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By M. Hansen, C. C. Wang

THE 6 phase of the Cu-Sn system (Cu,Sn, = 32.53 pct Sn) was considered to be stable down to room temperature until Owen and Iball showed by X-ray analysis that it undergoes a eutectoid decomposition into the a and e phases at a temperature near 300°C. Their findings have been confirmed by other investigators,2-5 a11 of whom used X-ray diffraction studies of powdered specimens. The transformation temperature has been reported by various authors as lying between 300" and 380°C. To our knowledge, no microscopic evidence of the eutectoid reaction has been published, as yet. It was in connection with other work that longtime annealings at 300°C were conducted with alloys containing 22, 32.6, and 35 pct Sn (nominal compositions) prepared from electrolytic copper and electrolytic tin and cast in a small iron mold. The specimens were first annealed at 700°C for 5½ hr and quenched from 400 °C after cooling to, and annealing at, that temperature for 9½ hr. After this treatment the sample with 22 pct Sn was cold worked for 15 pct reduction in thickness; the 32.6 and 35 pct alloys were too brittle to be cold worked. The final anneal at 300°C was done in a sealed pyrex glass bulb for 63 days. Fig. 1 represents the microstructure of the annealed alloy with 22 pct Sn. It shows primary a solid-solution crystals in a matrix of the (a + 8)-eutectoid formed at 520 °C. The a crystals contain 8 inclusions which precipitated from a due to the decrease in the solubility of tin in copper with fall in temperature. The decomposition of the 8 phase into a (light) and E (dark) can clearly be seen in some areas of the (a + 8)-eutectoid matrix. However, the decomposition is far from being completed, even after the long-time anneal used. Figs. 2 and 3 depict the microstructures of the annealed 32.6 pct alloy, which was intended to consist entirely of 6 phase. Due to some loss in copper on melting, the composition is slightly higher in tin. Accordingly, the sample after quenching from 400 "C consisted of grains of the 8 phase with the e phase arranged along the grain boundaries and as a Wid-manstatten precipitate within the 6 grains. After an annealing time of 63 days, the eutectoid decomposition, 6 + a + e, is still in its early, initial state. The pearlitic type of eutectoid is nucleated at the c crystals, preferably those surrounding the grain boundaries of the 8 phase. The appearance of the (a + €)-eutectoid in the 35 pct Sn alloy was very similar to that shown in Figs. 2 and 3. Again, the eutectoid decomposition nucleated at the 6 phase and proceeded from there into the 8 areas. As is evident from Fig. 2, the rate of decomposition of the 6 phase at 300°C is extremely sluggish: In the representative area shown only about 5 pct of the 8 phase has undergone the eutectoid trans- formation after annealing for 63 days. On the other hand, Owen and Williams2 have reported that X-ray photographs of powdered samples with between 17.5 and 34 pct Sn did not show 8 lines after annealing for only five to seven days at 300°C. This is in accordance with the fact that the rate of reaction in powdered samples is higher than in massive specimens, as a result of the excess free energy of the powder (due to its greater surface area). The authors wish to express their thanks to C. A. Johnson for preparation of the micrographs.

Jan 1, 1952

CARL A. WENDELL, New York, N. Y. (written discussion*) .-I have never seen in print anything that even remotely has approached this article in clearness and important conclusions in conjunction with work done on the sink-and-float test. I have had many hundreds of these tests made and on different specific gravity solutions and the resultant product analyzed, but I have never grasped nor been able to show what this article sets forth. This article brings out one factor very clearly to my mind; what is to take the place of the solutions of different specific gravities used to obtain the laboratory results, when it comes to washing on a large scale, since water has one constant weight only? The answer is, sizing of coal. And as we know the importance of size versus specific gravity of the material to be washed, perhaps defined (practical) lines can ultimately be gotten up so that the sizing, if any, may be determined at the same time as the laboratory work on the coal is being done. G. R. DELAMATER, ? Steelton, Pa. (written discussion?).-The authors' deductions are well founded and although they disclaim any wide experience in commercial coal washing, practically all of the data presented are applicable to coals of all parts of this country. The paper clearly sets forth the great necessity of careful preliminary investiga-tion of each contemplated washery undertaking and contains the follow-ing very true statements. "It is not safe to assume that any coal which can he successfully washed on coarse coal jigs can be cleaned more com-pletely by washing at a finer size on tables," and "The effect of finer crushing upon the completeness with which impurities may be separated from coal depends upon two opposing tendencies. First, that the more finely a raw coal is crushed, the more completely will the particles of impurities be detached from the particles of clean coal. Second, the finer a coal is crushed the more difficult it becomes to separate the pieces of clean refuse from the pieces of clean coal."

Jan 12, 1919

By John McDonald

THE amount of published literature in the field of mechanical proper-ties of magnesium alloys is not great; particularly with respect to rolled alloys. Haughton and Prytherch1 have summarized most of the articles to 1937, including their own work on sheet. Although many papers can be found dealing' with the technology of magnesium and the alloys now in commercial use, there does not seem to be any work dealing exclusively with the variation in properties of rolled alloys as caused by changes in alloy composition. Comparison of published data reveals considerable discrepancies in, properties of alloys of the same composition, probably due to differences in the details of working and heat-treating followed by different workers. The purpose of this paper is to study the proper-ties of alloys in conditions where the effect of such differences have been eliminated. It is well known that the strength and ductility of metals are functions of the working and heat-treating they have received, as well as of their chemical composition. In comparing alloys with respect to these proper-ties, therefore, all possible combinations of the variables of the fabrication procedure ought to be carried out on each alloy. One or more of these treatments will produce the highest ductility, or strength, or both. These highest properties would then be selected as characteristic of each alloy, and alloys would be compared on the basis of those properties. Thus a separation of the effect of composition and that of working and heat-treating would be achieved. In this paper, however, a compromise with completeness has been made by carrying out a restricted number of treat-ments. As a consequence, the properties obtained are not necessarily the best that the alloy is capable of exhibiting; but since all alloys have been treated by the same method, the results ought to be comparable. The elements selected for the study comprise a class that will alloy easily with magnesium, and that are relatively cheap. Each was added in different amounts, up to a limit that varied with the element.

Jan 1, 1939

By T. G. Sieber, T. D. Tiemann

The extraction of quartz from siliceous iron ores by dissolution in sodium hydroxide solution has been described in detail in AIME Transactions. l923 data reported covered the temperature range from 230-416°F, where a continuous increase in the amount of silica extracted with increase in temperature was found. It is the purpose of this paper to describe some unexpected results of more recent work exploring principally the range of 500600°F where higher rates and greater amounts of silica extraction were antici-p ted. In brief, the experimental procedure consists in digesting the ore under pressure in solutions of sodium hydroxide, filtering the suspension and weighing and analyzing the dried residue for iron content. The amount of extraction is calculated from the weight loss or from the iron analysis of the residue and that of the original ore.

Jan 1, 1969

By R. Silent, N. A. Rousselot

The first producing wells completed in the Kettleman Hills arca were noteworthy for their high gas-oil ratios. As a result they became the object of criticism, and controversies arose based on their alleged lack of gas conservation. Ultimately protracted hearings ensued in the District Court of the area, and diverse rulings and subsequent modifications have been handed down affecting the permissible gas-oil ratios. When the Kettleman North Dome Association was formed in April, 1931, and the control of the major portion of the North Dome area vested therein, it was decided to produce only those wells which had a relatively low gas-oil ratio. Among the wells having the highest gas-oil ratio were the Milham Elliott No. 1 (the discovery well) and the Continental Elliott 12-8. drilled as an offset to it. Under the numbering system adopted by the Kettleman North Dome Association, these wells are now known as 88-2P and 1-12P, respectively. Milham Elliott No. 1 was originally drilled to 7236 ft., then redrilled to 7108 ft. The upper portion of the Temblor Horizon produces with a very large gas-oil ratio; production which actually consists of light crude oil with an accompanying large.volume of gas. Little was known as to the location of the Temblor formation at that time but it is now generally accepted that its top was encountered at 6180 ft., giving 928 ft. of penetration. Initial production was estimated at 4000 bbl. of oil and 80 to 90 million cubic feet of gas per day, giving a gas-oil ratio in excess of 20,000 cu. ft. of gas per bbl. of oil. This ultimately increased to a ratio of about 48,000 at the time the well was killed when it was producing about 1100 bbl. of oil and 52 million cubic feet of gas, with a flow pressure of 1200 pounds. The Continental Elliott 12-8 was drilled to a depth of 6876 ft. with the top of the Temblor at 6100, giving a penetration of 776 ft. The estimated initial production of this well was 7000 bbl. of oil and 130

Jan 1, 1933

By Donald W. Scott, Nathaniel Arbiter, A. C. Richardson

THIS paper describes the application of amine flotation to a specific problem-that of increasing the grade of magnetite concentrates derived from an iron ore requiring extremely fine grinding for mineral liberation. Experiments conducted on an iron ore from Wisconsin had shown that concentrates containing 60 to 62 per cent iron and 12 to 14 per cent silica could be produced by magnetic separation. The residual silica occurred as quartz and hornblende, either entrained or locked with magnetite. Most advantageous utilization of the concentrate, however, necessitated that the silica content be reduced to about 5 per cent, equivalent to an iron content of 67.5 per cent. It had been demonstrated that tabling of the magnetic concentrate removed sufficient quartz and hornblende to yield an acceptable concentrate, but disadvantages inherent in tabling dictated that flotation be investigated as a substitute. The goals set for the flotation investigation were: (I) the production of concentrates of about 68 per cent iron content from the magnetic concentrate; (2) an iron recovery of about 85 per cent of that in the feed to flotation; and (3) minimum reagent cost. Both batch and continuous flotation tests were employed; the former, to establish the procedure and the latter to verify it. Although the data were obtained on a specific ore, and with a commercial application in view, it is believed that they have a bearing on other problems where amine flotation is being used or is anticipated. SAMPLES Two samples, designated "minus 100mesh magnetic concentrate" and "minus 150-mesh magnetic concentrate," were used for the batch experimental work. They differed only in the degree to which the crude ore was ground prior to magnetic separation. They were stored moist in steel drums in quantities sufficient for all the experimental work reported. This procedure had the advantage of allowing all tests to be made on common samples, but had the disadvantage that the individual flotation samples, because of the difference in storage time, were subject to various stages of surface alteration. Previous work had indicated that common samples were desirable for the batch studies, and it was decided that if these data appeared sufficiently promising the effect of surface alteration could be checked best by continuous tests. The size distributions and the assays of the samples are given in Table I. The minus 150-mesh magnetic concentrate, on which most of the flotation tests were made, assayed 60.9 per cent iron, 13.3 per cent silica, and 0.016 per cent phosphorus. The minus 325-mesh portion represented 78.1 per cent of the sample by weight, and assayed 67.9 per cent iron. Thus, the insoluble, mainly silica, was concentrated

Jan 1, 1945

By M. D. Banus, M. B. Bever, A. K. Jena

Measurements of the heat effects on addition of various solid phases of InSb to a solution calorimeter have confirmed the existence of a new high-pressure plzase InSbQII), which was jormed at 37 kbar and 623°K. The heats of formation of InSbQ), InSbfl), and InSb(111) have been measured and the heats of transjormation of InSb(1) to InSb(1l) and InSb(Iii) and of 'InSb(ll) to InSb(iiI) at atmospheric pressure and 78°K have been determined independently. Other thermodynamic properties of these phases, the phase boundary InSb(i)/InSb(ll), and the relative positions of the triple points are calculated. The pressure-Dolume term is shown to be more critical than the internal energy difference in making the phase InSbQ) less stable than InSb(II) at high pressures. Observations on partially transformed specimens suggest that the transformation of' metastable InSb (III) takes place in the two steps InSb(lll) — InSbQI) and InSbQI) — InSb(l). The compound InSb can exist as several phases depending on the temperature and pressure. The phase InSb(I), which is a semiconductor having the zinc-blende structure, transforms into the phase InSb(11) at a pressure of about 23 kbar and room temperature.'-3 The phase InSb(II) has the 6 tin structure,4-6 is metallic, and becomes a superconductor below 2.lok7 An orthorhombic phase of InSb has been reported to occur above a pressure of approximately 30 kbar at room temperature.' This phase is also a superconductor below about 3.4k9 The phase InSb(I1) is retained at atmospheric pressure if it is quenched to 78°K under pressure,6,7 but tends to transform at higher temperatures and does so explosively above approximately 210ok,7 A value of the heat of transformation of InSb(1) to InSb(II) at 210°K and atmospheric pressure has been reported.' A concurrent publication'0 reports evidence for a new solid phase InSb(III), which was formed by annealing InSb above 58 1°K at 37 kbar, above 560°K at 52 kbar, and above 473°K at 65 kbar. Specimens of InSb(II1) had a superconducting transition temperature of 4.lo ± 0.1oK. X-ray diffraction patterns also indicated the presence of a new phase. In this communication, thermodynamic properties of the phases InSb(I), InSb(II), and InSb(II1) are reported and discussed. The phase boundary InSb(I)/InSb(II) and the relative positions of the triple points are calculated. 1) EXPERIMENTAL 1.1) Preparation of Specimens. Specimens of the high-pressure phases of InSb were prepared in a belt-type high-pressure chamber by a tichnique described in detail elsewhere.'' Charges of 0.6 to 0.8 g of Cominco semiconductor grade InSb were used. The temperatures were measured with a chromel-alumel thermocouple, the hot junction of which was within 0.5 mm of the specimen. The specimens were heated under a pressure of 37 kbar for 1 hr at 723°K (which is well above the liquidus) and quenched to room temperature. One set was annealed at 523°K and another set at 623°K for 20 to 24 hr. These annealing temperatures were chosen because 523°K was below and 623°K was above the temperature of the transformation of InSb(II) to InSb(1Tl) at 37 kbar.10 The specimens were then cooled to 125°K by passing liquid nitrogen through the jacket of the belt die before the

Jan 1, 1968

By John D. Kalasky

The success in providing adequate ventilation to the active faces of a coal mine for all methods of mining depends upon good face control and the air distribution and control system. A good system provides overcasts, air locks, regulators and bleeders so that an adequate flow of air will be confined to the working places with least opportunity for interruption, and that a flow of air is maintained, however small, across the worked out area to the bleeder and away from men and equipment at all times. In gaseous mines, it is just as important to satisfy effective bleeding as it is to satisfy the air volume requirements in the operating splits. The two requirements go hand in hand. Although not complicated, ventilation and methane drainage in longwall mining in a gaseous mine require careful forethought and adequate facilities to make them safe.

Jan 8, 1966

Lucien Eaton, Ishpeming, Mich. (communication to the Secretary *):—I began to use water Leyner drills at the Cliffs Shaft mine at Ishpeming, Mich., over four years ago, and now have over 20 in use. The ore in this mine is hard specular hematite, and is mined by the room-and-pillar system, the rooms being driven as breast stopes. For many years only 3 1/4-in. piston drills were used in the mine, each machine ordinarily being able to drill from 15 to 25 ft. of holes in a shift. In the hardest ground, however, it was often, impossible to drill more than 2 or 3 ft. in a shift. When water Leyner drills were used the footage drilled was materially increased, especially in the hardest ground, but it was found that in very hard ground the breakage of machine parts, and especially of drill steel, was very high. At this time round steel with lugs forged on the shanks was used, and most of the breakage occurred at or near the lugs. Many experiments were made in an endeavor to overcome this breakage, and it was finally decided to do away with the lugs altogether, and use hexagonal steel. Accordingly I designed a chuck to use hexagonal steel without luge, a tappet being interposed between the hammer and the shank of the' drill steel. The design of this chuck of the proper size for the No. 18 Ingersoll-Leyner drill is shown in Fig. I. The different parts are also shown photographed in Fig. 2. A is the barrel of the chuck, which revolves inside the front head. It is made of machinery steel. B is the bushing which screws into the front end of the barrel A, and in which the drill steel fits loosely. This is turned down from a steel casting, the hexagonal hole being cast and then broached out to the proper size. It is case hardened inside. C is the tappet, which fits smoothly inside A just behind the bushing B. It is made of " N " temper Crescent tool steel and is carefully tempered. D is the tappet ring, which prevents the tappet from being pushed back too far by the

Jan 1, 1914

By Donald W. Scott, Nathaniel Arbiter, A. C. Richardson

This paper describes the application of amine flotation to a specific problem—that of increasing the grade of magnetite concentrates derived from an iron ore requiring extremely fine grinding for mineral liberation. Experiments conducted on an iron ore from Wisconsin had shown that concentrates containing 60 to 62 per cent iron and 12 to 14 per cent silica could be produced by magnetic separation. The residual silica occurred as quartz and hornblende, either entrained or locked with magnetite. Most advantageous utilization of the concentrate, however, necessitated that the silica content be reduced to about 5 per cent, equivalent to an iron content of 67.5 per cent. It had been demonstrated that tabling of the magnetic concentrate removed sufficient quartz and hornblende to yield an acceptable concentrate, but disadvantages inherent in tabling dictated that flotation be investigated as a substitute. The goals set for the flotation investigation were: (I) the production of concentrates of about 68 per cent iron content from the magnetic concentrate; (2) an iron recovery of about 85 per cent of that in the feed to flotation; and (3) minimum reagent cost. Both batch and continuous flotation tests were employed; the former, to establish the procedure and the latter to verify it. Although the data were obtained on a specific ore, and with a commercial application in view, it is believed that they have a bearing on other problems where amine flotation is being used or is anticipated. Samples Two samples, designated "(minus 100-mesh magnetic concentrate" and "minus 150-mesh magnetic concentrate," were used for the batch experimental work. They differed only in the degree to which the crude ore was ground prior to magnetic separation. They were stored moist in steel drums in quantities sufficient for all the experimental work reported. This procedure had the advantage of allowing all tests to be made on common samples, but had the disadvantage that the individual flotation samples, because of the difference in storage time, were subject to various stages of surface alteration. Previous work had indicated that common samples were desirable for the batch studies, and it was decided that if these data appeared sufficiently promising the effect of surface alteration could be checked best by continuous tests. The size distributions and the assays of the samples are given in Table I. The minus 150-mesh magnetic concentrate, on which most of the flotation tests were made, assayed 60.9 per cent iron, 13.3 per cent silica, and 0.016 per cent phosphorus. The minus 325-mesh portion represented 78.I per cent of the sample by weight, and assayed 67.9 per cent iron. Thus, the insoluble, mainly silica, was concentrated

Jan 1, 1947

By Donald W. Scott, Nathaniel Arbiter, A. C. Richardson

This paper describes the application of amine flotation to a specific problem—that of increasing the grade of magnetite concentrates derived from an iron ore requiring extremely fine grinding for mineral liberation. Experiments conducted on an iron ore from Wisconsin had shown that concentrates containing 60 to 62 per cent iron and 12 to 14 per cent silica could be produced by magnetic separation. The residual silica occurred as quartz and hornblende, either entrained or locked with magnetite. Most advantageous utilization of the concentrate, however, necessitated that the silica content be reduced to about 5 per cent, equivalent to an iron content of 67.5 per cent. It had been demonstrated that tabling of the magnetic concentrate removed sufficient quartz and hornblende to yield an acceptable concentrate, but disadvantages inherent in tabling dictated that flotation be investigated as a substitute. The goals set for the flotation investigation were: (I) the production of concentrates of about 68 per cent iron content from the magnetic concentrate; (2) an iron recovery of about 85 per cent of that in the feed to flotation; and (3) minimum reagent cost. Both batch and continuous flotation tests were employed; the former, to establish the procedure and the latter to verify it. Although the data were obtained on a specific ore, and with a commercial application in view, it is believed that they have a bearing on other problems where amine flotation is being used or is anticipated. Samples Two samples, designated "(minus 100-mesh magnetic concentrate" and "minus 150-mesh magnetic concentrate," were used for the batch experimental work. They differed only in the degree to which the crude ore was ground prior to magnetic separation. They were stored moist in steel drums in quantities sufficient for all the experimental work reported. This procedure had the advantage of allowing all tests to be made on common samples, but had the disadvantage that the individual flotation samples, because of the difference in storage time, were subject to various stages of surface alteration. Previous work had indicated that common samples were desirable for the batch studies, and it was decided that if these data appeared sufficiently promising the effect of surface alteration could be checked best by continuous tests. The size distributions and the assays of the samples are given in Table I. The minus 150-mesh magnetic concentrate, on which most of the flotation tests were made, assayed 60.9 per cent iron, 13.3 per cent silica, and 0.016 per cent phosphorus. The minus 325-mesh portion represented 78.I per cent of the sample by weight, and assayed 67.9 per cent iron. Thus, the insoluble, mainly silica, was concentrated

Jan 1, 1947

By J. M. McDowell

A study has been made to deter~r~irre how the behavior of a water drivee reservoir changes as a function of the permeability of the formation and as a function of the size of the aquifer. The effect of pressure maintenance programs on the rote of nat11rn1 water influx is also studied, (IS well as the influence on the influx of the position of water injection we1ls with reference to the oil-water contact. The results are determined by the use of an electrical reservoir analyzer and are plotted as families of curves of pressure, natural water influx, and water injection vs time or cumulalive production. Two size aquifers are studided. One is limited with a 36-inile radius, and the, other approximates an infinite reservoir. The field remains the same in all respects for the completed. study except that the permeability is changed to agree with that assumed for the aquifer. 1 N TR ODUCTI ON this study was undertaken in -dcr to determine how the pres- sure decline and water influx of a water drive field would change as a function of the rate of fluid withdrawals, as a function of the permeability of the formation, and as a function of the size of the aquifer. The effect of pressure maintenance programs on the rate of natural water influx was also studied as was the position of water injection wells with reference to the oil-water contact. The information has been determined by the use of an electrical reservoir analyzer1, sometimes referred to as a Carter type analyzer. This instrument is an analog type computer which can be set up to represent a water-drive oil field. It can reproduce the past performance of the field in terms of analogous electrical quantities when the proper circuit analog of resistors and condensers has been determined, also, it can determine the future behavior for any method of production which may be selected, or permit the comparison among several different methods. Although most applications of the reservoir analyzer"" have been to thc study of specific field performance, it is intended to use the analyzer here to help understand how various reservoir characteristics effect the final performance of the field and to sec under what conditions water injection will be of benefit and to what extent. Within the oil industry the performance of water-drive reservoirs was first described analytically by LV. Hurst' and M. Muskat2 for certain types of boundary conditions. The solutions of the equations developed involved products of exponential functions and Bessel functions. Later publications by Hurst4 and van Ever-clingen" and the hooks of Muskat6 gave further information on reservoirs with other boundary conditions. They also presented rather extensive curves and tables to help evaluate the analytical expressions involved. A rccent series of publications by Chatas. bascd on the work of Hurst and van Everdingen, gives quite complete charts and tables of data to evaluate the pressure decline or water influx in infinite or limited radial reservoirs. and in linear reservoirs. The curves in all of these publications are given in dimensionless form

Jan 1, 1956

By G. A. Parks, C. Kovacs

The xanthate flotation of chrysocolla can be improved by preheating the ore to 500° to 600°C. Addition of water vapor reduces the preheating temperature required. The temperature range of flotation improvement correlates well with the range over which dehydroxylation occurs. This observation is consistent with changes in the structure and properties of the mineral as detected by measurement of solubility, D.T.A., T.G.A., X-ray diffraction, and infrared absorption and with recently proposed explanations of chrysocolla flotation. A brief experiment by one of the authors several years ago showed that exposure of chrysocolla to high temperature water vapor resulted in increased recovery by subsequent xanthate flotation. Recently renewed interest in flotation and thermal properties of chrysocolla1-5 prompted further study of this effect and more detailed reporting.6 This paper explores the response of pure chrysocolla recovery in Hallimond tube flotation tests to the time and temperature of exposure and to changes in the water vapor pressure. Brief attention is paid to the effects of such treatment on accessory minerals. A single experiment with flotation of chrysocolla from an ore is reported. MATERIALS Chysocolla from Inspiration, Gila County, Ariz. was crushed in a porcelain mortar, cleaned of visible and magnetic impurities, and screened to obtain -48 +65 mesh (Tyler) material for flotation test work. The clean material contained 28.5% Cu and was identified as chrysocolla by comparison of X-ray diffraction, D.T.A., and infrared absorption data with that reported for similar materials by others.4,5,7 Samples of malachite and chalcopyrite, prepared in a similar way, were also identified by X-ray diffraction. The sources of these materials are unknown. A sample of chysocolla-bearing oxidized copper ore from Pima, Ariz. was crushed and dry ground for thermal activation and subsequent flotation. PROCEDURES Activation: The apparatus used for exposure of materials to high temperature water vapor is illustrated in Fig. 1. The furnace temperature was controlled to ±5°C Water vapor pressure was controlled by pre-saturating a nitrogen carrier stream with water in an adjustable thermostatted saturator (multiple bubbler). A water manometer and capillary orifice flow meter were used to measure nitrogen flow rates for activation and for subsequent Hallimond tube tests. Gas flow rate and temperature were adjusted prior to introduction of samples. Exposure time was measured from the moment of introduction of the sample to the furnace, hence includes an initial drop below the control temperature. After heating, the samples were removed from the furnace and stored at room temperature in air. Representative samples of activated materials were examined by X-ray diffraction and infrared absorption.

Jan 1, 1967

By C. Richards Honeycutt, Frederick C. Langenberg, Guenter Pestel

Solidification in a moving electromagnetic field was successful in altering the as-cast grain structure of steel ingots. The equipment is described and exerimental results are presented for several different alloys. Conditions for optimum grain refinement are described and an empirical design constant presented. The effect of the grain refinement on hot workability is briefly discussed. T HE grain structure of a steel ingot teemed into a metal mold can be defined by macroscopic examination in semiquantitative terms. For example, the relative volume of obviously differing structures can be estimated with the classic definitions of chill, columnar, and equiaxed zones. Experimental evidence has proven that the grain structure of an ingot is affected by changes in such factors as teeming temperature, rate of teeming, degree of turbulence, size of ingot, mold characteristics (including preheat temperature, design and coating), and composition of the metal (especially as it affects the range of solidification). Significant advances have been made in fundamental solidification studies; but the principles which have been developed are difficult to apply tothe complex and changing phenomena that occur simultaneously during ingot solidification. In particular, many attempts have been made to refine the as-cast structure of ingots, with special emphasis on the columnar grains. The formation of large columnar grains is generally considered harmful to the further fabrication of an ingot. It may also result in undesired ani-sotropic properties. However, columnar grains are not undesirable in all grades, or product applications, and caution must be exercised to determine in which grades and applications columnar grains are not desired in the ingot. Although the literature on the refinement of as-cast ingot grain structures is too vast in general to review here, it is noteworthy that such methods are additions of artificial nuclei, mold vibration, mechanical stirring or ultrasonic agitation of the molten metal, and controlled cooling and reheating during solidification have been tried with varying degrees of success. However, it is doubtful that any method of refining the as-cast ingot grain structure has been completely successful on a commercial basis. The purpose of

Jan 1, 1962

By J. H. Swisher

In measuvements of the solubility of nitrogen in fer-rilic Fe-P alloys, tile nitrogen solubility is found to be Less in pIrospliorus-bearing alloys than in pure iron. The reduction in solubility is about 20 pct in a 1.0 wt pct P alloy at 1300°C and about 30 pct in a 0.23 wt pct P alloy at 440°C. Diffusion coefficient measurements at 1150 and 585°C show that phosphorus also decreases the nitrogen diffusivity in iron. In previous work on the Fe-P-N system, phosphorus was found to reduce the nitrogen solubility in liquid iron slightly.&apos; Indirect evidence for similar behavior in a Fe at low temperature was obtained by Dickenscheid and Brauner.&apos; These authors found that phosphorus reduces the height of the internal-friction peak due to dissolved nitrogen. The results of Dickenscheid and Brauner were confirmed by J. C. Swartz of this Laboratory in a single internal-friction experiment using the same specimen stock as in the solubility measurements described below. In the present investigation, the solubility of nitrogen in a fer rite-stabilized Fe-1.0 wt pct P alloy was measured in the temperature range from 800" to 1300°C. Additional experiments were performed in the temperature range from 440° to 585°C, using an Fe-0.23 wt pct P alloy and NH3-H2 gas mixtures. EXPERIMENTAL The experiments were performed in a vertical tube furnace wound with platinum wire. For experimental temperatures of 800°C and above, a mixture of 5 pct Hz in N2 was used as the reacting gas. The gas mixture was prepurified from oxygen by passage over platinized asbestos at 450°C, and subsequently over anhydrone to remove water. Flow rates of the gases were measured with capillary flow meters. The temperature was measured before and after each experiment with a Pt/Pt-10 pct Rh thermocouple. The specimens used for the high-temperature solubility measurements were in the form of rectangular plates, 0.534 by 1.6 by 3.8 cm. The specimens were cleaned in trichloroethylene and annealed for 2 hr in hydrogen at the beginning of each experiment. In measuring the nitrogen solubility, the specimens were held in the reacting gas until equilibrated, then cooled in a water-cooled copper block at the bottom of the furnace. The time needed for equilibration at 1150°C was determined by measuring the average nitrogen content of the 1.0 pct P alloy as a function of reaction time. As will be described, the nitrogen diffusivity in the alloy at 1150°C is only slightly less than its calculated diffusivity in pure iron. At temperatures other than 1150°C, the reaction time used in measuring the nitrogen solubility was about twice the calculated equilibration time for pure iron at the same temperature. With a few exceptions, the procedure for the low-temperature solubility measurements was the same as that described above. The compositions of the NH3-H2 gas mixtures were determined by collecting gas samples from the gas train and analyzing them for NH3 by titration with HC1. The specimen thicknesses were less than those used for the high-temperature experiments, eg., 0.124 and 0.051 cm for measurements at 585° and 440°C, respectively. Nitrogen concentrations were obtained by chemical analysis, using the Kjeldahl method. The Fe-P alloys were made by adding ferrophos-phorus to electrolytic Plastiron (Type 104 A). Commercial ferrophosphorus, containing 3 pct Mn and 0.35 pct Si as the major impurities, was first purified by melting under an FeO slag. In a separate heat, the electrolytic iron was melted and vacuum-carbon-deoxidized prior to making the ferrophosphorus addition. The principal impurities and their concentrations in weight percent in the 1.0 pct P alloy are as follows: Mn, 0.01; Si, <0.01; C, 0.01; 0, 0.003; and N, 0.0012. The impurity levels in the 0.23 pct P alloy are con-

Jan 1, 1968

By Herbert E. Field

The study of the condition and action of carbon in iron and steel is singularly complicated, because one has to consider, also, many contemporaileous reactions foreign to the one under investigation. Great difficulty is experienced in studying iron in the melted state, or during its various treatments in a solid condition, hence such an inquiry must be confined chiefly to a study of the original substance, of the conditions surrounding its treatment, and of the finished product. From a knowledge of these three things, we must form our own conclusions as to what takes place during the transition-period. Inasmuch as it is impossible to determine quantitatively the changes which take place in iron during the various processes of treatment and alteration, we are forced at once into the field of theory for an explanation of many of the phenomena for which we have to account. A recapitulation of the recognized properties of iron and carbon, and of the conditions in which they exist in iron and steel, may be useful as an introduction to the discussion of the subject. Chemically pure iron is soft, malleable and easily welded. It carmot be hardened or tempered, as these terms are understood in relat.ion to steel. In contact with a magnet, it becomes magnetic, but loses this property when the magnet is removed. It is unfitted for castings on account of its lack of fluidity. Those properties of iron which render it valuable as a commercial product must, therefore, be primarily due to foreign substances contained in the iron; and the great variety of these properties is attained by changes in the amount and nature of these impurities, and by the physical treatment of the iron while it contains them. The following properties of carbon make it a prominent factor

Jan 1, 1904

By J. C. Deppe

A method is presented for calculating approximate injection rates in secondary recovery operations. The method can be applied to cases of unequal fluid mobilities, irregular well patterns and boundary patterns. The steady-state pressure distributions for the four flood patterns reported by Muskat and for five additional patterns reveal that most of the difference in pressure between the injection and producing wells occurs in regions around the wells which can adequately be described as regions of radial flow. This leads to a method of calculating injectivity by approximating the flood pattern with radial flow elements (or a combination of radial- and linear-flow elements for some patterns such as the direct line drive). Irregular and boundary patterns can also be approximated by radial and linear elements. Each of these elements can be described by radial-and linear-flow equations and the results combined as series flow resistances to give an approximate equation for the initial injection rate. The mobility ratio does not affect the initial rate; therefore, if the well pattern is one of those regular patterns for which theoretical rate equations have been derived for unity mobility ratio, the approximate initial rate equation can be improved by adjusting it to match the theoretical equation. The available theoretical rate equations are listed, including five new cases. As the flood progresses, the injectivity changes because in general the flood front will divide the pattern into areas of different fluid mobilities. Simple shapes can be assumed for the flood front so that both areas can be divided into radial- and linear-flow elements. Radial- and linear-flow equations are applied to these elements to account for the change in flow resistance behind the front. To calculate injection rates after breakthrough, it is necessary to know the sweep efficiency at breakthrough. Areal sweep data are available in the literature for a number of patterns, and sufficiently accurate breakthrough sweep efficiency can be estimated from these data if it is not otherwise available. Again, simple shapes for the flood front can be assumed after breakthrough, and injection rates can be calculated for the remainder of the flood. When areal sweep data are available, these data can be used to cbeck. the calculated injection rates after breakthrough. Injection rates calculated by this approximate method compare favorably with available model data. INTRODUCTION When the fluid mobilities in the swept and un swept regions are equal, the injectivity will not change as the flood front advances; and for regular patterns it can be calculated by mathematical formu1as.l When the fluid mobilities in the swept and unswept regions are not equal, the injectivity will increase or decrease as the flood front advances. In this case, the injectivity has not been calculated by analytical means for any practical well pattern; and, furthermore, scale model and analog4,6 results have been published only for the five-spot pattern. The main object of this paper is to present an approximace method for calculating injectivity for the case of unequal mobilities. The method can be applied to regular, irregular and boundary patterns. Before the approximate method is discussed, the analytical formulas for equal mobilities will be summarized, and the analytical solution for radial flow with unequal mobilities will be used to show how the injectivity changes as the flood progresses. EQUAL MOBILITIES, REGULAR PATTERNS In a flooding operation the injectivity, the rate at which fluid can be injected per unit difference in pressure between injection and producing wells, depends on basic physical properties and, in addition, on three variables to be treated here—the area of the swept region, the fluid mobilities in the swept and unswept regions, and the well geometry (pattern,

By Luke L. Y. Chang, Bert Phillips

A number of molybdenum oxides have been synthesized and their crystal structures have been described.&apos; No data have been published on the stabilities of these oxides nor on the phase relations in the system Mo-0. It is probable that the tendency toward oxidation of both the metal and the oxides with low oxygen content in addition to the high volatilization rate of the oxides with high oxygen content have precluded accumulation of reliable data for establishing phase relations. These problems make experimentation difficult, but a modifi-

Jan 1, 1965

By E. W. Mehal, R. W. Haisty, D. W. Show

The next generation of integrated circuits will probably include circuits constructed in and of GaAs. The existence of both semi-insulating and semiconducting forms of GaAs is the fact which will bring this about. In this paper we discuss the uses and limitations of semi-insulating GaAs for integrated-circuit applications. The two main areas considered are the electrical isolation that can be achieved between components on a semi-insulating substrate and the characteristics of p-n junctions in contact with semi-insulating GclAs. A process basic to attaining integrated circuits in GaAs to fully utilize the insulating properties of the substrate is selective epitaxial deposition. This process involves the deposition of a SiO2 layer onto a The trend in integrated circuits is towards the use of high-resistivity substrates or regions to achieve component isolation. The use of SiO, layers in the oxide isolation methods and the use of sapphire substrates are examples of this idea. GaAs is also a polished surface of a GaAs substrate, etching out selected area of the SiO, film to expose a GaAs surface, and deposition only onto the exposed GaAs surface. By using this process , islands of semiconducting GaAs are deposited onto a semi-insulating GnAs substrate, the islands being electrically isolated from one another by the substrate. The deposition of both p- and n-type semiconducting GaAs can be carried out in this nzanner to form p-n junctions in the island areas. This process can also be used to produce a planav structure by deposition of GctAs through a SiO, mask into holes etched into the GaAs substrate. This Putterned Epitaxial Technology (PET) is described. very promising material for use in future integrated circuits because of the existence of both semi-in-sulating and semiconducting forms. Active devices can be fabricated in the semiconducting material, and these individual components can then be electrically isolated from one another by using semi-insulating GaAs as the substrate. Epitaxial semi-insulating GaAs can also be produced thus making three-dimensional monolithic integrated circuits feasible.&apos; This paper describes the research aimed at developing the methods for producing both two- and three-dimensional integrated circuits in GaAs, and examines some of the properties of semi-insulating GaAs as they relate to these integrated circuits.

Jan 1, 1967

Jan 1, 1971