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By J. Rogers, H. F. A. Hergt, K. L. Sutherland

IN 1938 Ralston4 reviewed the many attempts to find a satisfactory collector for the separation of cassiterite from its ores and in 1944 Dean and Ambrose2 summarized some further attempts. Generally, soaps and amines are effective but nonselective collectors. We have discovered that reagents containing either the polar group -SO4- or _S03- are excellent collectors for cassiterite and promise to be selective.1 The response to these reagents of cassiterite and of minerals commonly associated with it was studied, using the captive-bubble technique. Using these fundamental data, the practicability of separation and concentration of tin was investigated by flotation tests in a 2000gram Denver cell. EXPERIMENTAL METHODS Reagents All inorganic reagents were of Analar grade. The preparation and purification of sodium cetyl sulphate, cetyl trimethyl-ammonium bromide, laurylamine and cetylamine have been previously described.5 The other collectors were commercial surface-active agents, which were used without purification. Tests Captive-bubble Tests and Cylinder Flotation Tests have been previously described.5-10 The full lines shown in the figures relating solution composition to contact (flotation) distinguish solutions in which contact (flotation) is possible from those in which it is not. The curve is derived by successive approximation and the accuracy is ±0.2 pH units and ± 5 mg. per liter of collector or depressant. Solution compositions for which it was shown experimentally that contact or flotation is possible are marked by a circle, those for which it is not possible, by a cross, and those for which it is doubtful by a cross within a circle. It is assumed that at all other solution compositions within (without) the curve, contact or flotation is possible (not possible). After testing in the collector solution, the mineral was removed, washed, and tested by the captive-bubble method in water, or floated in a cylinder with frother only. In this way the composition of solutions in which a mineral was conditioned but in which properties of the collector solution prevented contact or flotation can be defined. The composition of solutions in which conditioning was possible lie between the full and broken curve, and the experimental results are indicated by a square. The curves show the limits of composition of solutions in which flotation in a cell would be possible but many factors other than those considered in these tests determine recovery and grade of a given mineral in practice. Flotation Tests in 500 and 2000-gram Denver Submachines.--Melbourne tap water, containing 12 parts calcium, 6 parts

Jan 1, 1947

By Z. F. Oszter, D. Vincent, W. K. Behrands

With the expansion of open pit operations, belt conveyors are going to be used in the 13 608 to 18 144 t/h (15,000 to 20,000 stph) capacity range, which calls for a review of some of the horsepower calculation methods. This paper presents methods (based on German research data, field tests and theoretical considerations) for the evaluation of the Ky factor in the CEMA formula for belt conveyors of large carrying capacity, which fall beyond the limits of the data given in tables in the CEMA book. (The CEMA limits are 407 N\\m (300 lb ft) and Tave = 7.3 Mg (16,000 lb). At these large loads, the impression resistance of the belting on the idlers plays a major role, which in turn influences the magnitude of the drive horse power required. An example will illustrate the order of magnitude difference of the horsepower values obtained by using a conventional calculation method and the suggested method, as well as the beneficcia1 influence of the 4-roll idler in comparison to the standard 3-roll unit for a large caving capacity belt conveyor. This paper concerns itself with the analysis of the resistance to motion of belt conveyors, emphasizing the evaluation of the frictional resistance to motion due to load and belt pressure on the idlers and the flexing resistance of the belt and material when passing over the idlers. In the case of long and heavily loaded belt conveyors, the aforementioned resistances reach extremely high values calling for close analysis of the phenomena, presently not calculable with normally used formulas. This paper establishes correlation between experimental and empirical data presenting practical formulas a tool for the designer of high-capacity belt conveyors. The application of the formula is illustrated in an example in the Appendix.

Jan 1, 1981

By H. F. A. Hergt, K. L. Sutherland, J. Rogers

In 1938 Ralston4 reviewed the many attempts to find a satisfactory collector for the separation of cassiterite from its ores and in 1944 Dean and Ambrose2 summarized some further attempts. Generally, soaps and amines are effective but nonselective collectors. We have discovered that reagents containing either the polar group — SO4- or — SO3- are excellent collectors for cassiterite and promise to be selective. The response to these reagents of cassiterite and of minerals commonly associated with it was studied, using the captive-bubble technique. Using these fundamental data, the practicability of separation and concentration of tin was investigated by flotation tests in a 2000-gram Denver cell. Experimental Methods Reagents All inorganic reagents were of Analar grade. The preparation and purification of sodium cetyl sulphate, cetyl trimethyl-ammonium bromide, laurylamine and cetylamine have been previously described.5 The other collectors were commercial surface-active agents, which were used without purification. Tests Captive-bubble Tests and Cylinder Flotation Tests have been previously de- scribed.5,10 The full lines shown in the figures relating solution composition to contact (flotation) distinguish solutions in which contact (flotation) is possible from those in which it is not. The curve is derived by successive approximation and the accuracy is ±0.2 pH units and ± 5 mg. per liter of collector or depressant. Solution compositions for which it was shown experimentally that contact or flotation is possible are marked by a circle, those for which it is not possible, by a cross, and those for which it is doubtful by a cross within a circle. It is assumed that at all other solution compositions within (without) the curve, contact or flotation is possible (not possible). After testing in the collector solution, the mineral was removed, washed, and tested by the captive-bubble method in water, or floated in a cylinder with frother only. In this way the composition of solutions in which a mineral was conditioned but in which properties of the collector solution prevented contact or flotation can be defined. The composition of solutions in which conditioning was possible lie between the full and broken curve, and the experimental results are indicated by a square. The curves show the limits of composition of solutions in which flotation in a cell would be possible but many factors other than those considered in these the determine recovery and grade of a given mineral in practice. Flotation Tests in 500 and 2000-gram Denver SUbmachines,—Melboume tap water, containing 12 parts calcium, 6 parts

Jan 1, 1947

By J. Rogers, H. F. A. Hergt, K. L. Sutherland

In 1938 Ralston4 reviewed the many attempts to find a satisfactory collector for the separation of cassiterite from its ores and in 1944 Dean and Ambrose2 summarized some further attempts. Generally, soaps and amines are effective but nonselective collectors. We have discovered that reagents containing either the polar group — SO4- or — SO3- are excellent collectors for cassiterite and promise to be selective. The response to these reagents of cassiterite and of minerals commonly associated with it was studied, using the captive-bubble technique. Using these fundamental data, the practicability of separation and concentration of tin was investigated by flotation tests in a 2000-gram Denver cell. Experimental Methods Reagents All inorganic reagents were of Analar grade. The preparation and purification of sodium cetyl sulphate, cetyl trimethyl-ammonium bromide, laurylamine and cetylamine have been previously described.5 The other collectors were commercial surface-active agents, which were used without purification. Tests Captive-bubble Tests and Cylinder Flotation Tests have been previously de- scribed.5,10 The full lines shown in the figures relating solution composition to contact (flotation) distinguish solutions in which contact (flotation) is possible from those in which it is not. The curve is derived by successive approximation and the accuracy is ±0.2 pH units and ± 5 mg. per liter of collector or depressant. Solution compositions for which it was shown experimentally that contact or flotation is possible are marked by a circle, those for which it is not possible, by a cross, and those for which it is doubtful by a cross within a circle. It is assumed that at all other solution compositions within (without) the curve, contact or flotation is possible (not possible). After testing in the collector solution, the mineral was removed, washed, and tested by the captive-bubble method in water, or floated in a cylinder with frother only. In this way the composition of solutions in which a mineral was conditioned but in which properties of the collector solution prevented contact or flotation can be defined. The composition of solutions in which conditioning was possible lie between the full and broken curve, and the experimental results are indicated by a square. The curves show the limits of composition of solutions in which flotation in a cell would be possible but many factors other than those considered in these the determine recovery and grade of a given mineral in practice. Flotation Tests in 500 and 2000-gram Denver SUbmachines,—Melboume tap water, containing 12 parts calcium, 6 parts

Jan 1, 1947

By James R. Evans

Forecasting demand is an art as well as a science, and much personal judgment is required. National forecasts made for sand and gravel, crushed stone, and/or aggregate may be misleading or unhelpful locally. This is because of significant variation in demand within different geographic and/or political areas in the US, and/or the use of an inadequate data base and forecasting methodology. The best forecasts may be made for local or regional market areas, irrespective of geographic or political boundaries, provided a proper data base is available.1 The Bureau of Mines compiles detailed statistics on commodities sold or used in the construction industries and, therefore, is in an advantageous position to make national aggregate demand forecasts. Definitions of some terms used in this presentation are necessary before proceeding.

Jan 1, 1980

By S. Jana, C. M. Wayman

The reverse transformation of bcc martensite to the fcc phase was studied in an Fe-33.95 wl pct Ni alloy by nzeans oj dilatometry, melallography, and electron microscopy. Upon "slozc" heating (-1°C per min) length cJmnge us temperature plots showed u gradual contracLion over the temperature range 200" to 280"C ,followed by a more abrupt contraction beginning a1 -280°C. Howet,ev, zchen the heating rate was increased -4°C per tnin, no gradual contraction was observed and only the abrupt contraction starting at -2BO"C was found. Thus on slower heating- the AS "temperature" for the subject alloy, unlike the MS temperature, is better defined as a range of temperatures. Both optical and transmissiorl electron microscope observations showed that some of the martensite plates exizibited a partial loss of transformation twins during reversal. The midvib region of the martensite plates disappeaved relatively early duirng the reversal. Metallographic observations slowed that the earliest detectable stage of the rezlerse tvansforrvration begins (axd Moues inulardly) at The Martensens i te - parent interface. At higher temperatirres, the. formation of martensitically reversed jcc plates within the bcc martensite plales was observed. It is concluded that the reverse transformation consists of a diffusion less process (martensitic); but this is ps-obably aided by a prior or simultaneous dijjusiorz-comltvolled process, at leasl in the case of slower heat-ing' experiments. ALTHOUGH numerous investigations have dealt with the parent-to-martensite ("forward") transformation (fcc — bcc) in Fe-Ni alloys, comparatively little is reported on the ("reverse7') martensite-to-parent transformation.'-4 Even though such reverse transformations have been studied in detail in some nonferrous systems, one of the difficulties of studying the reverse transformation in most ferrous mar-tensites is that the martensite decomposes by tempering during heating. However, carbonless Fe-Ni alloys do not exhibit this difficulty since the transformation in these alloys is completely reversible. The present investigation represents an attempt to shed more light on the nature and mechanism of the martensite-to-parent transformation. 1) EXPERIMENTAL PROCEDURE 1.1) Alloy Prepatation. Fe-Ni alloys of compositions near 34 wt pct Ni were prepared from zone-refined iron (99.994 wt pct Fe) and high-purity nickel (99.999 wt pct Ni) by induction melting in recrystallized alumina crucibles in an argon atmosphere, with prior vacuum evacuation to 10"3 mm Hg. The alloys were homogenized by induction stirring in the molten state for 5 min. After solidification, the alloys were further homogenized in evacuated quartz capsules for 96 hr at 1230°C. 1.2) Dilatometry. Slices of the ingot were hot-forged (750°C in air) into approximate rod form and these specimens were then hot-swaged (750°C in air) into long cylindrical rods 0.55 mm diam. From the rods, specimens about 1 in. long were cut. These were then vacuum-annealed for 24 hr at 1200°C, cooled to room temperature, and subsequently transformed to martensite in liquid nitrogen (whereby about 40 pct transformation was obtained). Dilatation measurements were made by observing length changes in a vacuum dilatometer with an externally mounted LVDT sensing element. 1. 3) Preparation of Electron Microscope Specimens. Slices of the ingots were cold-rolled (with intermediate vacuum anneals) to -0.020 in. Out of these rolled sheets, specimens (about 1 by 1 in.) were cut. These were then vacuum-annealed, transformed to martensite by cooling in liquid nitrogen, and subsequently heated from room temperature to various temperatures to effect either partial or complete reverse transformation. These specimens were then chemically polished to 0.002 in. in l:l HsOz (30 pct) and &PO4 (85 pct) solution, and thinned to electron transparency in an electrolyte consisting of 150 g CraOs, 750 ml glacial acetic acid, and 30 ml ~~0.~ Observations were made with a 100-kv Hitachi HU-11 electron microscope equipped with an HK-2A tilting device. 1.4) Optical Microscopy. Metallographic observations were made with a Leitz MM5 metallograph on the same 0.020-in. sheet specimens as were used for electron microscopy and on bulk specimens which were 0.2 in. or more on a side. The chemical thinning solution when cooled below 20°C also served as an etchant for this alloy. Observations of surface relief were made with a Zeiss interference microscope employing a Thallium light source of wavelength 0.54 p. Specimens for interference studies were prepared by two-stage polishing on Buehler vibromet polishers using 0.3 and 0.05 p alumina abrasives. 2) EXPERIMENTAL RESULTS 2.1) Comparison of the MS,AS, and Af Tempera-tures wTth Previous Re sults. The AS aLd Af tempera -tures of several Fe-Ni alloys were determined dila-tometrically. The MS temperatures of the same alloys were determined by continuously lowering the temperature using a mixture of isopentane and liquid nitrogen and observing the highest temperature at which a prepolished specimen showed surface upheavals. For the present the As temperature is defined as the temperature at which an abrupt decrease in length occurs in the dilatation plot. The Ms,As7 and A determinations in the present investigation and those of Kaufman

Jan 1, 1968

By AIME AIME

STEADY advance has been made in the art of lead smelting and refining during the year. The bringing of natural gas to the Salt Lake valley has led to its adaptation to lead smelting operations. The Tooele plant of the Anaconda Copper Mining Co. has put into practice the high blast pressure and constant volume for lead blast furnaces, which we understand was first advanced by John F. Austin. It would appear that within limits, capacity is nearly proportional to the volume of air. If the charge is dense, a constant pressure, as in the old practice. did not get much air through the charge and the furnace slowed up. The constant volume idea makes the charge smelt at the same rate as if the charge were porous. The cost of a little additional power insures capacity operation at all times.

Jan 1, 1932

By A. A. Venghiattis

This paper is discussed not because of its intrinsic value but because it has been related by its authors to the oilwell gun perforators. It is well known that conditions almost ever present in oilwell perforations are the overburden and the presence of the casing. Because of the lack of information in the paper on the dimensions or confinement of the target rocks, one is led to guess that they were not confined at all and, particularly, that no steel front plates were used on the impact face of the rocks to materialize the presence of the cemented casing. This situation, plus the fact that small steel balls have been used as projectiles instead of actual bullets, makes the whole thing unapplicable to oilwell perforation. When shooting is performed against target rocks confined (as shown on Fig. 1) in such a way as to give a fair image of the overburden applied to the formation to be perforated, as well as of the cemented casing, the following are found. 1. There is no cratering worthy of mention, even with bullets having 10 times higher impact energy per unit projected area than the steel balls mentioned in the article. This has been confirmed with sandstone as well as with other rocks (granite, limestone and chalk). See Figs. 2 and 3. 2. Penetrations vary closely as the logarithm of the impact velocity. On this matter I have established the relation

By H. A. Lequear, J. D. Lubahn

A sudden change from one constant strain rate to another during a tensile test causes an unusual transient in aluminum alloy 61ST. A sudden change from one constant stress to another during a creep test does not produce an unusual transient in this material. A specially devised test shows that the nature of the previous steady-state conditions, which the sudden change disturbs, is one of the factors affecting the transient behavior. Some of the observations may be explained in terms of strain aging. USUALLY a sudden change during a tensile test from one constant strain rate to another causes a small, abrupt vertical shift from one stress-strain curve to another, parallel one. This behavior is apparently characteristic of all metals at very low temperatures and of many metals for wide ranges of temperature. It is illustrated in Fig. 1 for some early data on 61ST tested at — 195oC, and in Fig. 2 for some recent data on copper at room temperature. The greater accuracy of the results of Fig. 2 over previous ones' is due to the equipment shown in Fig. 3. Three levers apply the bulk of the load, while the changes in the small remainder load are indicated sensitively by a low capacity load scale. Refs. 2 and 3 describe the recording equipment. A test like those in Figs. 1 and 2 provides the information necessary to determine the rate sensitizrity, n,4 of the metal. ( a log s ) ? log s n = ------------------------ ----------------------------= ( a logs e, ? log e logS2-logS1 log S2/S1 log i2 — log e1 log e2/e1 where S equals stress: e is logarithmic strain or natural logarithm of (final gage length/initial gage length);" i is strain rate or de/dt: and n is rate sensitivity, rate of change of log stress with log strain rate at a given strain, or (a log S/a log i),. Normally, the rate sensitivity, n, is positive, which means that an increase in stress causes an increase in rate. However, certain exceptions, attributed to strain aging,5 have been observed. Fig. 2 indicates how rate sensitivity values are derived from the measurements. Table I summarizes the rate sensitivity values derivable from Fig. 1. In contrast to the behavior of copper in Fig. 2, the aluminum alloy 61ST, which strain ages when tested near room temperature, exhibits an unusual transient when the strain rate is suddenly changed,' as shown in Fig. 4. Initially, there is a comparatively sudden vertical shift of the stress-strain curve in a direction corresponding to the rate change, but then the curve gradually shifts back again. The initial shift is not as sudden as might be expected, because the testing machine is unable to achieve the impressed rate change instantaneously, as illustrated in Fig. 2. The behavior shown in Fig. 4 will be referred to as a tensile transient, the word tensile implying that the behavior was observed in a tension type of test. The corresponding test, where the strain rate is maintained constant except for the sudden change, will be called a tensile transient test. A creep transient, by contrast, will be defined as a temporarily abnormal behavior in a creep transient test, where there is a sudden change from one constant load to another.' In Fig. 4, a naive look at the gradually decreasing and then increasing load after a sudden rate incre-

Jan 1, 1957

By C. Y Garber

Interest in the sink-float plant operated by the Bunker Hill and Sullivan Mining and Concentrating Co. at Kellogg, Idaho, has recently been largely confined to the preparation and reconditioning of the galena medium. The ease and simplicity of these operations in a concentrating mill producing a flotation lead concentrate has occasioned enough comment to possibly justify a brief description. The subject is treated from an operator's viewpoint only; no effort is made to discuss it in a theoretical or technical manner. Plant at Bunker Hill The sink-float plant was first operated in December 1941. It was built for the purpose of quickly increasing mill capacity with a minimum of equipment. It is the Huntington-Heberlein sink and float process using galena medium and is operated under license from the Sink and Float Corporation, New York city. Lead-zinc ore from the Bunker Hill mine is crushed to pass a 1¼ in, screen and is then washed and separated on vibrating screens having 4½-mm. round-hole punched plates. The screen under-size, amounting to 33 per cent of the mill feed, is dewatered and sent to the ball-mill feed bins. The screen oversize goes to the sink-float plant, where 50 per cent of the oversize, or 33 per cent of the mill feed, is float, which is washed free of medium and disposed of as a tailing. The remaining 33 per cent is sink, which, after washing, is crushed to pass 36 in. and joins the under-size in the ball-mill feed bins. The normal plant capacity is 1700 tons per 24 hr. About 1.7 per cent of the total lead and 3.3 per cent of the total zinc in the feed is lost with the sink-float tailings (Table I). More complete descriptions of the H. H. process and Bunker Hill sink-float plant are given in several recent articles, listed at the end of the paper. Preparation OF Medium at Bunker Hill New medium is made intermittently as needed, usually 12 hr. in each 6 days. A small portion of the current mill flotation concentrate is diverted from the lead cleaner cells to a I-in. vertical sand pump and pumped to a two-cell 36-in. Agitair flotation machine, where NaCn and ZnSO4 are added and the grade of concentrate is improved as shown in Table 2. Tailing from this operation is returned by gravity

Jan 1, 1947

By C. Y. Garber

Interest in the sink-float plant operated by the Bunker Hill and Sullivan Mining and Concentrating Co. at Kellogg, Idaho, has recently been largely confined to the preparation and reconditioning of the galena medium. The ease and simplicity of these operations in a concentrating mill producing a flotation lead concentrate has occasioned enough comment to possibly justify a brief description. The subject is treated from an operator's viewpoint only; no effort is made to discuss it in a theoretical or technical manner. Plant at Bunker Hill The sink-float plant was first operated in December 1941. It was built for the purpose of quickly increasing mill capacity with a minimum of equipment. It is the Huntington-Heberlein sink and float process using galena medium and is operated under license from the Sink and Float Corporation, New York city. Lead-zinc ore from the Bunker Hill mine is crushed to pass a 1¼ in, screen and is then washed and separated on vibrating screens having 4½-mm. round-hole punched plates. The screen under-size, amounting to 33 per cent of the mill feed, is dewatered and sent to the ball-mill feed bins. The screen oversize goes to the sink-float plant, where 50 per cent of the oversize, or 33 per cent of the mill feed, is float, which is washed free of medium and disposed of as a tailing. The remaining 33 per cent is sink, which, after washing, is crushed to pass 36 in. and joins the under-size in the ball-mill feed bins. The normal plant capacity is 1700 tons per 24 hr. About 1.7 per cent of the total lead and 3.3 per cent of the total zinc in the feed is lost with the sink-float tailings (Table I). More complete descriptions of the H. H. process and Bunker Hill sink-float plant are given in several recent articles, listed at the end of the paper. Preparation OF Medium at Bunker Hill New medium is made intermittently as needed, usually 12 hr. in each 6 days. A small portion of the current mill flotation concentrate is diverted from the lead cleaner cells to a I-in. vertical sand pump and pumped to a two-cell 36-in. Agitair flotation machine, where NaCn and ZnSO4 are added and the grade of concentrate is improved as shown in Table 2. Tailing from this operation is returned by gravity

Jan 1, 1947

By L. Adler

Any design of a mine roof in bedded deposits which ignores differential deflections at the supports can quickly lead to dangerous overstressing. As illustrated by the typical case presented on page 1029, if one support deflects only 0.1 in. more than its neighbor, stresses 50 pct higher than anticipated will result. Previous studies1-3 have assumed that the mine roof acts like a beam clamped at both ends, with no deflection or slope' at the supports (Fig. 1). Essentially this assumes:5* ?A = ?, = ?b and dA = dB = 0. However, a host of conditions can cause differential sag or deflection at one support, and even an apparently trivial deviation can have major consequences in the beam: variations in spacing, size, and material of supports; local settlement due to floor heaving or lower mine openings; non-uniformity in wedging or bolt tensioning.8 In one particular instance concrete pillars, poured in place, shrank away from the roof upon setting.' When understood and controlled, differential sag becomes a definite advantage, permitting the transfer of loads from one support to another. Where one support is a bolt or prop and the other a pillar or rib, the load on the former can be reduced while the load on the pillar or rib is increased. This means two things: 1) savings can be effected by using smaller artificial supports such as props and bolts and 2) loads can be increased in the rib to induce eventual failure for longwall caving. In this last respect, another factor underlying coal bumps becomes understandable. The design of a mine roof by beam theory assumes that when a bedded formation is homogeneous, iso-tropic, and elastic, it will act like a uniformly loaded beam, fixed or clamped at both ends,6 s in Fig. 1.'" These are important assumptions. The uniform load is the weight of the beam itself or its body load. For a beam of unit width, this load becomes per foot: w = yhb. w = uniform load y = specific weight, lb per ft3 h = depth or thickness of beam, ft b = width of beam, ft Since b = 1, w - yh [ 1 ] A beam fixed at both supports is statically indeterminate to the second degree, that is, two equations in addition to those for static equilibrium are required to determine the reactions at the supports. These equations result from the geometry. From statistics: ^F,= 0;RA + RB — wL = 0 [2] wU S,M0 = 0 ; MB H------------MA — RBL = 0 [3] it Using superposition in which the left support is kept intact and the right one resolved into an active force and moment, we obtain from Fig. 2:" ?b = ?m + ? b2 + ?B3 = 0 dB = dB1 + dB2 + dB3 / wU Ma RBL \ V d°=(-r+-2—r)-zr [5] Where: Subscripts refer to position on axis of beam R = force, lb M = moment, ft-lb w = uniformly distributed load, lb per ft L = span, ft 0 = slope, radians d = deflection, ft E = Young's Modulus, lb per ft" 1 = Moment of inertia about the neutral axis, ft4 Solving Eqs. 2 through 5 for the four unknown reactions, we obtain: 2 L3 Fig. 3 is obtained by plotting MA and M, vs d, and then plotting RA and R, vs d, and adjusting their scales to coincide with MA and M, vs d,. It should be noted in Eqs. 6 and 7 that as dB increases, MA increases the same amount that Mn decreases. Eqs. 8 and 9 show a similar relationship between RA and R,. Proof that MA is the maximum absolute moment occurring in the beam is as follows: where M, = moment at x wx-When where M,., = maximum positive moment Eqs. 6 and 8 into above: For small dn: MA> M,,,

Jan 1, 1960

By M. J. Marcinkowski, D. Koskimaki, A. S. Sastri

THIS is the second in a trilogy of investigations carried out in order to understand the solid state transformations and their accompanying effects on the deformation behavior of near-equiatomic Ni-Ti alloys. The first stage of this effort has dealt with the strictly martensitic structures obtainable in these alloys, i.e., those in which diffusion processes were not involved.1,2 These martensites could be produced either by rapid quenching or by plastic deformation of the originally B2 type phase. The present investigation, on the other hand, will deal with those transformations in Ni-Ti which do involve diffusion. A majority of investigators3-10 have shown that the B2 modification of TiNi, which is stable at elevated temperatures, decomposes into one or both of the intermetallic compounds NiTi2 and Ni3Ti below about 650°C. On the other hand, this has been disputed by several Workers was undertaken in order to resolve this discrepancy, as well as to shed more light on the nonmar-tensitic decomposition of B2 NiTi. EXPERIMENTAL PROCEDURE Sample preparation, fabrication, and examination were the same as those described previously in Ref. 2. In addition to the 50 at. pct Ni (55.06 wt pct) hypoeu-tectoid alloy used previously, a second hypereutectoid alloy containing 54.4 at. pct Ni (60 wt pct) was also prepared for this study. RESULTS AND DISCUSSION The equilibrium diagram for the Ni-Ti alloy system in the vicinity of Ni-Ti is shown in Fig. 1. The solid lines have been established by the work of Poole and ~ume-Ftothery4 whereas the dotted lines are based on findings obtained in the present investigation as described below. Structure and Morphology. Fig. 2(a) shows a bright field transmission electron micrograph of a two-phase structure obtained in a polycrystalline Ni-Ti alloy that was furnace cooled (approx 200°C per hr) from 1050' to about 300°C. Large plate-shaped precipitates can be observed in a matrix which was found by electron diffraction to possess the high temperature B2 structure. A selected area diffraction pattern of the region covered by Fig. 2(a) is shown in Fig. 2(b), while Fig. 2(c) is a detailed schematic interpretation of Fig. 2(b). The B2 matrix reflections are illustrated by squares while those of the precipitate are shown as circles. The d values associated with the precipitate reflections could be determined quite accurately since the reflections from the B2 matrix, for which the lattice constant is known precisely, were simultaneously present in the diffraction patterns. All of the reflections

Jan 1, 1970

By T. E. Evans, C. T. Baroch

ZrB2 was produced in batches of 4 to 6 Ib by interaction of ZrO2, B4C, B203, and carbon at around 2000°C in a simple graphite resistance furnace. Techniques of production are discussed and the final design of a suitable furnace is described in detail. Several other borides were made by the same technique and the process appears to have possibilities for commercial production. N seeking out new hard and refractory com- pounds, many researchers have turned to the investigation of the borides and excellent papers have been published on the properties of these compounds. Few papers, however, have appeared on the techniques and problems concerned with the production of these high temperature substances. This report describes progress made in developing a method for preparing zirconium diboride, ZrB2, on a pilot plant scale. The literature of the borides and other refractory hard metals recently has been reviewed, annotated, and classified so completely' that it is needless to attempt such an outline here. It is enough to say that three borides of zirconium have been reported: ZrB, ZrB2, and ZrB12.2 ZrB2 is the most stable of these and is especially stable in the presence of carbon up to and including its melting point of around 3000°C. Like most borides, it can be prepared in several ways. It can be prepared by synthesis of the elements, but these are expensive and difficult to produce in a high state of purity. Obviously, production directly from the oxides would have decided economic advantages. In electrolytic production such as that of calcium boride,:' the product is recovered as a sludge mixed with electrolyte; and separation of product from adhering electrolyte and regeneration of the electrolyte is an involved and difficult process. The work on borides was started on a small scale in 1948. Late in 1949, Naval Ordnance expressed a specific interest in ZrB2 and the project then centered on this compound. After the usual experimental work necessary in a new field, ZrB2 of good quality was produced by heating mixtures of B4C, ZrO2, B2O3, and carbon to a temperature of about 2000 °C in a resistance-type electric furnace. Over 100 lb was made for experimental use tests, and the method of production probably could be expanded into a commercial operation. A similar process has been described by Kieffer and coworkers.' The main chemical problems were the development of proper charges to insure complete reduction of the elements, determination of the proper temperature range at which these reductions took place, and adoption of techniques necessary to pre- vent inclusion of such impurities as carbon and nitrides. The mechanical problems consisted of developing a simple practical furnace that would attain the high temperatures required and permit use of a controlled atmosphere when necessary and determining of suitable refractories. Both problems were solved by designing a crucible resistance furnace. Crucible Resistance Electric Furnace Attempts were first made to produce ZrB2 in an electric arc furnace, but such a furnace would not provide the degree of carbon control required for producing clean graphite-free borides, so it was decided to try working in a crucible. Obviously, the furnace would have to be constructed of graphite, as the temperatures required are too high for other refractories or heating elements. Crucibles were made by hollowing out segments of graphite electrodes, which were fitted with a cover and clamped between two electrodes so that the current passing through the thin wall of the crucible would generate heat, using the principle of the Helberger crucible furnace."? Preliminary tests with this type of furnace were encouraging and led to the furnace design shown in Fig. 1. The essential components were a thin-walled graphite crucible resting on a graphite block, which formed the lower electrode assembly, and a top electrode assembly swung from a pipe column making contact with the top of the crucible. The space around the crucible was filled with graphite prepared from waste electrodes crushed to about ¼ in. This packing had excellent insulating properties, both electrically and thermally, and could be removed easily and quickly from around the crucible by means of an industrial vacuum cleaner. The largest resistor crucibles were machined from 8 in. electrode stock and were 26 in. long, with a side wall Yi in. thick and a 1 in. bottom. Temperatures were determined optically by sighting down a 1 in. hole drilled longitudinally through the top electrode and the crucible cover. Sealing this hole at the top was a water-cooled brass sight-glass assembly, shown in Fig. 2. An opening was provided for a light flow of helium to keep the sight opening clear of smoke, and a glass prism above the sight glass changed the line of sight to the horizontal for easier reading. More recently, the prism and optical pyrometer were replaced by a photoelectric recording pyrometer. At first the charges were placed directly in the resistor crucible but this meant that everything had to be withdrawn from the furnace every time the charge was emptied. Later, smaller crucibles were made up that could be placed inside the resistor

Jan 1, 1956

By N. J. Grant, A. W. Mullendore

Three aluminum alloys of 0.94, 1.92, and 5.10 pct Mg, prepared from very high purity metals, were tested at 500°, 700°, and 900°F in creep rupture. The degree of strengthening through solid-solu-tion alloying and the effects on the deformation characteristics and fracture were examined. The ductility of the alloys as a function of stress and temperature was closely followed. STUDIES of the creep process in pure metals in recent years have done much to expand the understanding of the fundamental deformation and recovery processes that contribute to overall creep behavior. In order that this knowledge may be applied to commercial alloys, it is necessary to know the principles governing the effect of alloying on the mechanisms of creep. A limited amount of work has been performed in this field, but few investigators have attempted to follow the changes in particular creep mechanisms with alloying. Recently, studies of the effects of solid-solution alloying on the plastic properties of aluminum have been conducted by Dorn, Pietrokowsky, and Tietz,1 Sherby, Anderson, and Dorn,2 and Sherby and Dorn.3 This paper presents the results of an investigation of the effect of solid-solution alloying of high purity aluminum with magnesium on the creep-rupture properties, and correlates these observations with changes in the creep mechanisms. This work is thus an extension of the creep-rupture observations of Servi and Grant4,5 and the deformation studies of Chang and Grant.6,7 Experimental Procedure Three alloys of aluminum containing approximately 1, 2, and 5 pct Mg were tested. These alloying additions are all within the solid-solubility limit at the testing temperatures.' The analysis of the materials is presented in Table I. The tests fall into two categories: l—creep-rup-ture tests at 500°, 700°, and 900°F, and 2—structure study tests performed primarily at 700°F. Speci-mens of 0.160 in. diameter with milled flats for metallographic observations" ' were utilized for the structure studies. All specimens were annealed in one step to give the desired grain size for the tests. Table II presents the annealing data and final grain sizes. The specimens were polished electrolytically before testing with Jacquet solution (2/3 acetic anhydride, 1/3 perchloric acid) at 25" to 30°C, and 15 to 20 v. Creep-rupture testing was performed under constant load with the apparatus previously described." Results and Discussion Creep-Rupture Properties: The log-log plots of creep-rupture data are presented in Figs. 1 and 2. For these very pure single-phase alloys, the minimum creep rate and the rupture life both exhibit straight-line dependence on stress in this method of plotting as they have for commercial alloys0,10 and for pure aluminum." Curve breaks, based on the use of straight-line segments, at 500°F have been found by metallographic study to correspond to a transition from low to high temperature behavior and so represent zones of equicohesion. Specimens on the high creep-rate side of the break showed normal granular deformation processes whereas those on the low creep-rate side showed rapidly increasing grain-boundary sliding and migration with extensive evidence of intercrystalline cracking at 500°F. Two micrographs of the 0.94 pct Mg alloy, Fig. 3, show the increased participation of the grain boundary in the deformation process at 500°F with decreasing stress. In Fig. 3a is shown the structure of a specimen which exhibits little deformation along the grain boundaries and failed transgranularly; in Fig. 3b is shown the increased deformation along the grain boundaries at a lower stress for a specimen which showed appreciable intercrystalline cracking. The severity of intercrystalline cracking increased with increasing magnesium content at 500°F. Intercrystalline cracking disappeared in most of the specimens at 700°F and persisted only in the 5 pct Mg alloy at high creep rates. At 900°F all of the specimens deformed with extensive grain-boundary participation, including extensive grain-boundary migration. None of the alloys at 900°F showed intercrystalline cracking.

Jan 1, 1955

By S. R. Dunbas, D. C. Jillson, E. A. Anderson

THE present work was undertaken to furnish information, lacking in the literature, on the deformation mechanisms active in pure titanium at room temperature. Since it was started, Rosi, Dube, and Alexander' have indicated that slip can occur in coarse-grained (2 to 6 mm diameter) titanium on the {1010} and {1011} planes and twinning can take place on the {1072}, (1122) and (1151) planes. Liu and Steinberg,' working with titanium flakes produced by fused salt electrolysis, found evidence of twinning on the {1032$, {1121), {1122}, (1123}, and (1154) planes. The crystals used in the present work were substantially longer (up to nearly 2 in. in length) and possibly purer. Production of Large Crystals It was the purpose of this part of the work to provide single crystal or large grain specimens for use in the deformation studies rather than to study the mechanism of crystal growth. Accordingly, all further exploratory studies on methods were abandoned when it was found that cold-rolled bars sealed in vacuo in individual Vycor tubes and given three or more cycles of 4 hr at 1200°C and three to five days at 850°C, gave large grains. Eighteen specimens about 0.2 in. square x 2 in. long yielded 33 useful grains, ranging from Va in. to nearly 2 in. in length, with an agreeably wide range of orientations, Fig. l. The 0.25 in. thick strip from which the starting specimens were cut had been reduced 67 pct on 18 in. diameter rolls from a scalped, hot-forged (959" to 1000°C), arc-melted, iodide titanium ingot. Thc bar was at room temperature, but the rolls were at 200°C. Reductions of about 0.03 in. per pass were used. The bar was cut into four segments, each of which was rolled in a somewhat different manner. No effect on the growth of large grains was noted. The composition of the titanium, determined on turnings from the ingot scalping operations, is given in Table I. The Rockwell A hardness of the ingot was 26. The standard starting specimens, about 1/4x1/4x2 in., were milled on all four sides, hand polished on 280 and 400 mesh emery papers, etched for 3 min in a 50 HF-50 glycerine solution, rinsed, and dried in alcohol and ether just before sealing them in Vycor tubes. The average specimen weight was 7.5 g, and the tube volume was 6.5 cc. A vacuum of less than 1 micron pressure was applied. The specimen tubes were placed in an evacuated Inconel muffle to minimize the danger of collapse of the glass tubes at temperature. In practice the specimens were first heated to 1200 °C for 4 hr and then transferred fairly quickly to an 850°C furnace where they were held for three to five days. This cycle was repeated at least three times before the specimens were cooled, removed from the tubes, lightly polished and etched on one surface for examinstion. Those in which large grains had not developed were resealed in Vycor and returned to the cycling. Satisfactory specimens (about one out of every four cycled) were polished with emery paper on all four side;, then metallographically polished using ctchinz between wheels to remove distorted metal and, finally, given a very light etch to reveal the grain boundaries. This was necessary because the surface was roughened by the sublimation of titanium under high temperature vacuum conditions. Specimens were identified by TiXl numbers using supplementary letters to designate specific grains.

Jan 1, 1954

By Ralph Arnold

LESS than eight months ago at the annual meeting of the American Institute of Mining and Metallurgical Engineers, attention was called to the demoralizing effect of the abnormal oil production of Mexico on the oil situation in the United States, and it was predicted that this unstabilizing influence would probably become impotent in 18 to 24 months through ' the exhaustion of the principal producing fields of Mexico, unless new fields were found in- the meantime. When this statement was made, the daily production of Mexico was about 600,000 bbl. of crude oil; now it is about 350,000 bbl. No new pools of consequence have been opened, although extensions have been made to two old pools. Over 200,000 bbl., or more than half of the present daily production, comes from Los Naranjos, Amatlan and North Zacamixtle fields, in which practically every well is so affected by salt water that the potential production dropped 50 per cent. in the month of September, clearly indicating that these fields are moving rapidly toward extinction. How much longer the one remaining important pool will last is a matter of conjecture.

Jan 1, 1921

By Christie A. Callender, Harry M. Dahl

The Hobson uranium deposit is located in Karnes County, Texas, along the prominent south Texas uranium trend. The uranium mineralization occurs in the Deweesville Sandstone of the Whitsett Formation of the Eocene Jackson Group. The host rock is a friable, fine-grained, well-sorted, highly porous and permeable sandstone interpreted to be an ancient beach deposit. The sandstone contains significant volcanic constituents and ranges in composition from arkosic to tuffaceous. Locally, the host sandstone contains hard, dense opal cement. Bentonitic shales underlie and overlie the mineralized sandstone unit. Geometrically, the Hobson uranium-bearing zone resembles an elongated roll front type deposit. Chemical uranium values compared with gamma ray equivalent uranium values indicate that the uranium has been dissolved from the updip side and precipitated on the down- dip side of the roll front. Details of the uranium mineralization were studied using thin section microscopy, autoradiography, x-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS) techniques. The uranium mineralization occurs in the pores of the sandstone, as grain coatings and as replacement of sand-size and smaller grains. It is commonly associated with pyrite and other opaque minerals. Other favored hosts for uranium (other than pore openings) appear to be clay aggregates, altered rock and glass fragments, and carbonaceous plant debris. Aggregates of coffinite were identified by XRD and SEM/EDS analyses. Some uranium mineralization also appears to be dispersed and is postulated to be adsorbed on the clay and carbonaceous matter.

Jan 1, 1985

By W. H. Echols

An oil-emulsion mud, consisting of a mixture of oil-base mud and bentonitic water-base mud, has been used experimentally in drilling 8 of the 35 wells in the Sivells Bend field, Cooke County, Texas. Experience indicates the oil-emulsion mud can be controlled in much the same manner as a water-base mud, and the "drilling" functions of the two types of mud are comparable. The average water-loss for the oil-emulsion mud was 3.8 cu cm per well. When using oil-emulsion mud to drill the last 2000 ft of 7000 ft wells, the mud costs were approximately 2½ times that of water-base mud. There is nothing to indicate well productivities have been affected through the use of oil-emulsion mud. However, drilling time and bit footages were increased and the holes were maintained more closely to bit guage. The apparent advantages gained through the use of oil-emulsion mud in the Sivells Bend field do not appear to justify the increase in mud costs. Introduction until a comparatively few years ago most of the development of drilling mud was directed toward improving the functions of the mud as related to actual drilling operations. The industry has long recognized that one disadvantage of rotary drilling over cable-tool drilling is the possibility of injury to producing zones through the blocking effect resulting from the infiltration of water or mud into the sands. Recognizing this disadvantage, considerable attention has been diverted toward the development of muds that will improve the quality of well com-pletions through the reduction or elimination of water into the sands, but without sacrificing too many of their "drilling" functions and at a cost commensurate with the benefits derived from their use. This phase of mud research has already found practical application, for example, in the development of the Rangely field, Colorado, it appears the use of oil-base mud during drilling-in operations will contribute appreciably toward making this exploitation more profitable. Much of the discussion to follow will be better understood if a brief sketch of the Sivells Bend field is given. The Sivells Bend field, discovered by The Texas Co. in 1944 and still in the process of development, is in a large bend on the Texas side of the Red River about 85 miles north of Dallas. Geologically, the structure is an unsymmetrical anticline, with faulting having contributed to its development. The productive sands are of the Strawn series of Pennsylvanian age, the sands being lenticular in character and varying considerably in development from well to well. At Present there are 35 producing wells in the field, producing from seven different sand lenses. The productive sand lenses vary from 15 to 50 ft in thickness and the individual sands have average permeabilities of from 75 to 375 md. The presently productive sands are encountered at depths of from 6300 to 7300 ft, but testing has indicated that commercial production might be obtained from other sands as high as 5200 ft. Histories of older Strawn

Jan 1, 1948

By W. H. Echols

An oil-emulsion mud, consisting of a mixture of oil-base mud and bentonitic water-base mud, has been used experimentally in drilling 8 of the 35 wells in the Sivells Bend field, Cooke County, Texas. Experience indicates the oil-emulsion mud can be controlled in much the same manner as a water-base mud, and the "drilling" functions of the two types of mud are comparable. The average water-loss for the oil-emulsion mud was 3.8 cu cm per well. When using oil-emulsion mud to drill the last 2000 ft of 7000 ft wells, the mud costs were approximately 2½ times that of water-base mud. There is nothing to indicate well productivities have been affected through the use of oil-emulsion mud. However, drilling time and bit footages were increased and the holes were maintained more closely to bit guage. The apparent advantages gained through the use of oil-emulsion mud in the Sivells Bend field do not appear to justify the increase in mud costs. Introduction until a comparatively few years ago most of the development of drilling mud was directed toward improving the functions of the mud as related to actual drilling operations. The industry has long recognized that one disadvantage of rotary drilling over cable-tool drilling is the possibility of injury to producing zones through the blocking effect resulting from the infiltration of water or mud into the sands. Recognizing this disadvantage, considerable attention has been diverted toward the development of muds that will improve the quality of well com-pletions through the reduction or elimination of water into the sands, but without sacrificing too many of their "drilling" functions and at a cost commensurate with the benefits derived from their use. This phase of mud research has already found practical application, for example, in the development of the Rangely field, Colorado, it appears the use of oil-base mud during drilling-in operations will contribute appreciably toward making this exploitation more profitable. Much of the discussion to follow will be better understood if a brief sketch of the Sivells Bend field is given. The Sivells Bend field, discovered by The Texas Co. in 1944 and still in the process of development, is in a large bend on the Texas side of the Red River about 85 miles north of Dallas. Geologically, the structure is an unsymmetrical anticline, with faulting having contributed to its development. The productive sands are of the Strawn series of Pennsylvanian age, the sands being lenticular in character and varying considerably in development from well to well. At Present there are 35 producing wells in the field, producing from seven different sand lenses. The productive sand lenses vary from 15 to 50 ft in thickness and the individual sands have average permeabilities of from 75 to 375 md. The presently productive sands are encountered at depths of from 6300 to 7300 ft, but testing has indicated that commercial production might be obtained from other sands as high as 5200 ft. Histories of older Strawn

Jan 1, 1948