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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 M. J. Spendlove, H. W. St. Clair

An automatic surface-follower mechanism was used to measure the surface temperature and the rate of evaporation of molten zinc while undergoing distillation at low pressure. At pressures of 50 to 100 microns Hg, the rate of evaporation may be 60 to 80 pct of the theoretical maximum corresponding to the measured temperature. The rate decreases rapidly at pressures above 100 microns Hg, to only 7 pct of the theoretical maximum at 2000 microns Hg. Measured temperature gradients at the surface are in agreement with theoretical gradients calculated from the heat of vaporization, rate of evaporation, and thermal conductivity of molten zinc. THIS paper covers a series of careful measurements of the rate of evaporation of molten zinc at low pressures, undertaken as a part of a general investigation on the separation of metals by distillation.' Preliminary results on the rate of evaporation of zinc were described in a previous publication.' The results of the preliminary study are as follows: 1—The observed rates of evaporation of zinc were as high as 0.60 g per sq cm per min, corresponding to 75 pct of the maximum rate as determined by the temperature of the metal. 2—The evaporation rate was decreased from 0.30 g per sq cm per min at a pressure of 25 microns to only 0.09 g per sq cm per min when the pressure was increased to 5 mm. 3—The temperature of the surface during rapid evaporation may be 35" to 100°C less than the main mass of metal. Observed temperature gradients at the surface are consistent with those calculated from the heat of vaporization and the thermal conductivity of liquid zinc. In the preliminary experiments, the rate of evaporation was determined from the loss in weight of the metal in the crucible during the test. This was compared with the weight of the condensate. Obviously, this method was subject to error because of some uncertainty as to the period of evaporation that should correspond to the loss in weight. Furthermore, this method did not permit taking into account probable variations in the rate of evaporation during the test. A more serious shortcoming was that the temperature at the evaporating surface was not known, so the maximum theoretical rate of evaporation could not be calculated accurately. To improve the precision of rate measurements and to allow accurate measurements of the surface temperature, a refined experimental technique was developed whereby the temperature and position of the surface could be measured accurately. This was done by an automatic surface-follower mechanism that gave a continuous record of the surface temperature and the amount of zinc evaporated. These data permitted an instantaneous determination of the actual rate of evaporation and the surface temperature throughout the test. Pure zinc (99.99 pct Zn) was used in all experiments. Description of Distillation Furnace The details of construction of the distillation furnace are shown in Fig. l. The furnace is enclosed in a large quartz tube open at one end. The open end of the quartz tube is sealed by means of a water-cooled head. The entire enclosure is vacuum tight. The connection between the water-cooled head and the quartz tube is sealed by means of a rubber gasket which fits tightly against the smooth end of the tube. The metal is heated by induced current set up in the molten zinc and the walls of the graphite crucible by means of a water-cooled induction coil outside the quartz tube. High frequency current is passed through the induction coil from a 6 kw mer-

Jan 1, 1952

By Hsun Hu, R. S. Cline

The annealing behavior and the mechanism of re-orientation during recrystallization of iodide titanium cold-rolled 94 pct have been studied in detail. Results indicate that recrystallization occurs by the nucleation and growth of new grains, as in other common metals. Recrystallization nuclei form by the coalescence of subgraim, and the change in texture as a result of recrystallization is largely due to selective growth among the nuclei formed. The annealing of titanium is characterized by a wide range of overlap of the various stages of the annealing process, which may be responsible for a range of activation energies observed, and for the apparently gradual change in the annealing texture as a function of time or temperature. The deformation and recrystallization characteristics of titanium and zirconium are very similar. In cold-rolled strip, the deformation texture consists of two symmetrically oriented components, each having the basal plane laterally tilted at about 30 deg from the rolling plane and the [1010] direction parallel to the rolling direction. Upon annealing for recrystallization, the change in texture can be described, for simplicity,* as rotations around [0001].2'6'8 According to McGeary and Lustman,' recrystallization occurs in zirconium through normal growth of the subgrains, which they called "domains", without the nucleation of new grains; and the magnitude of rotation around the [0001] axis increases gradually during the progress of recrystallization. If these conclusions were true, the mechanism of recrystallization in zirconium would be basically different from that in most metals, since it is commonly known that recrystallization with reori-entation always involves the migration of high-angle boundaries. In an attempt to clarify the situation, the mechanism of reorientation during recrystallization in iodide titanium cold-rolled 94 pct was studied in detail. The structural and textural changes upon annealing at various temperatures were examined by optical and transmission-electron microscopy, X-ray pole figures, pole density distribution measurements, and micro-beam techniques. EXPERIMENTAL PROCEDURE Material and Specimen Preparation. An iodide titanium crystal bar was are-melted and solidified in a cold-hearth crucible under a purified argon atmosphere. The solidified ingot had dimensions of approximately 3 by 1/2 by 3 in. One face of the ingot was somewhat uneven, but was as clean and shiny as the remaining parts of the ingot. Large grains with a Widmanstatten internal structure were clearly shown on the shiny surfaces, indicating the occurrence of P — a transformation upon rapid cooling from the melt. Analysis of the are-melted ingot indicated C 0.033, N 0.010, H 0.013, 0 0.002 in weight percent, and traces of iron, copper, and silicon as detectable impurities. The ingot was cold-rolled -40 pct to 0.300 in. thick with a reduction of 0.005 in. per pass. The defects on the uneven side of the ingot were then removed by machining. This reduced the thickness to 0.285 in. The piece was then recrystallized by annealing at 800°C for 1 hr in a fused silica boat charged into a fused silica tube furnace under a vacuum of 10~5 mm Hg. To refine the grain size, the recrystallized metal was again cold-rolled 40 pct to 0.170 in., then annealed at 700°C for 1 hr. These treatments yielded a strip with a uniform equiaxed grain structure, having a penultimate average grain diameter of 0.04 mm and a hardness of approximately 90 Dph. Final rolling reduced the thickness from 0.170 to 0.010 in., corresponding to a reduction of 94 pct. The strip was rolled in both directions by reversing end for end between passes. Surface lubrication was provided by oil-soaked pads attached to both rolls. Specimens of 1 in. length (for X-ray examinations) and +in. length (for hardness and microstructure examinations) were cut from the rolled strip, and a width of & in. was cut from the edges of each specimen by a jeweler's saw. These specimens were then etched in a solution of 10 cu cm HN03, 5 cu cm HF, and 50 cu cm H,O to 0.008 in. thick to remove the surface metal, as well as the distorted metal at the saw cuts, prior to annealing or measurements. To minimize any surface reaction with the atmosphere, all specimens were kept in an evacuated desiccator. Isothermal Anneals. All annealing treatments were conducted in vacuum in a fused silica tube furnace as described earlier. The temperature of the furnace was controlled to within *2"C. The specimen was placed in a fused silica boat, then pushed into the hot zone of the furnace. It took about 5 to 6 min for the specimen to reach the furnace temperature. After the specimen was held at temperature for a desired length of time the boat was pulled to the cold zone of the furnace; the heating-up period was excluded from the isothermal annealing time. Thus, the uncertainty in annealing time is higher for very short anneals, but negligible for long anneals.

Jan 1, 1969

By J. H. Rushton, L. H. Mahony

Principles of fluid motion and turbulence which have been found to be of use in mixing and agitation problems are discussed, as well as suggested applications in extractive-metallurgy processes. Various types of impellers are described, together with other conditions that affect flow pattern and turbulence. The choice of equipment for particular requirements is considered, and equations for power input are given. Modern heavy-duty mixing and agitation equipment can take an increasingly important part in such extractive-metallurgy processes as solids handling, crystallizing and leaching, chemical operations, and flotation. Application of mixing and fluid-mechanics principles to extraction methods can lead to greater process rates and a resultant saving in time and money. MIXERS are being applied with increasing frequency to problems in the metallurgical industries. The increase represents in part the modernization of mechanical equipment used through the application of unitized drives, modern electric motors and speed reducers, and recently developed materials of construction. Some applications have resulted from process changes and the use of techniques for operations similar to those that have been demonstrated and proven in the chemical industry. Still more applications are being developed through the use of fluid-dynamics principles not previously recognized as applicable to these operations. It is the purpose of this paper to describe those principles of fluid motion and turbulence which have been found to be of use in mixing and agitation problems, and to suggest applications for them in the extractive-metallurgy processes. Modern mixing equipment has been designed to provide the fluid motion consistent with that best suited to different operations.' When properly applied, these more efficient fluid-handling mixers result in lower process-production costs. Metallurgical operations usually involve large amounts of solids. The characteristics of the ore control the process and only enough liquid is added to provide sufficient fluidity for handling and processing. The reactive part of the ore, the mineral value to be extracted, is likely to be low in percentage, and the quantity of reagent required is similarly low, but excessive dilution makes additional reagent necessary and therefore is undesirable. Thus, the primary problems in minerals processing are to handle as high a concentration of solids as possible and to distribute reagents uniformly. These pulps, or slurries, are in a range of solids concentration where hindered settling rates apply, and care must be taken to agitate and mix sufficiently to maintain suspension and flow throughout the equipment. Such slurries have high densities which are the weighted average of the components and viscosities that are spoken of as "effective viscosities" but are difficult to evaluate. It is convenient to separate metallurgical operations involving mixers and agitators into three categories: solids handling, mechanical or physical operations, and chemical operations. In each of these categories fluid motion is required to maintain suspension, to distribute surface-active agents, to blend components and reactants, and to induce high rates of chemical reaction. After a discussion of some basic principles of mixing and agitation, examples of application to the three categories will follow. Fluid Motion The fundamental problems of mixing and agitation of liquids have to do with the mechanics of fluid streams and the means by which they are

Jan 1, 1955

By T. J. Woodside

Prior to 1927 the lead blast furnace charge at El Paso consisted principally of direct-smelting carbonate ores, very low in zinc, and the resulting slag seldom carried more than 4.0 pct. With the exhaustion of the mines in Northern Mexico which supplied these ores, they were supplanted with a much smaller tonnage of sulphide concentrates containing appreciable amounts of zinc, and the zinc content of the slag rose to 10.0 pct. The Anaconda Company's slag fuming plant at East Helena, Montana, had then been in successful operation for several years, and it was immediately recognized that, while at that time the production of high zinc slag was small, if the grade held, a plant for the recovery of zinc from the accumulated slag might some day be practical. The grade not only held but became increasingly higher so that by 1946 suffcient slag had been accumulated to warrant the construction of a fuming plant regardless of future slag production from the blast furnaces, and with the removal of Government restrictions on construction at the end of the war the project was undertaken. The general design of the plant follows that at Bunker Hill, with waste heat boiler, unit coal pulverizers and even more extensive instrumentation and automatic control. The area around the lead blast furnaces is rather congested, being cut off from the nearest feasible site for the fuming plant by the copper plant, so that the most practical route for hot slag transfer is through the converter aisle. For this reason and also to make use of the existing converter cranes to serve the fuming furnace, an unused reverberatory at the north end of the converter building was dismantled and the fuming furnace and boiler located in its place. A flue at right angles to the furnace and boiler runs northward to the U-tube coolers and baghouse (Fig 1). From the bag-house a steel flue runs eastward to an existing and long unused 300 ft con- Crete stack. The coal handling system and de-leading plant lie north of the furnace and east of the cooling tubes and baghouse. The furnace is conventional, 8 X 21 X 33 ft high inside and completely water jacketed (Fig 2). There are 21

Jan 1, 1950

By R. W. Fountain, J. F. Libsch

ONSIDERABLE time and effort have been ex- pended recently in research designed to provide a better understanding of the solid state transformations leading to the permanent magnet qualities of many commercial alloys. The knowledge derived from these investigations has resulted in the development of new magnetic materials as well as improvements in some of the older materials. The permanent magnet qualities of the newer alloys having high residual inductions and high coercive force values, have been attributed to the precipitation of a second phase or an order-disorder transformation in a solid solution. The ternary Co-Fe-V alloys provide an interesting group of magnetic materials having a wide range of magnetic properties. The low vanadium alloys' possess soft magnetic properties similar to the binary Co-Fe alloys, while at higher vanadium contents (about 10 pct) interesting permanent magnet properties are obtained.2,3 Previous work by Nesbitt' on the ternary Co-Fe-V permanent magnet materials, resulted in the conclusion that the precipitation of a second phase, ?, was responsible for the permanent magnet qualities of these alloys. However, unlike the conventional precipitation hardening alloys, the ? phase, which is stable at high temperatures, is precipitated in the low temperature a phase upon aging. Recent work by Geisler and Martin"." has established that the order-disorder reaction inherent in the binary Co-Fe alloys is also present in the ternary Co-Fe-V alloys. On the basis of their investigation, it was proposed that ordering of the a phase is also a possible explanation of the mechanical and magnetic hardening in these alloys. Thus, it appears that the Co-Fe-V alloys are rather unique in that two solid state transformations are taking place which may account for the properties of these alloys. In view of these facts, the present investigation was undertaken to study the mechanism of mechanical and magnetic hardening in the 10 pct V-Co-Fe alloy with particular reference to the role of the ? phase; and to correlate the results of this study with other magnetic properties. In addition, the influence of increasing vanadium contents on the transformation of Co-Fe alloys was also undertaken to supplement the main objective of the investigation. Experimental Procedure The Co-Fe-V alloys used for study consisted of: 1—a commercial lot of Vicalloy I, a 10 pct V alloy, and 2—alloys prepared by powder metallurgy and containing 52 pct Co and 0 to 14 pct V, balance iron. The commercial alloy was received in the cast and forged condition and was used primarily for the detailed study of hardness, electrical resistivity, and magnetic properties of the 10 pct V alloy. The powder metallurgy alloys were prepared from electrolytic iron, commercial cobalt, and ferro-vanadium powders. The processing cycle was as follows: 1—Elemental powders were weighed and mechanically mixed for 24 hr. 2—Mixed powders were pressed at 60,000 psi into the form of bars 5/8 x 5/8 x 5 in. 3—Bars were sintered in an atmosphere of purified dry hydrogen for 24 hr at temperatures ranging from 1380" to 1340°C, depending upon the vanadium content. The as-sintered bars were cut in half; and one half was machined to 7/16 in. diam for thermal analysis. The remainder of the bar was hot forged to approximately 0.050 in. for X-ray diffraction analysis. Additional details of sample preparation are presented subsequently according to the type of test performed. Thermal Analysis Measurements One of the simplest and most widely used tools for determining phase relations as they change with temperature and composition is to study the rate of change of temperature of a material as heat is supplied or extracted at a constant rate. The thermal analysis method used in this investigation is the inverse-rate method described by Smith.'

Jan 1, 1954

By D. T. Peters, J. C. Bisseliches, J. W. Spretnak

The pain boundary relaxation phenomenon in high-purity copper, 0FHC copper, and a precipitation-hardenable alloy o-fCu-2 uit pct Co has been studied by internal ,friction and elastic aftereffect techniques. The data were analyzed by assuming the broad distribution of relaxation times observed obeys a lognormal distribution law which enables calculation of the relaxation strength. Grain size had no effect on relaxation strength, although the peak width increased with increasing grain size and decreasing temperature. A double grain boundary peak was produced in high-purity copper by annealing to produce secondary recrystallization. The activation energy measured for 99.999 pct Cu is 37.5 * 3 kcal per mol and 46.5 kcal per mole for OFHC copper. A small peak in the Cu-Co alloy at about 220°C at 1 cps was deduced to be the grain boundary peak. Its height increased and its activation energy decreased with increasing aging time. Except for erratic peak positions the observations were consistent with the theory of pain boundary sliding. BEFORE the mechanism of the grain boundary internal friction peak in metals can be satisfactorily explained, the detailed characteristics of the relaxation process must be documented. Of interest are the effect of grain size on relaxation strength, the high-temperature background, and peak width and position. The effect on the grain boundary peak of a precipitate at grain boundaries and of the change in distribution of the particles with aging time must also be explained by any existing or forthcoming theory. The model which has received the most attention was proposed by KG' and zener2 and proposes that the anelastic strain results from sliding of adjacent crystals at grain boundaries. The sliding is limited by the interlocking of grain corners. It follows, according to this model, that the relaxation strength is independent of and the relaxation time is proportional to the grain size. The proportionality between grain size, D, and relaxation time, t, has been confirmed by K&' and Bisseliches . In this case, the internal-friction peaks of various specimens can be superimposed by plotting Q-' as a function of the parameter vD exp H/RT where v is the frequency and H the activation energy. However, the data of Starr et 01.' and Leak6 fit better to a parameter containing D to an exponent near two. A meaningful relationship is not always deducible from the shift of peak temperature with grain size. KG7 demonstrated that a twofold variation in grain size obtained by varying the amount of cold work followed by identical recrystallization anneals will cause a peak shift that is too large to be accounted for even by an exponent of two. Since the decreased grain boundary area existing with a larger grain size is exactly compensated for by an increased sliding distance, the relaxation strength should not decrease with increasing grain size. The height of the internal-friction peak has generally been observed to be rather insensitive to grain size as long as the average grain diameter does not approach the specimen diameter. Exceptions have been reported by Koster, Bangert, and Lang8 for copper, and by Leak6 for iron. The observations for copper could well have been confused by the presence df 0.3 pct0. The possibility that the peaks may simply be increasing in width with increasing grain size and that the relaxation strength, which is proportional to the area under the peak, may remain constant was not examined. his point has been checked in this investigation using high-purity copper. Atomic mechanisms to account for damping by sliding at grain boundaries have been proposed by KG7 and Mott. KG predicts the activation energy to be identical to that for self-diffusion. Mott's "island" model suggests the activation energy is nL where n is the number of atoms in an island and L is the latent heat of fusion per atom. Other authors have felt that a value equal to the activa-

Jan 1, 1964

By M. J. Hordon

Measurements of the 103 yield stress of ordered and disordered poly crystalline Cu ,Au were related to the ordered antiphase domain size determined by resistivity measurements. For undeformed material, a yield stress maximum wa obtained at a critical domain diameter of about 40A. Plastic deformation resulted in a marked increase in the yield stress and electrical resistivity of the ordered alloy compared to the disordered, the strain hardening rate increasing regularly with initial antiphase domain size. Order hardening was accompanied by a sharp reduction in size of the initially large domains. It has been observed that the yield stress of ordered and partially ordered Cu3Au alloy varies sensitively with antiphase domain size aid degree of order.ly2 In addition, ordering of the lattice leads to a marked increase in the strain hardening rate (order hardening) as compared to the rate for the disordered alloy. In the present investigation, changes in the electrical resistivity and yield stress of ordered polycrystalline Cudu with varying initial domain diameters were measured after tensile plastic deformation in order to examine the effect of cold work on the antiphase domain size. EXPERIMENTAL PROCEDURE Au-Cu alloy of 99.99 pct purity analyzing 50.85 wt pct Au-balance copper was obtained from the Handy-Harmon Co., N. Y., in the form of 0.061 in. diam drawn wire. Wire specimens 3 in. in length were given the following annealing treatment in nitrogen: 500" for 72 hr, 820" for 15 hr, and 450" for 5 hr, followed by a water quench. The annealing sequence resulted in a completely disordered structure with a grain size of about 0.2 mm. The disordered specimens were then reannealed at 360' in nitrogen for periods varying from 10 min to 150 hr followed by quenching to produce ordered structures with varying domain sizes. The degree of ordering and variation of domain size was followed by electrical resistivity measurements made at room temperature using a low resistance precision Kelvin double bridge apparatus. The specimen resistance was determined over a length of 4.0 cm between two brass knife-edge contacts while the specimen was immersed in an oil bath to minimize temperature variations. In addition, the current flow in the circuit was minimized by a current pulse technique in balancing the bridge in order to avoid heating the specimen. Using a sensitive galvanometer to detect the bridge null, the accuracy of the resistance measurement Wire specimens were plastically strained in tension with an Instron tensile unit at strain rates in the range 5 x 10"5 sec-' to 2 x 10"4 sec-'. Stress and extension data were fed into the Instron chart drive amplifier to obtain the actual stress-elongation curve from which the yield stress at 10"3 strain was determined. The maximum resolution of the apparatus was approximately 50 psi stress and 3 x 104 strain. At various plastic strain levels, deformation was interrupted and the electrical resistivity determined after removing the stress. RESULTS AND DISCUSSION 1) Yield Strength of Ordered Cudu. In order to determine the effect of the ordered antiphase domains on the initial yield stress, specimens were prepared with varying domain sizes ranging from zero for 5 completely disordered structure to about lo5A for a completely ordered structure by suitable annealing treatment. Domain sizes were estimated by comparing room temperature electrical resistivity data with the original data of Jones and sykes3 as modified by rdle.' In agreement with previous work, the resistivity varied sensitively with domain diameter and degree of order, decreasing from approximately 11.6 x l0- ohm-cm for the disordered structure to about 5.9 x l0- ohm-cm for ordered domains above 10"3 cm in diameter. Fig. 1 shows the change of the 103 yield stress with ordered domain size. It is evident that the maximum

Jan 1, 1963

By Harlowe Hardinge

The sound made by ball, pebble and rod mills has long been used by the operator as the "telltale" of their operation. The nature of this sound depends upon local conditions and the type of mill used. By experience an operator can tell whether the mill is running properly or not. Some operators are able to detect the difference in sound much better than others and get better results running the same mill under the same conditions. The automatic operation of a mill using sound as the fundamental means for maintaining control presents many problems. The satisfactory solution of these problems requires, for given operating conditions, a greater average output, with improved product for subsequent processing, than can be obtained by manual control. Relation of Sound to Useful Grinding Energy Experience has taught us that there is a difference in character as well as in intensity of sound between a mill grinding wet and one grinding dry, in open or closed circuit, to obtain a coarse or fine product, on the same material, to say nothing of the effect with a variety of different materials. Broadly speaking, a wet-grinding mill operates best at a lower sound level than the same mill grinding dry, with other conditions the same. Several reasons for this variation in sound intensity under these conditions can be advanced, but the important point is that there is a difference, based upon practical results. Since these reasons may be more or less involved, and may be subject, to much discussion, only one will be considered here. It is apparent that two balls hitting together or a ball striking the lining, if there is no intervening material, will produce the maximum sound. If a complete cushion of material is placed between the balls or ball and liner, so that the energy is dissipated without doing useful work, the balls will be unable to create enough pressure or force to fracture the particles, and the sound will be at a minimum. At some point in between—that is, where there is sufficient material between the balls or ball and liner so that the ball will fracture the particles without mashing them unduly—the sound

Jan 1, 1939

By Harlowe Hardinge

The sound made by ball, pebble and rod mills has long been used by the operator as the "telltale" of their operation. The nature of this sound depends upon local conditions and the type of mill used. By experience an operator can tell whether the mill is running properly or not. Some operators are able to detect the difference in sound much better than others and get better results running the same mill under the same conditions. The automatic operation of a mill using sound as the fundamental means for maintaining control presents many problems. The satisfactory solution of these problems requires, for given operating conditions, a greater average output, with improved product for subsequent processing, than can be obtained by manual control. Relation of Sound to Useful Grinding Energy Experience has taught us that there is a difference in character as well as in intensity of sound between a mill grinding wet and one grinding dry, in open or closed circuit, to obtain a coarse or fine product, on the same material, to say nothing of the effect with a variety of different materials. Broadly speaking, a wet-grinding mill operates best at a lower sound level than the same mill grinding dry, with other conditions the same. Several reasons for this variation in sound intensity under these conditions can be advanced, but the important point is that there is a difference, based upon practical results. Since these reasons may be more or less involved, and may be subject, to much discussion, only one will be considered here. It is apparent that two balls hitting together or a ball striking the lining, if there is no intervening material, will produce the maximum sound. If a complete cushion of material is placed between the balls or ball and liner, so that the energy is dissipated without doing useful work, the balls will be unable to create enough pressure or force to fracture the particles, and the sound will be at a minimum. At some point in between—that is, where there is sufficient material between the balls or ball and liner so that the ball will fracture the particles without mashing them unduly—the sound

Jan 1, 1939

By N. Brown, H. Green

The effect of quenching temperature and of aging temperature and time on compression stress-strain curves of ß brass was investigated. Age softening occurs at a rate which decreases with decrease of quenching temperature below the critical temperature for ordering. The activation energy for softening is 15,400 cal per mol. No matter how rapidly brass is quenched or what the temperature from which it is quenched, practically complete order is obtained at room temperature. It has been demonstrated that with respect to the specific heat,',' electrical resistivity," X-ray diffraction, and microstructure, the slowly cooled and rapidly quenched specimens are the same and that complete long range order exists in both cases. However, Smith" showed that the hardness of ß brass depended upon the cooling rate and the temperature from which brass is quenched. Smith showed that the hardness was a maximum for specimens quenched from about 445 °C and that the as-quenched structure softened at room temperature at a rate depending upon the temperature prior to quenching. This softening after quenching is in this paper referred to as age softening. The results of this investigation are qualitatively the same as the findings of Smith. However, a more detailed analysis of these phenomena has been possible since the stress-strain curve offers a more sensitive index of the state of the metal than hardness. It is the purpose of this paper to show how the mechanical properties are related to the ordering of ß brass. A 200-lb ingot made from electrolytic copper and electrolytic zinc was extruded to 1/2in. rod. Chemical analyses at frequent intervals along the rod showed that the alloy contained 51.5 pct Cu with the greatest impurity being iron, at 0.01 to 0.001 pct. To obtain a constant test material, the 1/2in. extruded rod was warm-rolled to % in. diameter at 200°C and then recrystallized to a grain size of 2.0 mm. The specimens for the compression test were % in. high and % in. in diameter. The specimen ends were polished on 600 metallographic paper and coated with Molykote for a lubricant. The compression rig consisted of an anvil resting on the machined table of the Baldwin Southwark testing machine and a plunger fixed to the movable cross

Jan 1, 1954

By T. V. Philip, R. E. Lenhart

When commercial silicon iron sheets of varying magnetic quality are isothermally annealed at high temperatures, extremely large grains develop in the material having good magnetic properties. These grains are of the (110) [001] orientation and are formed by secondary recrystallization. The primary driving force for this secondary recrystallization is grain boundary free energy. For the secondary grains, activation energies of 103 kcal per mole for nucleation, and of 75.5 kcal per mole for growth, were obtained. The activation energy for nucleation of the secondary grains is consistent with a model involving redistribution of a precipitate acting as the primary grain growth inhibitor. SINGLY oriented silicon iron sheet was first produced in 1935.1 The material as commercially produced today has a very highly developed preferred orientation or texture; up to 95 pct of the grains are crystallographically oriented with their (110) planes in the plane of the sheet and their [loo] directions parallel to the rolling direction. This texture, usually written as (110) [00l], is referred to as the "GOSS" or the "cube-on-edge" texture. Because the magnetic properties of this material are superior to those of the nonoriented sheets in the direction of rolling, the oriented silicon iron has acquired tremendous industrial importance especially in the manufacture of transformer cores and other electrical equipment. The commercially produced material is essentially an iron-silicon alloy containing about 3 1/4 pct Si with minor impurities totaling less than 0.15 pct. The silicon steel heat is melted in the open hearth or electric furnace. The ingots are hot rolled, with or without being slabbed, to strips of 0.100 to 0.080 in. thickness. They are then cold reduced to an intermediate thickness, recrystallized, cold reduced to final thickness, decarburized, and finally annealed at a high temperature. During this high-temperature anneal, extremely large grains with the cube-on-edge texture are produced in the sheet. Several papers have appeared in the literature2-10 relating to the production of the Goss-textured material. Most of these describe the textures produced on cold rolling and on subsequent annealing of single crystal or polycrystalline silicon iron. May and Turnbull11,12 have recently shown the necessity of a second-phase dispersed impurity in the material for the production of the Goss texture. However, none of these papers describes in detail the nucleation and growth kinetics of the (110) [001] grains during the final high-temperature anneal.* The present work, therefore, is an attempt to understand the nucleation and growth kinetics of the cube-on-edge grains in the silicon iron sheet during the final high-temperature anneal.

Jan 1, 1962

By E. A. Barnard

ARSENIC is a very old substance. The ancients speak of it in their writings, and its use has developed very little until recent years. The ancients used it in making pigments, in medicine, and for poison. They also tell of the difficulties of handling it-an experience which is very similar to our own. Until about 10 years ago, arsenic was very cheap and was a drug on the market. About that time the boll weevil began making serious inroads on the American cotton crops, and after much investigation the Depart-ment of Agriculture developed a very successful poison for this pest, consisting of calcium arsenate. The weevil pest has continued, and as the cotton planters have become convinced that calcium arsenate is the best material to use against the weevil, the demands for it have been steadily increasing, resulting not only in a rising price of arsenic but in a very serious shortage so far as our country is concerned. So serious has this shortage become, and so vital is it to the cotton growing industry, that Congress has appointed a committee to investigate and report on the situation. A meeting of arsenic producers and consumers was held in New York last December to take stock of the situation and to see what could be done. The extreme increase in, the market price of arsenic-from 6 c. to 15 c. per lb. in less than a year-has been very harmful to the producers as well as to the consumers. Some very interesting' data were brought out at this meeting, as follows: CONSUMPTION PER YEAR, SHORT TONS Arsenate of lead 2,000 Paris green 1,200 Proprietary mixtures 750 Sheep dips : 1,000 Weed killers 1,500 Glass : 2,000 8,450 1922 Consumption as calcium arsenate 4,000 12,450 1923 Estimated consumption as calcium arsenate... 12,000 Estimated 1923 consumption 20,450

Jan 8, 1923

By AIME AIME

CHARLES A. CHASE, manager of the Shenandoah-Dives Syndicate, operating the Shenandoah Mines in southwestern Colorado, reviewed the current work at that property at a recent meeting of the Colorado Section, in Denver. This operation is a new one, having been in effect only two years, but the properties that were consolidated by Mr. Chase had had certain production in earlier years, since when they had: been inactive. These properties are located. in the high mountains of the San Juan section in Colorado, and although they had had a substantial production of ores of good grade in the upper levels, the project as a whole involved the bold undertaking of driving through the mountain, starting on the Mayflower claim on the Arrastre Gulch side and passing through the Mayflower, Slide, Terrible, North Star, Dives and Shenandoah No. 3 claims. This is a distance of over 8,000 ft. which is known to be mineralized, and the main operating tunnel was started at an elevation of approximately 11,000 ft. The main exploration work has already extended in nearly 4,200 ft. and the present mining production of nearly 550 tons daily is being secured while the main exploration work is being continued. The main heading is now within the North Star claim and the plan of operations involves continuing ahead for a few hundred feet and then starting an upraise which will he 2,200 ft. high and which will connect with the old workings of the North Star mine. The plan of ruining then will he to drive levels along the vein in both, directions to daylight and retreat downward, taking out all the ore and abandoning, the workings after the ore is removed. In this way one level after another progressing downward will be abandoned. The raise will be of two compartments, one of which will carry the 8-ton skip and the other the counterweight and manway. So far the ore has been broken over an average width of more than 11 ft., with an output of 39 tons per machine shift.

Jan 1, 1932

By N. Jaffee, J. E. Dorn

An activation energy of 27,400 5 1000 cal per mole was obtained for the creep of poly crystaLline aluminum over the temperature range of 273° to 350°K, at strains varying from 0.003 to 0.230. Stresses varied fronz 2250 to 6000 psi, strain rates from 0.1145 x 10-5 to 29.5 x 10~s min.-1. A strain temperature-compensated time correlatzon was oblained indicating that the structure was depedent solely upon the strain at a given stress; X-ray diffraction analyses and tensile tests on precrept specimens verified this. PREVIOUS investigations1 have revealed that the apparent activation energies for creep of high-purity polycrystalline aluminum are insensitive to the applied stress, strain, and strain rate. On the other hand, the apparent activation energy is dependent on the temperature1,2 as shown by the data reproduced in Fig. 1. Each plateau of this curve is associated with a unique rate-controlling dislocation mechanism for thermally activated creep. It is now very well-established that over the high-temperature range, where the activation energy is about 35,500 cal per mole, the creep rate is controlled by the dislocation climb mechanism. 3 Over the intermediate range of temperatures, from about 260° to 370°K, another unique activation energy, namely 28,000 cal per mole, is obtained. Current evidence strongly supports the contention that cross slip is the rate controlling mechanism for creep in this case: 1) Crystal recovery can occur by a number of mechanisms prominent among which are climb and cross slip. Astrom,4 using the Borelius micro-calorimeter, reported rapid crystal recovery of cold-worked polycrystalline A1 at 340° to 370°K giving an activation energy of 28,000 cal per mole and additional recovery at 455° to 478°K giving an activation energy of 3 6,000 cal per mole. Whereas the latter recovery process was clearly associated with the dislocation climb mechanism, the former, 28,000 cal per mole process could have arisen as a result of the cross-slip mechanism. 2) Single crystals of high-purity A1 favorably oriented for octahedral glide exhibit an activation energy for creep of about 3400 cal per mole over the range from 0° to 400°K and that of about 28,O:O cal per mole over the range from 600° to 775°K . Whereas the lower activation energy process is accompanied by the development of sharp slip-band traces, the 28,000 cal per mole process was uniquely characterized by extensive cross slip. 3) Theoretical calculations by Seeger and schoeck6 suggest an apparent activation energy for cross slip in A1 of about 24,000 cal per mole and another theoretical estimate by Friedel 7 gives the observed 28,000 cal per mole as the theoretical activation energy. It is therefore consistent with this evidence to, at least tentatively, ascribe the 28,000 cal per mole creep process in A1 to the operation of cross slip as the rate controlling mechanism. Although creep has been rather well-explored in the dislocation climb range, very little, excepting perhaps the activation energy, is known about creep in the cross slip range. This investigation was undertaken, therefore, to reconfirm the activation energy for creep in polycrystalline A1 in the intermediate temperature range and to study the strain-time relationship for creep at a constant stress in the cross slip region. EXPERIMENTAL PROCEDURE AND TECHNIQUE The three types of high-purity A1 alloy specimens described in Table I were used in this investigation. Specimens were milled from 0.100 in. thick cold-rolled sheets with their tensile axes in the rolling direction following which they were given a recrys-tallization and grain growth heat treatment at temperatures well above those which were subsequently employed in the creep tests.

Jan 1, 1962

By B. M. Larsen, T. E. Brower

Introduction and Summary By "thermochemical factors" we refer to those variables which affect the net heat which must be put into the bath in order to make a heat of steel from any given set of charge materials. This is admittedly only one phase of the production rate problem. The whole problem includes also consideration of rate of charging, flame radiation intensity, rate of optimum fuel input obtainable without undue damage to the furnace structure and any variations in conditions such as stirring, slag volume or viscosity which affect the rate at which heat can flow down and away from those exposed surfaces where the heat is first received from the flame. Because a given type of charge in a shop is often considered as being nearly constant in both physical and chemical characteristics from one heat to another, and because such a state of affairs may be thought of as resulting in a reasonably constant net heat requirement, this requirement is usually neglected as an invariable, inevitable matter, about which nothing can be done. With normally variable charge, and variable percentages of limestone and cold pig, however, the net heat requirement can be subject to very appreciable change; it may also be affected by such things as the currently popular procedure of blowing oxygen into the bath. To bring the general problem of production rate into better perspective, therefore, it seems worthwhile to try to evaluate the net bath heat requirement and the amount by which it may change through variation in different factors. Because our calculated values of net heat are admittedly uncertain, we have tried to check them in part by statistical data on actual production rates over rather large groups of commercial heats. The results of calculation of net heat requirements in a wide range of actual commercial practices may first be summarized briefly. We find a wide range between the extremes of different practices, as would be expected, with duplex practice (essentially blown metal plus hot metal) having essentially a zero net heat requirement, an all-cold charge practice somewhat over I million Btu per ton of steel and a high hot metal practice about 0.75 million Btu per ton. Over the commercial range of scrap plus hot metal practice, increasing the percentage of hot metal from 40 to 78 pct, with other factors nearly constant, decreased the net heat by only some 5-10 pct. The net heat is increased by about 1.2 pct for each I pct of the metallic charge present as cold pig. Calculated values of oxygen supplied by air varied from about 25 up to 60 lb per ton of steel, and in a 60 pct hot metal practice, an increase from 32 to 52 Ib oxygen from air decreased the calculated net heat from 0.88 to 0.74 million Btu per ton. Use of pure cold oxygen to substitute for about one half of the total charge ore (about 28 Ib oxygen replacing 145 Ib ore per ton of steel) decreased the

Jan 1, 1949

By B. M. Larsen, T. E. Brower

Introduction and Summary By "thermochemical factors" we refer to those variables which affect the net heat which must be put into the bath in order to make a heat of steel from any given set of charge materials. This is admittedly only one phase of the production rate problem. The whole problem includes also consideration of rate of charging, flame radiation intensity, rate of optimum fuel input obtainable without undue damage to the furnace structure and any variations in conditions such as stirring, slag volume or viscosity which affect the rate at which heat can flow down and away from those exposed surfaces where the heat is first received from the flame. Because a given type of charge in a shop is often considered as being nearly constant in both physical and chemical characteristics from one heat to another, and because such a state of affairs may be thought of as resulting in a reasonably constant net heat requirement, this requirement is usually neglected as an invariable, inevitable matter, about which nothing can be done. With normally variable charge, and variable percentages of limestone and cold pig, however, the net heat requirement can be subject to very appreciable change; it may also be affected by such things as the currently popular procedure of blowing oxygen into the bath. To bring the general problem of production rate into better perspective, therefore, it seems worthwhile to try to evaluate the net bath heat requirement and the amount by which it may change through variation in different factors. Because our calculated values of net heat are admittedly uncertain, we have tried to check them in part by statistical data on actual production rates over rather large groups of commercial heats. The results of calculation of net heat requirements in a wide range of actual commercial practices may first be summarized briefly. We find a wide range between the extremes of different practices, as would be expected, with duplex practice (essentially blown metal plus hot metal) having essentially a zero net heat requirement, an all-cold charge practice somewhat over I million Btu per ton of steel and a high hot metal practice about 0.75 million Btu per ton. Over the commercial range of scrap plus hot metal practice, increasing the percentage of hot metal from 40 to 78 pct, with other factors nearly constant, decreased the net heat by only some 5-10 pct. The net heat is increased by about 1.2 pct for each I pct of the metallic charge present as cold pig. Calculated values of oxygen supplied by air varied from about 25 up to 60 lb per ton of steel, and in a 60 pct hot metal practice, an increase from 32 to 52 Ib oxygen from air decreased the calculated net heat from 0.88 to 0.74 million Btu per ton. Use of pure cold oxygen to substitute for about one half of the total charge ore (about 28 Ib oxygen replacing 145 Ib ore per ton of steel) decreased the

Jan 1, 1949

By C. H. Mahoney, P. E. LeGrand, A. L. Tarr

MAGNESIUM, it is now generally realized, differs in some important aspects from most other structural metals, not excepting even its close neighbors, the aluminum-base alloys. This is particularly true with respect to the effects of elevated temperatures on the two light metals when in the molten state. Aluminum, on the one hand, should not be raised above its melting point any higher than is absolutely necessary if one is to avoid danger of gas absorption and a tendency toward grain growth in the resultant casting.1 Magnesium alloys, in sharp contrast, actually benefit by being heated to temperatures considerably above their melting point. It is a commonly accepted practice to establish the desired fine grain in the industrial magnesium alloys of the aluminum-bearing group by raising the temperature of the melt after the refining treatment to some 25e C (482°F.) above the melting range. To recall briefly the typical practice for magnesium alloys, the molten metal is refined by fluxing at about 730° C. (1350 F.), and after the melt has been covered with a suitable flux, the temperature is raised to between 870°C. (1600°F.) and 930°C. (I700°F.). It is then cooled as quickly as possible to the casting temperature. This superheating, as it is called, results in a fine-grained cast metal structure which has superior mechanical properties, enhanced amenability to solution heat-treatment, and better machinability than cast metal that has not been superheated. The minimum temperature of superheating varies to some extent with the composition of the alloys to be treated and usually increases with the percentage of magnesium in alloys containing the same constituent metals.2 It should be noted that the grain-refining effect of superheating is markedly apparent only in connection with the alloys containing aluminum as an alloying constituent-the binary alloy containing r.5 per cent manganese, for example, is not refined in grain to any noticeable extent by a superheating effort. While the phenomenon of superheating is well known in the magnesium industry, the mechanism of the process has remained a mystery. During the superheating cycle something occurs that forces a fine grain upon the solidifying metal. The process has been controlled in an empirical manner, and occasionally, especially on large-scale melts, and for no apparent cause, no grain refinement is obtained from a superheating treatment. Only a few papers of importance have been published on the subject. Of these, one of the most helpful is the paper by Achenbach, Nipper and Piwowarski,3 which gives considerable data concerning the effect of superheating on various properties such as fluidity, shrinkage and hot crack formation, as well as grain size, and a discussion without any definite conclusions on the theoretical aspects of superheating. A short article by Murphy, Wells and

Jan 1, 1945

By G. Sachs, L. J. Ebert, W. F. Brown

INTRODUCTION ISOTHERMAL transformation, or "austempering," of a carbon-containing austenite at elevated temperatures yields so-called "intermediate products." Their structure and properties are, for a given hardness, rather different from those of "tempered martensite" obtained on conventional quenching and tempering.1 Several investigators2,3 have found that for high carbon and slightly alloyed steels the intermediate products formed at temperatures close to that of the martensite reaction possess strength properties superior to those of tempered martensite. The structure of these low temperature, intermediate products is generally acicular (bainite) but clearly different from that of martensite. However, at higher austempering temperatures, between 1000 and 1300°F (540 and 700°C) carbon steels were found to exhibit a rather low ductility.4-5 Thus notch bar tensile tests showed the ratio between notch strength and regular tensile strength to decrease with increasing austempering temperature. For ductilities below a few percent this notch strength ratio is a measure of ductility, according to investigations on low alloy steels.6-7 Furthermore the presence of intermediate products formed unintentionally on quenching was considered as responsible for the low ductility and impact energy of some heat treated steels.8 These intermediate products could result from partial transformation at the so-called "nose-temperature" where the rate of the transformation is a maximum. Tempering improved such mixtures of martensite and intermediate products, their properties approaching those of tempered martensite of equal hardness. The following investigation constitutes an attempt to determine certain strength properties of a partially austempered and subsequently quenched low alloy steel, namely, a chromium steel (SAE 5140). The structures formed by such a treatment should consist of a mixture of intermediate products formed on austempering and a martensite formed on oil quenching from the austempering temperature. It was intended, by varying the austempering time, to vary the quantity of the intermediate products between zero and 100 pct. The austempering temperature of 860°F was selected after extensive preliminary tests close to the nose-temperature. Austempering at this temperature yielded an acicular intermediate product. Additional tests under less exacting conditions were made for an austempering temperature of 950°F where the intermediate product appeared to be very fine pearlite. To determine the effects of tempering on structures containing various amounts of

Jan 1, 1948

THE first session of the production engineering group on Wednesday, morning, with J. B. Umpleby as chairman, recorded the principal developments since the Fort Worth meeting. Added to this was a lively discussion of pressure maintenance. Recent advances in the air-gas lift have resulted from the need of applying the method to smaller wells at lower costs. In many places intermittent flow has given excellent results, and numerous mechanical de-vices for its automatic control have been, developed. Papers by C. V. Millikan on the Mid-Continent field and by A. H. Bell on California, fields formed the basis for discussion. The maintenance of initial sand pressures was ably discussed for two Texas fields by t. V. Foran in a paper that not only outlined the technic of operation and the results obtained but also contained noteworthy cost data in terms of increased ultimate production. Mr. Foran recommends the use of air in the first stages of pressure maintenance as a means of determining sand conditions and directions of flow, later turning to gas, if available, because of its greater solubility on oil. A round table discussion on petroleum engineering educational problems, with H. G. George as chairman, brought out much interesting discussion that is difficult to summarize. The other Wednesday morning session was a refinery engineering symposium with T. G. Del-bridge as chairman and the economical application of heat for the general topic. A paper on the modern pipe -still, by H. S. Bell, and another by C. W. Stratford on the modernization of the cylindrical still elicited a lively discussion.

Jan 3, 1928