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By L. B. Ticknor, M. B. Bever

An isothermal calorimeter suitable for measurements of heats of solution in liquid tin as solvent is described. Measurements of the heats of solution of gold, silver, copper, and a gold-silver alloy are reported. The heat of formation of this gold-silver alloy is also reported. HEATS of solution in liquids can be determined directly, but few such data have been published for metals as solvents. Knowledge of heats of solution is desirable because it contributes to the general understanding of energy relations in metallic solutions. Thermochemical measurements of this type also furnish answers to specific problems: For example, from the heats of solution of an alloy and of a mixture of its constituent elements in a given solvent, the heat of formation of the alloy may be found. Similarly, differences in the energy content of samples of the same metal in two different states, such as the annealed and cold worked states, may be determined. In the work reported here, gold, silver, and an alloy of gold and silver were dissolved in liquid tin at 240°C and gold, silver, and copper were dissolved in tin at 300 °C. The experiments yielded the heats of solution of these metals in tin. The heat of formation of the gold-silver alloy was also determined. The same calorimetric method is being used to measure the energy stored in metals during cold working and preliminary results have been published.' Equipment and Experimental Procedure The isothermal calorimeter used in this work, Fig. 1, consisted of a Dewar flask completely immersed in a constant-temperature salt bath. A long neck provided space for thermocouple leads and a stirrer shaft and permitted the injection of solute samples. The metal bath in the calorimeter flask was stirred at about 100 rpm by a small glass impeller driven by a constant-speed motor. The shaft of the stirrer passed through a Wilson vacuum seal.2 All measurements were made under vacuum in order to eliminate temperature disturbances resulting from gas convection and to prevent the oxidation of tin. The calorimeter flask was joined by an all-glass connecting line to a gas-control system which made possible the use of a protective atmosphere of deoxidized and dried hydrogen. At the operating temperature of the calorimeter tin oxide was not reduced by hydrogen, presumably because the reaction rate was too slow. Part of the closed system was a removable side tube through which the solute sample could be introduced and in which it was held at a temperature of 0°C prior to injection into the metal bath. The salt bath containing a mixture of sodium, lithium, and potassium nitrates was similar to that described by Beattie3 and was equipped with a stir-

Jan 1, 1953

By AIME AIME

MEXICO embraces one of the great metal and petroleum producing provinces of the world. In this respect its history dates back to the overthrow of the Aztec empire by a Spanish force under Hernando Cortes between 1519 and 1.521. Even before then, its richness in silver and other minerals was not unknown. But it was a treasure house for the Spanish conquerors until the country became independent in 1821. It has been computed that in the 400 years following 1521, Mexico yielded 1.55,000 metric tons of silver, worth $3,000,000,000, two-thirds of the entire world production. In 1935 the country accounted for 36 per cent of the world's silver output, 14 per cent of its antimony (in 1934), 13 per cent of its lead, 3 per cent of its zinc and copper, and 21/2 per cent of its petroleum. Contrary to the impression of some, its gold output is now comparatively small, though important in the past. Its oil, as well, formerly hulked much larger than now, in 1921 being one-fourth of the world output.

Jan 1, 1936

By J. B. Cohen, M. B. Beaver, R. J. Black

RECENT investigations have shown that face-centered cubic metals may deform by twinning. Blewitt, et al' found that at 4.2"K the mode of def~rmation of single crystals of copper changed at large strains and markings formed on (111) planes. Later they- emonstrated by X-ray diffraction and metallography that the markings were twins and showed that favorably oriented single crystals of copper deformed by twinning at 78°K. They also observed twinning in silver and gold deformed at 4.2 and 78°K. Wagner3 obtained evidence for twinning from the peak shape of diffraction lines of silver cold-worked at 78°K, but twins small enough to cause such effects are not likely to be detected metal-lographically. In the work reported here lamellar structures were observed in deformed silver-gold alloys. They appeared to be mechanical twins, but metallography could not establish this conclusively. Their tendency to form depended on strain rate, temperature and composition. Specimens of silver-gold alloys (0 to 83 wt pct Au) were deformed plastically. One set was worked by hammering under liquid nitrogen, at room temperature and at intermediate temperatures. Another set was compressed slowly in liquid nitrogen to the same reductions as those produced by hammering. Tensile specimens (0.015 x 0.120 x 1.5 in.) of various compositions and approximately equal grain size (0.011 to 0.016 cm) were tested at -195°C and at room temperature. In microsections of all specimens deformed by hammering at —195°C thin lamellae appeared, Fig. 1. They were aligned in definite directions in each grain. In some grains they had two orientations. Where lamellae intersected, a displacement was apparent. Near the center of the left margin of Fig. 1 shear has taken place beyond the fully developed intersecting lamella. Many lamellae resembled Neumann bands in alpha iron. They were parallel to one side of triangular etch pits in the matrix (as in Figs. 1 and 2). The individual lamellae were narrow and had little substructure. This suggested that they did not result from concentrated local slip. The shape of etch pits within the lamellae differed from that of pits in the matrix, as can be seen in Fig. 2; this indicated a difference in orientation. Specimens slowly deformed at —195°C contained regions in which the lamellae were clustered. In these specimens some lamellae were bent and presumably had formed before the termination of the deformation. Structures of greater width than the lamellae were also seen.4 More lamellar structures formed on impact than during slow compression to a given reduction. This was true of all compositions. The structures became less abundant with increasing temperature of deformation. None was observed after extension to fracture at room temperature, but they could be pro-

Jan 1, 1959

By B. H. Kear, S. M. Copley

Stress-stvain curves are presented for Ni3Al (y') cvystals in several ovientations, deformed in tension and compression at constant displacement rate, at temperatures from 70° to 2000°F. Both the yield stress and wovk havdening increase with temperature, with the magnilude of the effect dependent on ovientation. The yield stress maximum occurs at 1500°F in [001], at 1400°F in [011], and at 1200°F in [111]. The suppression of the yield stress peak in [011] and [111] orientatiorzs is due to the onset of cube slip, rather than octahedval slip, a1 elerated temperatures. The temperature and orientalion dependence of work hardening in nominal single slip orientations corvelates with changes in the CRSS ratio for octahedral slip and cube slip, in agreement with a model for work hardening based on pinning of screw dislocalions by cross slip from an octahedral plane into a cube plane. It is concluded that the unique plastic properties of y' have a decisive influence on both ductility and strength characleristics of y +y' nickel-base superalloys. It has long been recognized that the strength of y + y' nickel-base superalloys depends on the precipitation of the y' phase [basically Ni3(Al,Ti)]. This paper presents new data on the strength characteristics of single crystals of simple y' (Ni3Al), and forms the first step in a systematic program aimed at elucidating the mechanisms of hardening in the complex commercial alloys. 1) EXPERIMENTAL PROCEDURE Single crystals of off-stoichiometric NiA1 were grown from the melt under vacuum by a modified Bridgman method. The melt was poured into a preheated alumina mold and crystal growth was promoted from one end by gradient cooling. The crystals were homogenized by annealing in hydrogen at 2400° F for 72 hr followed by furnace cooling. Chemical analysis of samples taken from several crystals gave an average composition of 88.2 wt pct Ni. Spectrographic analysis gave as the principal impurities in weight percent— Si (0.02), Mg (0.01), Fe (0.02), Ti (0.002), Cu (0.008), and Co (0.03). Tensile specimens with specifications as in Fig. 1 were prepared by a series of operations involving electrical discharge machining, precision grinding, and electropolishing. Compression specimens with dimensions 1/4 by 1/4 by -3/4 in. were prepared in a similar manner, except for the initial shaping operation using a precision cut-off wheel/two-circle goniometer unit to give selected crystal orientations. Specimens were deformed in a Baldwin-Wiedemann testing machine with furnace attachment, using a strain rate of 5 x 10-4 sec-1. The strain measuring device consisted of extension arms attached to the tensile grips (or compression plattens) at one end and leading out of the furnace to an LVDT at the other. Temperature was controlled by a thermocouple placed in contact with the specimen. According to the known phase diagram for the Ni/A1 system,' when an alloy of the specified composition is cooled from the melt, primary y (nickel solid solution) dendrites grow at the expense of the liquid phase, which becomes enriched in aluminum. At the eutectic composition the remaining liquid freezes as a two-phase mixture of y + y' (Ni3Al). Upon further cooling, a solid state transformation occurs, involving the precipitation of y' in the primary dendrites, and the complete transformation of the eutectic mixture to massive y'. The as-cast structure consists, therefore, of y + y' dendrites with interdendritic regions of massive y', i.e., transformed eutectic, Fig. 2. 2) DISCUSSION OF RESULTS 2.1) Stress-Strain Curves. Fig. 3 shows tensile stress-strain curves for crystals in orientations close to [001] deformed at temperatures from 70° to 2000°F. Both the yield stress and total elongation are strongly temperature-dependent. At 70°F, easy glide is absent, and the work hardening coefficient BIT - G/300. At T > 1500°F, the negative slope of the stress-strain curves is due to pronounced necking in the crystals. The yield stress maximum at 1500° F corresponds with a minimum in the ductility, Fig. 4. The extensive duc-

Jan 1, 1968

EXECUTIVE COMMITTEES OF LOCAL SECTIONS Arizona E. P. MATHEWSON, Chairman W. V. DECAMP, First Vice-chairman F. W. MACLENNAN, Second Vice-chairman E. D. GARDNER, Secretary-Treasurer, U. S. Bureau Of Mines, Tucson, Ariz. MICHAEL CURLEY J. P. HODGSON HENRY F.1 ASTER CLYDE E. WEED Boston Meets first Monday each winter month GEORGE A. PACKARD, Chairman FRANKLIN B. RICHARDS, Vice-chairman F. LEROY FOSTER, Secretary-Treasurer Rooms 8-219 Mass. Inst. of Tech., Cambridge, Mass. G. W. METCALFE D. H. MCLAUGHLIN

Jan 1, 1932

By Charles H. Fulton

THE Engineering Education group began its sessions Tuesday morning, Feb. 16, as a Committee and wound up the day as the Institute's fifth " Division." C.II. Fulton presided. The first paper for discussion was entitled "Teaching Management in Engineering Schools,"' by Eugene McAuliffe, president of the Union Pacific Coal Co., space for which may be found later in these pages. In it, Mr. McAuliffe argued that an engineering student should be taught the knowledge of men, much as a medical school teaches surgery. He then went on to indicate, out of the wealth of his administrative experience, the problems an executive needs to be equipped to handle, and said that every student engineer should look on himself as a potential manager.

Jan 1, 1932

By George H. Deike

DURING the past year a survey was conducted by the Committee on the Promotion of Student Interest in Coal Mining to determine whether the program as laid down in past years was operating effectively. It is a source of satisfaction and pleasure to be able to report considerable headway among operating companies in putting cooperative scholarship plans into operation. In previous committee reports the pioneer work along this line by Eugene McAuliffe, president of the Union Pacific Coal Co., has been cited. That Company now has in its employ, in responsible positions, three men who received their education under such scholarship plans. One student under a similar plan is now studying at the Colorado School of Mines.

Jan 1, 1942

SAN FRANCISCO SECTION T. A. RICKARD, Chairman W. H. SHOCKLEY, Vice-Chairman C. E. GRUNSKY, JR., Secretary-Treasurer, 57 Post St., San Francisco, Cal. E. A. HERSAM H. W. YOUNG. A meeting of the San Francisco Section was held at the Engineers' Club of San Francisco on Mar. 28, 1916. Dr. Bailey Willis, Head of the Geological Department of Stanford University, read a paper on The Relation of the Major Structural . Features of the South American Continent to the Mineral Districts. Vice-Chairman Shockley interested the Section with an account of his experiences in South America. Discussion was participated in by C. F. Tolman, Jr., A. C. Lawson, Frank Probert, and E. A. Hersam. C. E. GRUNSKY, JR., Secretary.

Jan 5, 1916

(Members are urged to send in for this column any notes of interest concerning themselves or their fellow-members.) Members and visitors who registered at Institute headquarters during November: George W. Otterson, Mauson, B. C. Roy H. Allen, Chihuahua, Mexico. E. L. C. Ayres, Bound, Brook, N. J. George A. Packard, Boston, Mass. M. Russell, Bound Brook, N. J. Richard C. Patterson, Jr., Kansas City,,Mo. Carlo Spruyt, Antwerp, Belgium. Francis C. Phillip, Pittsburg, Pa. Charles A. Pringle, San Francisco, Cal. M. H. Kuryla, Mexico City, Mexico. E. S. Bardwell, Great Falls, Mont. Arthur Chippendale, Mexico City, Mexico. Sir Robert Hadfield, London,, England. F. Danvers Power, Sydney, Australia. James A. Barr, San Francisco, Cal..

Jan 12, 1913

By Paul F. Kerr

The insufficiencies of our mineral resources are becoming well known, and the national political conscience seems to be troubled at last by our dependence upon mineral commodities which must come from other lands. This realization places increased responsibility upon the industrial, educational, and governmental groups whose task it will be to solve the problems of mineral supply. As we all know, from the time that man first sought mineral deposits until recent years, prospectors have been largely responsible for mineral discoveries. Today the era of the prospector is almost over. The human ants that have literally examined all accessible outcrops and have tested the gravels of nearly all stream beds in the United States have left undiscovered few worthwhile mineral deposits within the scope of their recognition. The pages in the history of mineral exploration are now being turned from the era of the surface prospect to the era of the hidden de- posit.

Jan 1, 1949

By F. L. Bosqui

NO metallurgical process developed in the last half century has been more widely advertised to both technologists and lay- men, or has done more to promote efficiency and economy in the extraction of the valuable portions of ores than has the flotation process. Practically everybody has heard of this strange procedure whereby the heavy portions of an ore are made to float while the light parts sink. Some- times it is called froth flotation, the mineral-bearing froth being from the first a distinguishing characteristic. Many times it is called oil flotation, because a thin film of oil was commonly applied to the particles to be floated to make them adhere to the bubbles that rise through the pulp to form the surface froth. Oil, though commonly used, is not, however, necessary for this purpose, which is one of the facts that has been learned as the process has been developed.

Jan 1, 1940

By AIME AIME

THE Institute of Metals held a well rounded out symposium on the working of metals, distributed over two sessions. At the first session* four papers were presented, two dealing with the, cold working of metals and alloys and two with the hot working of non-ferrous alloys. The first paper by E. V. Crane, dealt with "Metal Working in Power Presses." Mr. Crane pointed out the empirical nature of engineering data available for use in calculating the probable stresses developed and power requirements, for the shearing, drawing, binding and other forming operations. He described the various operations, methods of determining stresses developed and presented data obtained. In the discussion C. F. Hammond took exception to Mr. Crane's objections to the rather too frequent. annealing operations in drawing of cartridge cases, pointing out that the material was-manufactured to meet specified structure and physical requirements, which could only be met by carefully controlled sequences of working and intermediate annealing operations.

Jan 1, 1931

By AIME AIME

The following acts of the Directors are reported for the information of members:¬ At a meeting held November 3, 1905, Messrs. Henri Le Chatelier, of Paris, France, and Andrew Carnegie, of New York, N. Y., having been nominated by a large number of members, and recommended by unanimous vote of the Council, were unanimously elected Honorary Members, in recognition of their distinguished services to the arts and professions represented by the Institute. At a meeting held February 7, 1,906, Dr. James Douglas, of New York, N. Y., having been" nominated by a large number of leading members, and recommended by unammous vote of the Council, was unanimously elected an Honorary Member, in recognition of his distinguished services to the practice and the literature of mining and metallurgy, his zealous and loyal devotion to this Institute, his fraternal generosity towards professional colleagues, and his effective advocacy, by public utterance and private example, of the free communication of technical knowledge and experience. At the same meeting, By-Law IV., which now authorizes the Secretary to appoint an '1 Assistant Editor," was amended by substituting the words, " Assistant with the title of Editor." At the same meeting, the resignation of Mr. Theodore Dwight, as Assistant Secretary and Assistant Treasurer of the Institute, was presented and accepted, and the Secretary was instructed to express to Mr. Dwight the thanks of the Board for his loyal and efficient services, and its regret that he could not continue in that position. . [SECRETARY'S NOTE.-Mr. Dwight's resignation, dictated solely by the demands of private business, covers only his immediate management of this office. He is still a Director and Councilor, and a representative of the Institute in matters connected with the new Carnegie Building, etc.-R. W. R.] At the same meeting, the Secretary and the Treasurer reported respectively their appointment of Mr. Henry WT. B. Howard as Assistant Secretary and Assistant Treasurer, to fill

Mar 1, 1906

By ALEXANDER S. CORSUN

THE main orebody in the Hecla mine, Burke, Ida- ho, occurs along a nearly vertical shear zone in the Burke quartzite, with a substantial gouge and lamprophyre dike occurring in an irregular manner throughout the lode. The veins range from 3 to 40 ft. wide and dip from 70 deg. to 90 deg. There is 110 definite line of demarcation between the lode and the wall rock. Stringers of ore are often found in the wall rock for irregular distances. Horizontal but irregular quartz stringers are also found running into the walls and positions of the wall have a tendency to break to the quartz stringers and the accompanying gouge, which causes indefinite, uneven and extremely heavy side and top pressures.

Jan 1, 1930

By J. G. Baragwanath

CUBA'S lateritic iron ores, occurring on the northern coast of that island, though known to the Spaniards. did not receive any general attention until the close of the Spanish-American War. Preliminary studies of these deposits at that time indicated that the limonite contained small percentages of nickel and chrome, and it ryas subsequently discovered that although the average nickel content was only approximately 0.6 per certain limited areas of ore were suffiniently high in nickel to be considered commercial provided a suitable process fur its recovery could be developed. Early in 1937, Pardners Mines Corp. began a series of investigations which led to the development of such a process. Coincidentally, this company acquired option' on certain properties in the Levisa Bay and Moa Bay regions and conducted a systematic campaign of exploration by test pits and hand-auger holes in the course of which an aggregate of 90.000.000 tons of ore was developed in eight deposits.

Jan 1, 1945

By Sydney H. Ball

MINERALS used primarily for personal adornment and decorative purposes are called precious stones. To be so prized, the stones must possess beauty of color, must not be too common, and must be hard enough to withstand ordinary wear. If transparent, they must have brilliancy and fire. Almost one hundred minerals have been used as precious stones, the noble gems being the diamond, emerald, ruby, and sapphire; pearls are frequently included by courtesy. These gem stones, however, are sometimes equaled in beauty by fine opals, aquamarines, ourmalines, spinels, chrysoberyls (both cat's-eye and alexandrite), and spodumenes (hiddenite and kunzite). The Greeks, Romans, and medieval Europeans grouped together gem stones according to color and degree of transparency, and only as the niceties of mineralogy began to be known, about a century ago, was it realized how many different minerals have the beauty required of gem stones. Pliny, for example, did not distinguish between rubies and the red varieties of spinel and garnet, although he conjectured that the beryl and emerald were one mineral. GENERAL SURVEY Early man treasured bright colored berries, attractive shells, white teeth of wild animals and brightly colored pebbles, and used them as personal ornaments. In the eastern hemisphere, the earliest stones used were members of the quartz family (100,000 to 75,000 B.C.); then obsidian and amber (50,000 to 25,000 B.C.); the jade minerals, fluorspar and jet (22,000 to 7000 B.C.); turquoise (7000 to 3400 B.C.); lapis lazuli and garnet (prior to 3500 B.C.) ; emerald (2000 to 1800 B.C.) ; sapphire, ruby and diamond (800 to 500 B.C.). Indeed, gem mining is the oldest form of mining, and before any metals were known primitive man recognized about 18 gems and decorative stones. At first he sought them in stream gravels and residual deposits but by 3400 B.C. the turquoise mines of the Sinai Peninsula were operated. This was the world's first important hard-rock mining enterprise. The Afghanistan lapis lazuli mines may

Jan 1, 1949

By AIME AIME

WEDNESDAY night, by long tradition, is al- ways set aside for the annual dinner, even when, as it was this year, it is Ash Wednesday. Whether the somewhat smaller attendance than last year is attributable to that cause, the unexpectedly long persistence of business depression, or whatever may have been the reason, it was a joyous occasion, and the grand ball-room of the Commodore Hotel was as completely filled With diners as * was consistent with com- fort. In the half hour before the dinner was actually served the guests assembled in an adjoining room and not only exchanged greetings but proceeded along the receiving line to greet the guests of honor. The number present was so large that hardly more than half of them had been able to do this before the summons to the dining room sounded and a hearty and immediate response was made to it. Toy balloons at each plate, inflated and directed at the heads of companions or nearby friends, but which were just as likely to carom from the nose of a hurrying waiter, successfully broke the ice as well as not a few plates. It would be interesting to know whether the pleasure the guests derive from these de- vices is in part based on the all-too evident annoyance of the waiters, and what the relative quantitative relationships are.

Jan 1, 1931

By Neil O. Johnson

In the cyanidation of gold, silver and mixed ores, the solids, suspended in the pulp after fine grinding, primary settling and scries agitation arc subjected to a washing step known, generally, as countercurrent decanta-tion, abbreviated C.C.D The conventional C.C.D. plant consists of a series of separate thickeners—three to five in number—arranged in series on slightly different elevations. Solids settled in the first thickener are pumped at maximum density into the second thickener, where they arc diluted with weak solution overflowing the third. After settling in the second thickener they are pumped to the third, where the process of repulping with still weaker solution is repeated, and so on throughout the system, until they reach the last thickener and are repulped with barren solution or water. Recently there has been developed a new type of thickener, known as the Dorr Washing Tray Thickener, consisting of up to five individual thickeners, which performs in a single unit all the functions of a conven-tional C.C.D plant. Fig. 1 illustrates the essential features. It is a multicompartment tray thickener, in which the trays operate in scries instead of in parallel for countercurrent washing. Feed enters the top compartment via a central, semisubmerged feed well. Strong solution overflows into a peripheral launder. Solids settle to the bottom, are raked to the center and flow into the top of the second compartment, directly below, via an inverted cup and scal. Solids pass downward, compartment by compartment, against a counter flow of wash solution and finally of fresh water. Thus, in accord-:trice with the basic C.C.D. principle, the solids transfer the dissolved metal content to the wash solution and finally are removed by a diaphragm pump from the bottom compartment virtually free of valuable material. Similarly, the wash water, as it flows through the system, becomes increasingly enriched in dissolved metal until it overflows from compartment two and returns to the process.

Jan 1, 1939

By Neil O. Johnson

In the cyanidation of gold, silver and mixed ores, the solids, suspended in the pulp after fine grinding, primary settling and scries agitation arc subjected to a washing step known, generally, as countercurrent decanta-tion, abbreviated C.C.D The conventional C.C.D. plant consists of a series of separate thickeners—three to five in number—arranged in series on slightly different elevations. Solids settled in the first thickener are pumped at maximum density into the second thickener, where they arc diluted with weak solution overflowing the third. After settling in the second thickener they are pumped to the third, where the process of repulping with still weaker solution is repeated, and so on throughout the system, until they reach the last thickener and are repulped with barren solution or water. Recently there has been developed a new type of thickener, known as the Dorr Washing Tray Thickener, consisting of up to five individual thickeners, which performs in a single unit all the functions of a conven-tional C.C.D plant. Fig. 1 illustrates the essential features. It is a multicompartment tray thickener, in which the trays operate in scries instead of in parallel for countercurrent washing. Feed enters the top compartment via a central, semisubmerged feed well. Strong solution overflows into a peripheral launder. Solids settle to the bottom, are raked to the center and flow into the top of the second compartment, directly below, via an inverted cup and scal. Solids pass downward, compartment by compartment, against a counter flow of wash solution and finally of fresh water. Thus, in accord-:trice with the basic C.C.D. principle, the solids transfer the dissolved metal content to the wash solution and finally are removed by a diaphragm pump from the bottom compartment virtually free of valuable material. Similarly, the wash water, as it flows through the system, becomes increasingly enriched in dissolved metal until it overflows from compartment two and returns to the process.

Jan 1, 1939

By S. Luszcz, R. W. Vook, Fred Witt

In situ X-ray investigations were made on polycrys-talline silver films deposited by vacuum evaporation on (111) CaF2 and (100) NaCl single-crystal substrates at 80°K. The films were evaporated and annealed in an X-ray diffractometer attachment having a residual gas pressure of 2 x lo-' Torr. All measurements were made without exposing the films to the atmosphere. Measurements were made on the films in the as-deposited state and after various annealing treatments. The intrinsic stacking and twin fault densities, the magnitudes of the uniform and nonuniform strains, and the crystallite sizes were determined. In addition the textures in the films were measured qualitatively. The results obtained for the as-deposited films on single-crystal substrates are in substantial agreement with previously reported results for silver films deposited on glass. Intrinsic stacking and twin faults, as well as uniform and nonuniform strains, were present in these films. During the various annealing treatments (up to 350°C) the faults and nonuniform strains annealed out. Considerable grain growth and texture changes occurred also. The effects were much greater for the NaCl substrate than for the CaFz substrate. The relative magnitudes of the grain growth in the variously oriented grains could be explained qualitatively in terms of the thermal strains and strain energies introduced into the differently oriented grains during the initial, irreversible anneal. These strains were due to the different thermal expansion coefficients of the film and substrate. X-RAY diffraction measurements on evaporated films deposited on substrates at low temperature have the advantage that many of the imperfections introduced into the film during deposition are "frozen in". Thus, the influence of a very important experimental variable, substrate temperature, on the imperfection structure of evaporated metal films may be studied. Moreover, the effects of annealing such films makes possible the study of thermally activated recovery processes in these films. The present study was designed to determine the influence of single-crystal substrates on the resultant film structure relative to the previous results obtained using glass substrates.' To this end great care was taken to keep the experimental variables the same in the two cases. Different experimental conditions would, of course, result in films having different physical properties. Again the initial substrate temperature was in the neighborhood of 80°K and the films were subsequently annealed to 350°C. The pure metal silver was chosen for evaporation, primarily because of its relatively low stacking fault energy and consequent high fault density in the as-deposited state. The silver films were formed by evaporation onto air-cleaved {ill} CaF, and (100) NaCl surfaces cooled to 80°K in an X-ray diffractometer attachment2 having a base residual gas pressure of 2 X l0-' Torr. The films were not exposed to the atmosphere until all of the X-ray data had been recorded. In this way one of the most important experimental variables, environment, could be well-controlled and reproduced. X-ray measurements were made at the temperature of deposition and included determinations of the diffraction line peak positions, line shapes, and integrated intensities. The peak position measurements were used to determine the intrinsic stacking fault densities and the average uniform strain in the film. The shapes of the diffraction lines provided information on the twin fault density, true crystallite size, and average nonuniform strain. The preferred orientation in the film was determined qualitatively from the integrated intensities. I) EXPERIMENTAL PROCEDURE The evaporator attachmentZ was charged with 99.999 pct Ag pellets positioned in a tantalum filament which had been outgassed previously at l0-8 Torr. The CaFz and NaCl single crystals were cleaved in air and then placed in position in the chamber so that their cleavage surfaces were on the diffractometer axis. The chamber was prepumped using a sorption pump, sealed off, and then baked at 150°C for 24 hr. The ion pump operated during the bakeout cycle. The substrate was then heated to 500° C by means of an auxiliary heater and kept hot until the rest of the chamber was cooled slowly to room temperature. This bakeout procedure consistently resulted in an ultimate pressure in the low lo-' Torr range. The substrate was then cooled down on 80°K. Its temperature was monitored by a thermocouple wedged into the rear of the copper substrate holder. The diffracted intensity and peak position of the 111, 222, and 333 CaF, lines were measured prior to evaporation. Nickel-filtered, pulse-height-discriminated copper radiation was used. Similar measurements were made for the 200 and 400 lines from NaC1. These measurements were used as a lattice parameter check and to determine the thickness of the evaporated silver films from the attenuation of the substrate lines. The evaporation rates were approximately 3A per sec for both films while the maximum pressures during evaporation were 3 x lo- ' and 7 x 10"8 Torr for the CaF, and NaCl cases, respectively. The film thickness was measured by the attenuation of the CaF, and NaCl substrate lines and by at optical interference method. Values of 1700 and 1500A, respectively, were obtained for the silver

Jan 1, 1969