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By W. A. Tiller, J. P. McHugh

THE phase diagram of the Ge-Te system was first investigated by Klemm and Frischmuth.' They arrived at the phase diagram shown in Fig. 1 indicating the presence of a peritectic phase boundary at the 50 at. pct Ge composition. Later, Schubert and Fricke2 obtained data which suggested to them the possible existence of a eutectic at about 55 at. pct Ge. In order to resolve these differences, we have carefully studied this system in the region 40 to 60 at. pct Ge using both the conventional thermal analysis technique and a new solidification technique.3y4 The alloys were prepared from semiconductor grade germanium and 99.999+ Te by reacting the elements in evacuated, graphite coated, vycor tubes. The samples were placed in a thermal analysis apparatus described elsewhere4 and cooling curves were taken of each alloy to determine the liquidus surface. The cooling curve for a 50 at. pct alloy shows two distinct arrests about 1°C apart which

Jan 1, 1961

By H. I. Aaronson, C. Laird

Cold rolling by 50 pct a A1-4 pct Cu alloy containing many 0' plates has been found to accelerate markedly the transformation of 8' to 0 upon further aging. Although the basic mechanism of this transformation remains unchanged by plastic deformation, the nuclea-tion kinetics of 8 become appreciably more rapid and also less dependent upon temperature. Particularly at lower aging temperatures, rounded idiomorphs replace several faceted rnorphologfes. The rates of growth of 9 idiomorphs in deformed specimens aged at 300°C are appreciably more rapid than simple volume diffusion control allows. This observation is shown to be explained by an excess vacancy, rather than by a dislocation Piping mechanism of growth. ThE rather complex phenomenology of the 8' —8 transformation in Al-Cu alloys has been recently elucidated in considerable detail by means of transmission electron microscopy.'-4 This technique was also employed in the present investigation in order to examine the effects of plastic deformation upon the transformation of 8' to 8. The mechanism of the transformation in undeformed Al-Cu alloys has been established as the following sequence of events.1"4 The first step is the nucleation of 9 at (Y:8' boundaries. Nucleation of a 0 crystal takes place, however, at only a very small proportion of the 8' plates present. Each 0 crystal simultaneously consumes the host 8' plate and the a! in the immediate vicinity, with growth into a being the rate-controlling process. The remaining 8' plates are then dissolved as they fall under the concentration shadow of the growing 8 crystals. The evidence on the effects of plastic deformation upon these processes is intriguing, but much less detailed. The careful X-ray studies of Graf and Guinier have shown that the aging times required to form detectable amounts of 8' and 8 are reduced by prior cold working. Thomas and Nutting confirmed these results by replication electron microscopy. Nile-shwar,* on the other hand, reported that creep deformation decreases the rate of formation of 0. While this difference may have been caused by the use of concurrent rather than successive deformation and ag- ing, the X-ray technique which he used was able to monitor only the 0 phase. It is thus possible that the times needed to form 8' were increased moreg than the kinetics of 8' — 8 transformation were accelerated. At 90 pct deformation by cold rolling, Graf and Guinier found that the usual 0' —0 8 sequence is reversed: 0 forms first. von Heimendahl 10 confirmed this result with transmission electron microscopy. Pollard and Nutting, 11 and more recently Driver and Barrand, 9 having used the same technique, report that 9 also forms first during creep deformation. In the present study, the maximum amount of deformation was limited to 50 pct reduction by cold rolling in order to insure that 8 formed principally by the decomposition of . I) EXPERIMENTAL PROCEDURES This investigation was conducted on an Al- 3.93 pct Cu alloy, prepared as previously described. 4 Morphological and crystallographic effects of plastic deformation were studied in specimens annealed 6 hr at 548°C, quenched, and then aged for either 3 or 8 hr at 250°C to form large numbers of 0' plates. After cold rolling to a 50 pct reduction in thickness, the

Jan 1, 1969

By C. C. Koch, M. L. Picklesimer

PHYSICAL metallurgists interested in the alloying behavior and phase transformations in rare-earth metals and alloys require a strain-free polished and etched surface for both metallographic and X-ray examination. However, the rare earths have presented a problem in this respect since they are difficult to polish free from strain and are very reactive to the atmosphere. Their tendency to oxidize readily even at room temperature necessitates careful preparation and rather elaborate protection if their surface is to be examined for any length of time. The "light" lan-thanides (i .e., atomic numbers less than 63), especially lanthanum and cerium, are particularly bad in this regard; they oxidize very rapidly at room temperature. To eliminate the problem of plastic deformation remaining on the surface after mechanical polishing, electropolishingl and chemical polishing techniques2 have been developed. The electropolishing technique requires the specimen to be immersed in an electrolyte at -77°C and thus obviates a metallographic study of, for example, the fcc —double-hexagonal close-packed (dhcp) transformation in cerium which begins at -10°C. The chemical polishing solution has been used only on several of the "heavy" rare-earth metals. However, a convenient method for protecting the polished and etched surfaces from atmospheric corrosion has not been available. Our interest in the superconducting properties of lanthanum, and in the phase transformations in lanthanum and cerium, has led us to develop a technique for the metallographic preparation of lanthanum and cerium which clearly reveals the microstructure and preserves the etched surface for days. The specimens are chemically polished and anodized. The chemical polishing is performed at room temperature, the anodic oxide film provides the required protection from the atmosphere, and colors produced in the film provide a simple positive technique for phase identification. Lanthanum and cerium metal ingots obtained from Johnson Matthey and Co., Ltd., were remelted to suitable shapes and heat-treated to produce various microstructures. The samples were placed in epoxy mounts and, after a small hole was drilled in the back of the mount for electrical contact, were ground on silicon carbide

Jan 1, 1968

By R. H. Singleton

ThE purpose of this investigation was to determine the effect of cerium upon the nonmetallic inclusions found in cast and wrought steel containing various amounts of sulfur, oxygen, and nitrogen. Interest of the Physical Metallurgy Laboratory of the Watertown Arsenal Laboratories in this type of research was stimulated by the reports from industry that rare-earth metals imparted beneficial effects upon the mechanical properties of steel, but that the mechanism was not understood. Berry and Dorvel' found that misch metal improved the impact properties of aluminum-killed cast steels. They reported that the rare earths modified the intergranular-film type nonmetallic inclusion, present with aluminum as the sole deoxidant, to a randomly distributed globular type. Lilliequist and Mickelson2 observed the improvement of ductility and toughness of quenched and tempered cast steels through rare-earth additions. They also observed the change from angular to duplex inclusions when rare earths were present. They con-

Jan 1, 1960

By W. D. Bennett

AN interesting effect has been observed in the vacuum etching of titanium in the high temperature ß phase. Using a high vacuum annealing furnace, operating at less than 2x10-6 mm with a tubular titanium liner, it has been found possible to etch polished metallographic specimens at different temperatures between room temperature and 1000°C without contamination or increase in hardness.' Heat etching of titanium has been reported by other workers,' but the following example is of interest as an experiment under high vacuum in the absence of any contamination. Two polished specimens of iodide-processed titanium are placed at different positions along the axis of the furnace corresponding to temperatures of 900" and 800°C above and below the a-ß transus. The specimens are then raised to these temperatures and annealed simultaneously for 3 hr under the same high vacuum conditions. After cooling and withdrawing the specimens, their surfaces are photographed without further treatment. Figs. 1 and 2 show the results for the 800" and 900°C specimens, respectively. Fig. 1, corresponding to a vacuum etch in the a region, shows a typical equiaxed structure with what appears to be a slight shift of grain boundaries. Fig. 2, corresponding to a vacuum etch in the ß region, shows an equiaxed type of structure with the growth of striations in certain grains. The striations are only superficial, as a light polish and chemical etch restores the clean equiaxed structure. The vacuum etch, occurring as it does above the a-ß transus, records the state of the metal in the ß phase by means of the surface relief produced by the selective evaporation of metal from different grains; the metal itself reverts to the equiaxed a on cooling. The nature of the ß etch" (Fig. 2) suggests that, in transforming from the close-packed-hexagonal a to the body-centered-cubic ß lenticular-shaped laminae are formed parallel to common planes of the two structures. This would explain why some grains appear to be unaffected by the etch. The technique has interesting possibilities in the investigation of the mechanics of high temperature transformation. Acknowledgment This note is published by permission of the Deputy Minister, Dept. of Mines and Technical Surveys, Ottawa, Ont., Canada.

Jan 1, 1956

By J. W. Whalen

The design, operation and evaluation of an instrumental method for the determination of fluid saturation in porous materials during multiphase flow studies is described. The presence of a magnetic tracer comprising approximately 20 per cent by weight of the aqueous phase is necessary in the utilization of this method. The results of two-phase relative permeability studies on two samples of porous media are presented. The realizable accuracy of the magnetic susceptibility apparatus in fluid saturation determination is estimated to be 2 saturation per cent. The response characteristics of the instrument, together with its simplicity of operation and maintenance are sufficient to recommend its use in routine laboratory studies. INTRODUCTION The problem of fluid saturation determination in laboratory multiphase flow studies characterizing oil recovery processes is one which has been given exhaustive study. Briefly the requirements which are considered essential for a method sewing this purpose are: (1) that the measurement be made external to the porous rock sample under study with no interruption of the fluid flow pattern, (2) the saturation indication must be independent of fluid distribution in the volume scanned by the measuring device, (3) the sensing element should have a small field of definition enabling several independent measurements to be made along the length of a core sample, and (4) the properties of the fluid phases should not be too greatly influenced by required tracer substances. Several methods of saturation determination have found acceptance as meeting most of the above requirements. These include resistivity,1 X-Ray absorption,2,3,4 radiotracers,5,6,7 and neutron8 diffraction The merits of these techniques have been discussed elsewhere in detail and will not be considered here. It may, however. be pointed out that the elaborate instrumentation required by the methods mentioned above, with the exception of the resistivity method (which is undesirable from other standpoints) encourages the development of methods of saturation determination which, while meeting the requirements listed, are simple to operate and maintain. It is the purpose of this paper to describe the instrumentation and evaluation of a technique for the determination of fluid saturation which combines relative simplicity with an accuracy and applicability comparable with methods now in practice. DESCRIPTION OF THE METHOD If the magnetic susceptibility of one of the fluid phases contained within a porous material is sufficiently greater than that of the remaining phases, the fluid content of the material with respect to that phase may be determined by an induction measurement. This may be accomplished by measuring the induced voltage in the secondary of a transformer which contains the porous sample and its interstitial fluids as a portion of the magnetic flux path. Since the fluids used in multiphase flow studies involving petroleum reservoir samples possess uniformly low magnetic susceptibilities, the use of a magnetic tracer in one of the fluid phases is required. In view of the relatively high paramagnetic susceptibility of salts of the transition elements, together with their high water solubility. these compounds become logical choices as tracer materials. Cobaltous chloride, having a specific magnetic susceptibility of 17.5 x 106 cgs electromagnetic units, was used as the tracer material throughout this work, in a concentration of approximately 20 per cent by weight in the aqueous phase. MAGNETIC SUSCEPTIBILITY APPARATUS Basically, the magnetic susceptibility apparatus consists of a transformer serving as the detecting head, a

Jan 1, 1955

Draftsman and transitman for coal mine work in Middle West. Salary $125 per month. No. 277. Mechanical draftsman familiar with mill and machinery design for metallurgical and chemical plants. Advise experience, salary expected, and references. No. 289. Two cyanide shift bosses, one cyanide mill supt, and one assayer, for work in South America. Expenses clown and return if two year contract is made. No. 290. In assay laboratory of University in the Middle West, man to take charge of ore-dressing and. help in assay laboratory work. Willing to give right man assistant professorship. No. 291. Experienced appraisers familiar either with field or office methods, capable of field survey of the physical properties and able to check up their survey on the books of the company, which require a very intimate knowledge of accountancy. Salary $2000 to $2700. No. 292. Young man trained in chemistry and engineering to conduct experimental work on storage of coal. No. 293.

Jan 4, 1918

By C. D Looker

Common salt is mentioned in the most ancient writings as an important article of diet. It is fairly certain that it was used by men and animals long before the dawn of civilization. Its presence in natural springs has often been the determining factor in colonization; wars have been fought for possession of salt deposits; trade routes have been established expressly for the purpose of traffic in salt. Naturally this led men into adventures and discoveries that altered history and advanced civilization. In the early days the uses for salt were few and the methods of manufacture were crude and the purity low when compared to salt of the present day. Then the salt came largely from springs, shallow wells or the ocean, while today deep wells must be drilled to the natural brines or beds of rock salt and spacious shafts sunk so that the ancient deposits may be made to yield their supply of stored mineral. Mining and Purification The quantity of available salt seems inexhaustible. It occurs in practically every country of the globe. About 20 million tons is produced and consumed annually in the world. Of this amount about 7 million tons is produced in the United States; 13/4 million tons of rock salt, 2 1/4 million tons as evaporated salt and 31/2 million tons in brine used in the chemical industry. Mined rock salt is used in its natural state without purification. It is classified for the trade by crushing and screening. The average purity of rock salt mined in the United States is about 98.3 per cent pure sodium chloride1. The usual impurities are gypsiferous shale, anhydrite and silica, with traces of potassium, magnesium and calcium compounds. Refined or evaporated salt is made by crystallizing the salt from brine in open pans or vacuum pans. A comparatively small amount of salt is made from ocean water or the brines of inland lakes or seas, sometimes by solar evaporation. By far the larger amount of brine is obtained by drill-

Jan 1, 1938

By C. D. Looker

Common salt is mentioned in the most ancient writings as an important article of diet. It is fairly certain that it was used by men and animals long before the dawn of civilization. Its presence in natural springs has often been the determining factor in colonization; wars have been fought for possession of salt deposits; trade routes have been established expressly for the purpose of traffic in salt. Naturally this led men into adventures and discoveries that altered history and advanced civilization. In the early days the uses for salt were few and the methods of manufacture were crude and the purity low when compared to salt of the present day. Then the salt came largely from springs, shallow wells or the ocean, while today deep wells must be drilled to the natural brines or beds of rock salt and spacious shafts sunk so that the ancient deposits may be made to yield their supply of stored mineral. Mining and Purification The quantity of available salt seems inexhaustible. It occurs in practically every country of the globe. About 20 million tons is produced and consumed annually in the world. Of this amount about 7 million tons is produced in the United States; 13/4 million tons of rock salt, 2 1/4 million tons as evaporated salt and 31/2 million tons in brine used in the chemical industry. Mined rock salt is used in its natural state without purification. It is classified for the trade by crushing and screening. The average purity of rock salt mined in the United States is about 98.3 per cent pure sodium chloride1. The usual impurities are gypsiferous shale, anhydrite and silica, with traces of potassium, magnesium and calcium compounds. Refined or evaporated salt is made by crystallizing the salt from brine in open pans or vacuum pans. A comparatively small amount of salt is made from ocean water or the brines of inland lakes or seas, sometimes by solar evaporation. By far the larger amount of brine is obtained by drill-

Jan 1, 1938

By F. Garofalo

It has been shown by various investigators that during constant stress creep the dependence of minimum creep rate, 6,, on stress, o, is given by em = A onat low stress levels, md by 6, = A' exp [ß s] at high stress levels. In these relations A, n, A', and ß are constant at constant temperature. A single relation has been found which satisfies conditions for both high and low stresses and agrees well with experimental results. This relation is 2, = AN (sinh a s)n, where A" is a constant at constunt temperature and a = p/n. This relation also satisfies the linear relation, 6, = k s, found at temperatures near the melting point at low stresses. EXPERIMENTAL creep results have led to a number of empirical relationships between minimum creep rate, 6,, and the applied stress, s. Under conditions of constant stress it is generally found that at low-stress levels,'-' the dependence of minimum creep rate is given by 6, = Asn. At high-stress levels'74 the experimental results fit the relation, 6, = A' exp [po l. In these relations A, n, A' and ß are constant at constant temperature. A model based on climb-of-edge dislocations from a pile-up array leads to a relation similar to that found experimentally at low stresses.' On the other hand. theories based on chemical-reaction rate,5 nonconservatively moving dislocation jogs, and jog migration and climb-of-edge dislocations4 lead to a relation similar to that found experimentally at high stresses. No difference in mechanism between low and high stress levels has been clearly defined; it is questionable whether such a difference really exists. In any event, the major argument usually given in substantiation of a change in mechanism from low to high stresses is that no single relation exists for defining the stress dependence of the creep rate over wide ranges in stress. However, such a relation has been found and is of the form, dm = A" (sinh a s)n, where A" is a constant at con- stant temperature and a = ß/n. This relation agrees well with experimental results over wide ranges in stress and temperature for copper, aluminum, an A1-3.1 pct Mg alloy, and an austenitic stainless steel. STRESS DEPENDENCE OF MINIMUM CREEP RATE At low stress levels the minimum creep rate, gm, depends on the stress, 0, under conditions of constant stress creep through the relation em=Aon [1] The quantities A and n have been defined previously. In the range in which this relation applies, a linear dependence is found in a log em,-log o plot. Above the stress range of application of relation [I], the minimum creep rate increases much mar; rapidly than predicted by relation [I]. This behavior is shown in Fig. 1 for a series of creep tests on copper4 at various temperatures ranging from 673 o to 973°K. Relation [I] is satisfied at the lower stresses, although the results at 973°K are quite limited. In all cases the transition beyond the applicable range of relation [I] is a gradual one indicating no abrupt change in mechanism. For all test temperatures, values of n have been determined from the results in Fig. 1. These are reported in Table I under Alog tm/hlog o. At high stress levels the stress dependence of minimum creep rate under conditions of constant stress is given by im = A' exp [ß a] 2] All factors have been defined previously. In a log em-0 plot, relation [2] predicts a linear function. Experimentally, a pronounced deviation from the prediction of relation [2] is found at lower stresses. As the stress is lowered, the minimum creep rate decreases more rapidly than predicted by relation [2]. This shown for copper in Fig. 2. Again it is found that the transition from high to low stresses is gradual and no really sharp change is found. Values of p determined from the high stress results are given in Table I. The dependence of minimum creep rate on stress at constant temperature for all ranges in stress

Jan 1, 1963

By Y. A. Chang

Phase relationships in the system Cr-Si have been established based on the melting point, X-ray, metallo-graphic, and DTA studies. The three intermediate phases, Cr3Si, Cr5Si,, and CrSi,, melt congruently at 177V ± I@,Cr3Si, 1680"i 20°, and 1490" *20°C, respectively, while the fourth intermediate phase CrSi, melts peritectically at 1413" i 5°C to Cr5Si3 and a melt containing 51 at. pct Si. The temperatures and compositions of the four eutectic isotherms occurring in this system are given below: DTA and metallographic evidences indicate that Cr5Si, undergoes a phase transformation at 1505" i20°C. The high-temperature form of this phase could not be retained by the quenching techniques used in this study. TECHNOLOGICAL interest in the developing of composite systems, consisting of Sic on the one hand as a fiber-reinforced material and metallic substances such as chromium, nickel, or Cr-Ni alloys as a binding agent on the other hand, stimulated the present investigation of phase relationships in the binary system Cr-Si. Earlier works concerning this system have been evaluated and summarized by ansen and Anderko.' Their phase diagram was based mainly on the works of Kieffer, Benesovsky, and schroth2 and Kurnakov.~ According to these authors, the three intermediate phases Cr3Si, CrSi, and CrSi, all melt congruently at approximately 1730°, 1600°, and 1550°C. However, they did not agree on the compositional stability of the fourth intermediate phase between Cr3Si and CrSi. Later Parthe, Nowotny, and schmid4 determined the structure of this phase to be tetragonal T-1 type using the single-crystal method, and concluded that this phase had a formula of Cr5Si3. Since the compilation of Hansen and Anderko,' a new phase diagram for the system Cr-Si has been proposed by Elliott5 based on the works of Goldschmidt and rand,' Guseva and ~vechkin,~ and Trusova, Kuzev, and Ormont8 and the earlier works quoted by Hansen and Anderko.' According to this proposed phase diagram, all four intermediate phases have large ranges of homogeneity and all melt congruently. More recently, Svechnikov, Kocherzhinskii, and yupkog studied the system Cr-Si by the DTA-method. According to their findings, the three intermediate phases, Cr3Si, Cr5Si3, and CrSi,, melt congruently at 1700°, 1720°, and 1475"C, respectively, while the fourth intermediate phase, CrSi, melts peritectically at 1475°C to Cr5Si3 and a melt containing 50 at. pct Si. The temperatures and compositions of the four eutectic isotherms were found to be: In view of the discrepancies existing in the literature concerning the system Cr-Si, it was decided to rein-vestigate the phase relationships in this system. EXPERIMENTAL a) Starting Materials. Chromium disilicide and chromium or silicon powders were used in the present study to prepare the melting point and DTA samples. CrSi, was obtained by directly reacting cold-pressed elemental powders in an atmosphere of Hz at a temperature of about 1250°C. Chromium powder, purchased from Stark Chemical Co., had the following impurities in ppm: Fe, 200; Mg, 1000; and 0, 250; while silicon powder, purchased from the Welded Carbide Co., had the following impurities in ppm: Ca, 700; and Fe, 3500. b) Melting-Point Determination and Differential Thermal Analysis. Cylindrical melting-point samples of approximately 13 mm in diam and 30 mm in length with a rectangular groove in the center were prepared by hot-pressing of well-mixed powder mixtures in graphite dies. Before the melting-point determination, the hot-pressed samples were ground on a sand paper to remove any minute surface contamination of graphite. A small hole of 1 mm in diam, drilled on the center portion of the samples, served as a blackbody cavity for the temperature measurements. DTA samples approximately 13 mm in diam and 15 mm in length were prepared in a manner similar to the melting-point samples. Melting points were determined using the Pirani technique under a helium atmosphere of 40 psi. The design, performance, and operation of this apparatus have been described in detail by Rudy and ~ro~ulski.'~ The temperature measurements were carried out with a calibrated disappearing-filament-type micro-pyrometer. The measured temperature was corrected for losses from the quartz window of the melting-point furnace and for deviations from blackbody conditions of the observation hole. The procedure for temperature correction has also been previously described." The DTA method of Heetderks, Rudy and Eckertl' was also used to check any phase transformations of selected alloys in the system Cr-Si. It was not possible to make remated runs on the same sample once melt-

Jan 1, 1969

By H. B. Fuqua, B. E. Thompson

The area discussed herein, commonly known as the North Texas district, embraces the following 10 counties: Archer, Baylor, Clay, Cooke, Foard, Hardeman, Knox, Montague, Wichita and Wilbarger. It is underlain by two major structural features. The northernmost portion of the district, including Cooke, Montague, northern Clay, Wichita, Wilbarger, Foard and Hardeman counties, is underlain by the system of buried mountains known as the Red River uplift, which is parallel to and closely related to the Wichita-Amarillo uplift of Oklahoma and the Texas Panhandle. While the presence of a great majority of the numerous oil fields of the area is traceable to this feature, the production in Archer, southwestern Clay and southeastern Baylor counties is due to the influence of what is known as the Cisco Arch (so called because of its influence on Cisco deposition), the axis of which extends in a north\lest-southeast direction across Archer County. Discussion of Tables Preliminary to discussing developments during the year 1933, it appears advisable to offer a few words of explanation on Tables 1 and 2, included as part of this paper, in which an effort has been made to sumlllarize oil and gas development in North Texas to Jan. 1, 1934. One of the chief objectives of this publication is understood to be to show production by individual pools, and, if possible, by distinct pays in a pool. This the authors haw been unable to do for North Texas. It is a generally recognized fact that there are well over 100 individual pools, which should perhaps be mow properly called "productive spots," in Archer county alone, with perhaps an even greater number in Wichita County. It can be found upon investigation that an apparently continuous productive area covering Many acres consists of a half dozen lenticular sands, all stratigraphically different,, which produce only under portions of the apparently continuous area. It is also a fact that practically all gross production records are carried by the various intcrcsted parties by major districts or by counties. It is obvious therefore

Jan 1, 1934

By Per Kofstad, Hallstein Kjöllesdal

The oxidation behavior of niobium (columbium) has been studied in the temperature range 500° to 1200°C and at oxygen pressures of 760,100, 10, 1, and 0.1 mm of Hg. The work comprises kinetic studies of the oxidation as well as structural investigations of the oxidized specimens by means of X-ray diffraction, electron diffraclion, electron microscopy, and metal1ographic techniques. The oxidation reaction has a highly irregular temperature dependence and is unusually sensitive to changes in the oxygen pressure. The complex oxidation behavior is suggested to be due to formation of different Nb2O5 modifications in different temperature regions. During oxidation oxygen is also dissolved in the metal. Formation of oxide whiskers take place on the oxide surface at temperatures above approximately 800°C. VARIOUS aspects of the oxidation of niobium have been studied.l-12 The investigations show that niobium has a complex oxidation behavior, and the oxidation

Jan 1, 1962

By Staff

Concentrates at the rate of 1000 tons a day are being smelted by International Nickel Co.'s new commercial flash smelting furnace. Developed by Inco, the process is a radical departure from the former practice which involved conventional smelting in coal-fired reverberatory furnaces. In the new process copper flotation concentrate and flux are injected horizontally with oxygen into a specially designed reverberatory furnace, and smelting temperature is maintained solely by the flash combustion of iron and sulphur while the particles are in suspension. The major benefits of this new process stem from two sources: 1)-Substitution of energy from local resources for imported coal; and 2)-Production of liquid sulphur dioxide, replacing equivalent imported sulphur. A measure of these benefits is afforded by considering the saving, in 1954, of 60,000 tons of coal and the production of 70,000 tons of liquid sulphur dioxide, equivalent to 35,000 tons of sulphur.

Jun 1, 1955

By F. W. von Batchelder

The principles of microradiography and their application practically coincided with the discovery of X-rays. These principles were first used in the metallurgy field by Heycock and Neville1 in a study of the dendrite structure of alloys of Au-Na, Au-A1, Cu-A1, and Ag-A1. The method was introduced in the USA by clark2 after a visit to France. Scores of papers have been written, and a very complete bibliography on this subject was compiled by the Eastman Kodak company. Although a number of papers have discussed X-ray

Jan 1, 1959

By S. C. Sircar, B. K. Dhindaw

KINETICS and mechanism of sulfation reactions have been studied extensively. Qualitative and quantitative data are reported for the kinetics and mechanism of sulfation reaction of copper oxide pellets;''2 yet it remains a controversial Subject. The mechanism and kinetics of the sulfation of zinc oxide powder (B.D.H. analar quality) were studied by gravimetric technique. A spring of high-carbon steel wire with accuracy well within 0.2 mg was used for measuring weight change. The sample was taken in a Pyrex glass bucket, hanging freely inside a Pyrex glass tube reactor, with a gold wire attached to the spring, the reactor being surrounded by a movable furnace (double wound type) with a temperature control within *5"C. Flow of oxygen, 60 cu cm per min, and sulfur dioxide, 45 cu cm per min, were measured through calibrated flowmeters and the mixture dried over PZ05 before entering the reactor. The experimental results are presented in Figs. 1 and 2. The plot of weight change of zinc oxide, giving the amount of zinc sulfate formed, was found to be linear over the temperature range of 500" to 700° C and up to a conversion of approximately 60 pct, as beyond it they divert from linearity.' The rate of sulfation was found to be affected by total flow rate of gases at a fixed ratio of SO2/O2, up to 60 cu cm per min, and was found to be linearly dependent on quantity of total powdered sample taken. The plot of rate of sulfation of zinc oxide, 70 mg, with varying amounts of vanadium pentoxide, at a constant ratio of gases as mentioned above, and at a constant temperature of 625"C, was also found to be linear as seen in Fig. 2. Extrapolation to zero V2O5 addition gives the same rate of sulfation, as in case of pure zinc oxide, 70 mg. Vz05 was prepared by heating ammonium vanadate at 600°C for 15 min in a muffle furnace. The available literature points out that the theory of sulfation that has received the maximum support postulates the following mechanism for sulfation of ZnS: 2ZnS + 30, = 2Zn0 + 2SOZ; the ZnO formed acts as a catalyst for the reaction, 2 S02 + O2 = 2S03. This SO3 reacts with ZnO to give zinc sulfate. It is suggested here that the above widely supported mechanism is operative in the sulfation reaction and that the rate-controlling step in the sulfation reaction of ZnO is the formation of SO3 from SO, and 0,. The authors are carrying on further work in this line, and the details will be published later. The authors wish to acknowledge the facilities provided and the help extended by Prof. P. R. Dhar, Head, Department of Metallurgical Engineering, and the permission granted to publish this note by the Director, I. I. T., Kharagpur.

Jan 1, 1969

By Simon D. Strauss

What are future prospects for U.S. mining? In many quarters the assumption is made that this country has passed its zenith as a mineral producer -- that it is in a period of decline and that it is becoming a have-not nation like Japan and much of Western Europe. These industrial rivals of ours must depend almost entirely on others for their mineral supplies. In trying to answer this question one must of course distinguish between resources and productive capacity. In today's volatile and competitive markets, the definition of what are reserves and what are merely identified resources becomes ever more difficult. Many large deposits have been found that are unlikely to be viable in the marketplace under normal conditions but that can be of significance to the nation's military and industrial security in times of emergency. I should like to draw on personal experience from World War I1 for illustration. 4fter Pearl Harbor great concern developed over the availability of a long 1ist of strategic materials for which this country was largely dependent on imports. Included were a number of minerals of which domestic deposits had been identified. Among these were chromite, manganese ore, mercury, mica and tungsten.

Jan 1, 1982

By Irving Hale

The superiority of electric power for mining purposes was recognized in a general way as soon as the electric motor be-

Jan 1, 1897

By D. Harker, W. E. Seymour

CERTAIN alloys of iron and nickel, when rolled and annealed, possess a preferred crystal orientation: (001) in the rolling plane and [loo] in the rolling direction, when recrystallized at 850" to 1050°C after approximately 98 pct cold reduction. Since the preferred orientation makes a direction of easiest magnetization coincide with the rolling direction, these alloys, especially a 50 pct iron in nickel alloy, have found wide application in the electrical industry' for choke coils and special types of transformers. The rate of the recrystallization reaction was studied at temperatures ranging from 500° to 600°C. The heat of activation for the reaction was calculated from the observed rates, and crystal orientation determinations were made before and after re-crystallization. A vacuum melted iron-nickel alloy* analyzing 49.6 pct nickel, 0.018 pct carbon, and 0.30 pct manganese was used for the experiments. The alloy was cold-rolled 98 pct into strips 1/2 in. wide by 0.002 in. thick. Specimens 1 in. long were sealed under a vacuum (approximately 10-8 mm Hg) in 1/2 in. ID pyrex glass tubes. For heat treatment these tubes were fastened to Nicrohm wires and submerged in a molten salt bath controlled to ±2°C. (The maximum measurement error was within 3°C.) The time at temperature was varied logarithmically from one sample to another, and runs were made at 500°, 525", 550" and 575°C. A molten lead bath was used for a run at 600°C which was controlled to the same accuracy. To determine the extent of recrystallization after a particular time at a given temperature, a method was used suggested by the work of Decker, Asp, and Harker.3,4 This method employs an X-ray spectrometer whereby X rays are diffracted from crystallites whose diffracting atom planes are parallel to the rolling plane of the specimen. The intensities of the diffracted rays are measured by a Geiger counter. The counter can be rotated through a range of angle, and can be motor driven through this range at a speed of 2" per min. The measured intensities are plotted vs. angle by a potentiometer recorder. In a 50 pct iron-nickel alloy it was found that only (200) reflections were obtained from the rolling plane with recrystallized material, and that only (220) reflections were obtained from the rolling plane with unrecrystallized material. No other reflections were obtained under these conditions over a range of Bragg angle of 0 to 45" using either type of specimen. As a consequence, the intensity of the (200) reflections from the rolling plane was taken to indicate the amount of recrystallized ma-terial present in a specimen, and the corresponding intensity of the (220) reflections was taken to indicate the amount of unrecrystallized material present. To insure flatness and proper alignment of the reflecting specimen in the spectrometer, the sample was laid in a slot 1/2 in. wide x 0.001 in. deep which was machined in a 3/4x2x1/2 in. steel carrier. The specimen then was taped down with cellophane tape. This steel cradle was mounted vertically in the specimen holder of the spectrometer so that the bottom edge of the carrier rested against a horizontal shoulder. Intensity data used in plotting the percent of recrystallized material vs. time at temperature were obtained by directly counting the diffracted beam of nickel filtered copper Ka radiation used throughout the work. The X-ray spectrometer was employed also in obtaining pole figure data to be used for orientation determinations. At the beginning of this investigation a transmission pole figure holder was used." As a thickness of 0.002 in. of this alloy was found to be opaque to the copper Ka radiation, it was necessary to reduce the thickness of the pole figure specimen. A cold-worked sample was etched in a 50 pct HCl solution for 5 min and was found to transmit a

Jan 1, 1951

By Burnham E. Field

The chemical industry is constantly looking for new materials which either are more resistant to corrosion than those now available or have improved physical properties to meet the requirements of higher temperatures and greater pressures. Attack by acids is one of the more important forms of corrosion and in the last few years the development of acid-resistant alloys has been quite rapid. Perhaps the most notable example is that of nitric acid, the problem of which has largely been solved by the chromium-iron and chromium-iron-nickel alloys. Sulfuric acid may be handled in lead, iron, or the iron-silicon alloys, depending on conditions. As to hydrochloric acid, no metal or alloy can be called entirely satisfactory for handling this acid under plant conditions.' The results of our investigations on the resistance of the nickel-molybdenum alloys to hydrochloric acid have been confirmed by those of Guertler, Rohn, Schulz, Jenge, and others12 but thus far only one such alloy has approached commercial production in Germany; this contains approximately 15 per cent. chromium and 7 per cent. molybdenum with the remainder chiefly nickel. Dr. S. W. Parr, as far back as 1914, developed a complex alloy known as "illium," with a nickel base and containing some molybdenum. 3 Dr. Parr was primarily interested in an alloy for lining bomb calorimeters, and while illium does show good resistance to acid it is too expensive for general use. Two United States

Jan 1, 1929