin layer of silicone grease. Liquid He, HZ, N2, and O2 baths were used to calibrate the resistor. Temperature variation is estimated to be *2"K with a slightly higher uncertainty at room temperature and 264°K. The thermal expansion of high-purity germanium from 373" to 900°K was measured as a calibration for the Unicam camera. This value was compared with the known value1' for the thermal expansion. A discontinuity in the thermal-expansion coefficient of the CdS a, parameter was observed. Similar discontinuities in the resistivity and differential thermal analysis at the same absolute temperature indicate that the temperature error is *5°K in the temperature range above 500°K. Temperature errors in the Unicam camera below 500°K are appreciably higher due to large gradients in the resistance furnace. II) SAMPLE PREPARATION The CdS was Eagle Picher ultrapure grade. The crystallite size range of the as-received powder

Jan 1, 1965