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By S. M. Moos, R. E. Dugger

In reviewing available vacuum filtration equipment in this paper, several types of filters have been included which are probably not familiar to operators in the mining industry. However, it was felt that these units might be of interest in the event that an application should arise for the filtration of a product in the future that does not exist today. In addition, exposure of our industry to equipment used in other industries might have a tendency to be thought provoking and perhaps lead to the development of equipment and/or applications in our industry which do not necessarily exist at this time. Most innovations in filtration equipment have been confined to the improvement or design change of components and accessories, particularly reflecting the availability of materials of construction that have been developed. Recent developments in the application of horizontal belt filters have been innovative. The application of this unit as a substitute for or an adjunct to thickeners in a CCD circuit can certainly be innovative and perhaps provide a basis for reduction in capital and operating costs in this area. For example, mill tails are generally pumped at the highest possible density that will adequately flow. Tailings ponds and dams with their attendant design requirements are based upon this estimated water volume. Availability of a much dryer, non-flowing filter cake opens up several new options for disposal. Considerable cost savings could result in the design and planning of disposal areas for containing dryer material. No attempt has been made in this paper to provide a manual for the operation of all of the many types of equipment that are available. Rather, the paper tries to present an overview. Fundamentals of Vacuum Filtration Filtration may be defined as the separation of solids from a liquid effected by passing the liquids through a porous medium. If the filtrate is induced to flow through the medium by hydrostatic head, we refer to it as gravity filtration. If we utilize super-atmospheric pressure upstream of the medium we call it pressure filtration and if sub-atmospheric pressure is applied downstream of the medium we call it vacuum filtration. Centrifugal filtration occurs when a centrifugal force is applied across the medium. Centrifuges will not be discussed in this paper. The process goal of filtration may be the production of dry solids where the cake is the valuable product, clarified liquid

Jan 1, 1980

By T. D. Murphy

The element silicon, with its usual partner, oxygen, plays the same role on this planet relative to inorganic materials as carbon and hydrogen play with respect to living organisms. The crystallographic structure of silicon dioxide (SiO,) consists of one atom of silicon well-nigh inseparably bonded to four contiguous atoms of oxygen, a gas of but slightly more than half its atomic weight, forming a three-dimensional network of SiO, tetrahedra (Dietz, 1968). This wispy arrangement is the fabric of the mineral quartz which is one of the harder, more abrasive, and chemically stable raw materials to be found in Mother Nature's cupboard. Most of us are vaguely familiar with the observation that nearly 60% of the lithosphere to an approximate depth of 10 miles is composed of these two elements, which proportion actually rises to about 75% if the atmosphere, hydrosphere, and biosphere are included (Parker, 1967). Elemental silicon is a brittle steel-gray metalloid with a density of 2.42 and does not occur in nature. In its limited commercial form, which is still brittle and metallic in appearance, its density drops to 2.33. It combines with oxygen to form the gaseous oxide SiO, or the solid dioxide SiO, (analogous to its congener carbon in CO and CO,); a tetrachloride SiCl, (analogous to CC1,); or, combining with oxygen and one or more metal ions, forms the largest rock-making family of all, the silicates. Further, next to the feldspars, quartz is the most abundant known mineral and, in some form or another, accounts for roughly 12% of surficial terrestrial rock. It is this so-called "free silica" to which your attention is chiefly directed in this chapter. In any such consideration of silica, its several crystalline phases with their attendant differing physical properties appear worthy of delineation. Alpha quartz is the only one of this interesting polymorphic family that is thermodynamically stable at normal pressures and temperatures up to about 573°C. The low phases of tridymite and cristobalite can exist in the so-called metastable state below 117°- 200°C but seldom occur in nature in these two different crystal forms (Sosman, 1965). Opaline silica, now considered by most researchers to be a variety of cristobalite, occurs in abundance and is the only exception. The three remaining polymorphs, keatite, coesite, and stishovite, also are metastable under ambient conditions. Keatite, however, is not known to occur naturally and has only been synthesized in the laboratory. The other two have been identified in submicron sizes and in microscopic amounts, occurring naturally as a result of high order shock-wave pressures generating quite elevated temperatures-such as might accompany the impact of a large meteorite on a hard sandstone terrain (Chao, et al., 1962). An intriguing characteristic of these silica minerals, and one which has very practical applications, is their extremely variable densities. The classic 2.65 specific gravity of alpha quartz drops to 2.20 in tridymite, cristobalite, and lechatelierite (natural silica glass), as well as in many man-made glasses of commerce which are merely noncrystalline or amorphous solids in the form of super-cooled liquids which can no longer change their shapes (Pauling, 1950). It rises again to 2.50 and 2.93 for keatite and coesite, respectively, and finally becomes a reported 4.35 for stishovite-nearly a 50% range in density for the known physical combinations that silica naturally assumes (Frondel, 1962; Konnert, et al., 1973; Pecora, 1960).

Jan 1, 1975

By R. M. Hudson

Equilibrium constants have been determined for the jeaction C (in steel) + H2O = CO + H2 as a function of carbon content (0.013 to 0.74 ujt pct) and temperature (1200° to 1800°F) by using a flow system in which the water-vapor content of various gas mixtures containing hydrogen, carbon monoxide, and nitrogen was systematically controlled. The equilibrium partial-pressure ratio K1 = PcoPH2/PH2O was obtained for two low-carbon steels and four Fe-C binaries from a series of runs made at each temperature. By comparison of Ki with the analogous ratio for the reaction C (graphite) + H2O = CO + H2, the activity of carbon in steel (ac) was comDuted for each temperature and carbon content studied. From these data values of the equilibrium constants for two other carburization-decarburiza-tion reactions of importance were estimated. The chemical compositions of the two steels and four Fe-C binaries used are given in Table I. Specimens of Steel E were cut from a 0.035-in.-thick commercially box-annealed and temper-rolled lot of a low-carbon low-metalloid steel. Steel F was a commercially hot-rolled rimmed steel that was cold-reduced at the Laboratory to a 0.059-in. thickness. Fe-C binaries A, B, C, and D were vacuum-melted and poured, hot-rolled, pickled, and cold-reduced at the Laboratory to furnish specimens 0.035 in. thick. Sheet specimens were cut from all lots to approximately 3/4 by 3 in. by gage and were vapor-degreased with trichlo-roethylene and weighed before heat treatment. Heat treatments were carried out in a hinged-top Hevi-Duty electric furnace with a Vycor-glass tube. When the furnace was at the desired

Jan 1, 1965

By Kenneth M. Ritchie

Mineral wool is a term applied to man-made fibers of silicate glass with useful properties resulting from their fibrous nature. In contrast with crystalline fibrous minerals such as asbestos, mineral wool fibers are amorphous, solid filaments produced by drawing from molten liquid and subsequent cooling. Chemically they are silicate glass with varying percentages of metallic oxides, especially those of aluminum, calcium, magnesium, iron, and in glass wool, sodium, potassium and boron. Other elements such as manganese, titanium, sulfur, etc., result from their presence in the raw materials used and are not purposely added. In the United States, mineral wool is a generic term and may be applied to rock, slag or glass wool. In Europe, glass silk and silicate cotton are products in the same category, but the term mineral wool is less commonly used. Current usage is to ignore the actual source and to differentiate products on a composition basis; thus rock and slag wools have about 35-45 pct of silica, while glass wool has 54 to 60 pct. Much mineral wool of slag origin is called "rock wool," and this practice is increasing, although wool made of slag from lead or copper refining is often referred to as "lead slag wool." Its greenish-gray to greenish-black dark color, due to 5-25 pct Fe (reported as FeO), distinguishes it from "white" wools made from iron, blast furnace slag containing only 1-2 pct FeO or Fe203. Most mineral wool is used for thermal insulation against heat and cold; sound absorption and isolation are probably the next most important uses. Both its thermal and acoustic values result primarily from the physical structure of the heterogeneous mixture of fibers and air which is the form in which the fibers are first obtained and handled. For this reason, within fairly wide limits, differences in chemical composition are relatively unimportant, and for most conventional applications all types are competitive in properties and value. Mineral wool intended for extreme conditions of high temperature, acid resistance and special purposes must have a chemical composition which will insure the desired properties. This may differ greatly from that of ordinary wools; for example one product approximately 98 pct Si02 and another consisting of 50 pct A1203 and 50 pct Si02 are produced and sold for high temperature service up to 2000°F or more. These are considerably more expensive to manufacture and their cost limits their use. Historical The manufacture of mineral wool consists fundamentally of a process which subjects molten material to shear and/or tensile forces that draw them into fibers. The liquids are cooled at a rate which solidifies them quickly. As a solid glass they are technically super-cooled liquids since they have no true melting point. The drawing out of glass into thin rods, filaments and tubes was known from very early times, and present day continuous production of glass filament for textiles was evolved gradually by adapting hand methods to automatic machinery. Rock and slag wool manufacture had a somewhat different development. Early explorers reported finding filamentous material

Jan 1, 1960

By W. H. Fitch

HAVING been asked to make some remarks after the reading of Mr. Dyrssen's paper, I regret that a test started some months ago has not yet been completed, but some of the things which I can tell you at this time seem interesting and shed a little different light on the idea of a recuperator. The device referred to is becoming more than. a recuperator, largely taking the place of a regenerator. I assume there is familiarity with the sketches that I presented in October, 1926, before the Engineers' Society of Western Pennsylvania, describing our re-cuperator combination with checker chambers, and I have additional ones to show at this time. The follow-ing remarks will deal with modifications that have been made. At that time I suggested the gases leaving the regenerators at, say, 1400°, be reduced to 500° F. The opinion of the operating men consulted since that time is that, under the best operating conditions, the tem-perature may be 750° to 800° F. after the recuperator and on entering the stack. While the lowest final temperature of the gases en-tering the stack is important from the economic stand-point of fuel burning, and operating in general, it is not the whole story. The method of getting the heat out of the checkers is important. It is believed by many with whom we have talked that a better way is by a combination of checkers and a carborundum re- cuperator of the type described as it will stand all tem-peratures met in practice and might be called a super-refractory.

Jan 1, 1928

pAbad, Leopoldo F., Min, Engr,, Div. of Mines, Bureau of Science Manila, P. 1. '23 Abadilla, Quirico A,, Geol., Lago Pet. Corp Box 172, Maracaibo, Venezuela, '20 Abbey, Robert Graham, The W. W. Sly Mfg, Co Train Ave., Cleveland, Ohio. '21 Abbott, A. N., Mines Supt., Mazapil Copper Co., Ltd Concepcion del Oro, Mexico, '28 Abbott, Clarence E., Mgr., Mines & Quarries, Tenn, Coal, Iron & R. R, Co,, 1242 Brown Marx Bldg,, Birmingham, Ala. '04]

Jan 1, 1928

By Alden B. Greninger

THE time-honored description of the growth of metal crystals to form polycrystalline aggregates is. one in which two important steps are considered: (1) nucleation, and (2) dendritic growth, each dendrite starting from its individual nucleus and resulting (upon slow cooling, assuming no solid phase changes) in a macrograin. This picture of the process of crystallization is incomplete, and it is with the hope of enlarging upon it that the following summary and correlation of experimental results are given. MOSAIC STRUCTURE For an exact definition of the mosaic structure of metal crystals-if, indeed, one can be found that will hold for all metals-one must await the results of much experimental work in this field. The writer's investigations have been. confined almost entirely to copper and a few of its alloys. The following terms are proposed, and will be used in this report: Macromosaic Structure1.-Large-scale mosaic structure; more specifically, mosaic structure of a scale large enough to produce splitting of Laue spots on back-reflection Lane X-ray patterns2. The deviation from exact parallelism of neighboring macromosaics varies from a few

Jan 1, 1935

By T. D. Murphy, G. V. Henderson

The element silicon, with its usual partner, oxygen, plays the same role relative to inorganic materials as carbon and hydrogen play with respect to living organisms. The crystallographic structure of silicon dioxide (SiO2) consists of one atom of silicon well-nigh inseparably bonded to four contiguous atoms of oxygen, a gas of but slightly more than half its atomic weight, forming a three-dimensional network of SiO4 tetrahedra (Dietz, 1968). This wispy arrangement is the fabric of the mineral quartz which is one of the harder, more abrasive, and chemically stable raw materials to be found in Mother Nature's cupboard. Most of us are vaguely familiar with the observation that nearly 60% of the lithosphere to an approximate depth of 10 miles is composed of these two elements, which proportion actually rises to about 75% if the atmosphere, hydrosphere, and biosphere are included (Parker, 1967). Elemental silicon is a brittle steel-gray metalloid with a density of 2.42 and does not occur in nature. In its limited commercial form, which is still brittle and metallic in appearance, its density drops to 2.33. It combines with oxygen to form the gaseous oxide SiO, or the solid dioxide Si02 (analogous to its congener carbon in CO and CO2); a tetrachloride SiCI4 (analogous to CC14); or, combining with oxygen and one or more metal ions, forms the largest rock-making family of all, the silicates. Further, next to the feldspars, quartz is the most abundant known mineral and, in some form or another, accounts for roughly 12% of surficial terrestrial rock. It is this so-called "free silica" to which your attention is chiefly directed in this chapter. In any such consideration of silica, its several crystalline phases with their attendant differing physical properties appear worthy of delineation. Alpha quartz is the only one of this interesting polymorphic family that is thermodynamically stable at normal pressures and temperatures up to about 573°C. The low phases of tridymite and cristobalite can exist in the so-called metastable state below 117° to 200ºC but seldom occur in nature in these two different crystal forms (Sosman, 1965). Opaline silica, now considered by most researchers to be a variety of cristobalite, occurs in abundance and is the only exception. The three remaining polymorphs, keatite, coesite, and stishovite, also are metastable under ambient conditions. Keatite, however, is not known to occur naturally and has only been synthesized in the laboratory. The other two have been identified in submicron sizes and in microscopic amounts, occurring naturally as a result of high order shock-wave pressures generating quite elevated temperatures --such as might accompany the impact of a large meteorite on a hard sandstone terrain (Chao et al., 1962). An intriguing characteristic of these silica minerals, and one which has very practical applications, is their extremely variable densities. The classic 2.65 specific gravity of alpha quartz drops to 2.20 in tridymite, cristobalite, and lechatelierite (natural silica glass), as well as in many man-made glasses of commerce which are merely noncrystalline or amorphous solids in the form of super-cooled liquids which can no longer change their shapes (Pauling, 1950). It rises again to 2.50 and 2.93 for keatite and coesite, respectively, and finally becomes a reported 4.35 for stishovite-nearly a 50% range in density for the known physical combinations that silica naturally assumes (Frondel, 1962; Konnert et al., 1973; Pecora, 1960). Pursuing its esthetic aspects, briefly, silica is well-represented among gem stones which, to qualify as such, must have the attributes of beauty, durability, and rarity (Jahns, 1983). As quartzose gems usually have but one or, at

Jan 1, 1983

By C. F. Floe, M. Cohen, M. B. Bever, V. G. Paranjpe

NITROGEN is becoming recognized as one of the important elements in ferrous physical metallurgy. Several investigations indicate that nitrogen plays a significant part in such phenomena as strain aging and temper brittleness. Nitrogen is known to be a powerful austenite stabilizer and may be a useful alloying element in stainless steels. The hard-enability of steels has been found to be increased by nitrogen. The nitriding and carbonitriding pro- cesses are examples of successful industrial application of nitrogen in ferrous materials. For a complete understanding of the various roles played by nitrogen in ferrous metallurgy a knowledge of the phase relations in the binary iron-nitrogen system is essential. The literature contains a variety of iron-nitrogen phase diagrams. Those suggested by Fry, Sawyer,² Epstein and his coworkers,³,4 Lehrer,5 Eisenhut and Kaupp, and Hägg7,8 differ significantly from one another. Moreover, the most recent of these investigations dates back about twenty years. A re-determination of the entire diagram, therefore, appeared desirable. In addition to the published phase diagrams, investigations have been carried out on portions of the iron-nitrogen system. Bramley and Haywood determined the composition and temperature of the iron-iron nitride eutectoid. The maximum solubility of nitrogen in a iron was investigated by Portevin and Seferian10 and by Diikstra. 11 Several investigators have determined the crystal structure of the various iron-nitrogen phases. In fact, Eisenhut and Kaupp6 and Hägg7 based their entire phase diagrams on the results of such studies. Epstein' and Emmett12 reported lattice-parameter measurements on the E (hexagonal close-packed) phase. Osawa and Iwaisumi13 also studied the change in lattice parameters of the a, ? and E phases with nitrogen content. Brill" and Hägg7 showed that the y' phase has an ordered structure, and Hendricks and Kostingsl5 suggested a structural relation between the E and phases. In a recent investigation Jackl6 arefully studied the super-lattice reflections from the y' and phases. Experimental Procedure A large variety of experimental methods has been used by previous investigators in studying the iron-nitrogen system. These methods include thermal analysis, microscopic examination, X ray diffraction, magnetic measurements, dilatometric analysis and anelastic experiments. Thermal analysis is of low accuracy in determining changes in the solid state. This accuracy is further decreased for iron-nitrogen alloys since composition changes will occur during heating or cooling unless extreme care is taken to use a proper atmosphere. Metallographic methods are of small value . because homogeneous iron-nitrogen alloys of sufficient size can be produced only with great difficulty. The dilatometric method is open to the same objections as thermal analysis in that changes in composition may occur during heating and cooling. Lattice parameter measurements by X ray diffraction can be used satisfactorily for determining phase boundaries if cooling is fast enough to prevent structural changes. In view of the limitations of the various other techniques two methods only were adopted in this investigation, (1) X ray diffraction measurements, and (2) a controlled nitrogenizing method. The second method is an innovation for investigating the iron-nitrogen system, and will be described at length. Materials: All iron-nitrogen alloys were prepared from carbonyl iron powder of the analysis shown in table I. The average particle size was about 20

Jan 1, 1951

By Oliver Bololes

UNDER the able leadership of Samuel H. Dolbear, the Committee on Nonmetallic Minerals furnished a program of sixteen papers comprising three sessions. An outstanding accomplishment in technology presented at the first session by Benjamin L. Miller and C. H. Breerwood is the application of flotation to the purification of limestone used in cement manufacture. In place of selective quarrying to provide high-grade raw material, the quarry-run stone is pulverized and treated in froth flotation cells for removal of free silica and mica. Some advantages are cheaper quarrying, more complete utilization of quarry rock, avoidance of purchasing high calcium stone, lower fuel cost and improvement in the finished cement. Paul M. Tyler presented the general subject of milling methods as applied to nonmetal lies. He pointed out the importance of some of the more recent refinements in ore dressing, and urged the need of a wider appreciation of their possibilities. The gypsum industry of Canada was described by L. H. Cole. Crystal growth during the setting process was illustrated by moving pictures. The Coastal Plain and interior salt

Jan 1, 1935

By A. E. Dwight

Lattice parameters were determined for eighteen equiatornic alloys of the CsCl-type structure, ten of which were previously un-reported. It was found that fomation of the CsCl-type structure in binary alloys of the transition elements is largely dependent on position of the elements in the periodic table. The relative size of the two elements was not found to be a controlling factor. A recent paper by Beck, Darby, and Arora1 corre-lates the occurrence of CsC1-type ordered structures with the position of the constituent elements in the periodic table for the first long period. It was also suggested that a definite increase in relative bond strength between unlike atoms occurred when, in binary alloys of iron-group elements, the other component is changed from a chromium-group element, to a vanadium-group element, to titanium. A later paper by Philip and Beck2 noted that the lattice contraction increased in the order CrFe, VFe, and TiFe. It was also noted by Philip and Beck2 that the lattice contractions of CsC1-type alloys decreased in the order: TiFe, TiCo, and TiNi, which is an apparent reversal of the contractions expected from the position in the periodic table. It was suggested that the increasing lattice contraction is an indication of increased stability, i.e., greater A-Bbond strength. The present investigation was carried out to determine whether the relation of the position in the periodic table to the formation of the CsC1-type structure was also correct for alloys involving the second and third long-period elements. A systematic search was made for CsC1-type structures among equiatomic alloys and for those found, the lattice contraction was determined. EXPERIMENTAL TECHNIQUE The elements Y, Gd, Ti, Zr, Hf, V, and Cb are designated the A group and the elements Mn, Re, Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt, Cu, Ag, and Au are designated the B group. Equiatomic alloys were prepared for 57 AB combinations. The alloys were arc melted in a multicrucible furnace3 in buttons ranging from 5 to 20 g. Chemical analyses were not made, as the charge weights agreed closely with those of the buttons after melting. The alloy buttons were homogenized at 800° to 900°C. Metal log raphic and X-ray specimens were prepared and heat treated at temperatures from 600° to 1200°C. Specimens for X-ray diffraction were usually ground to a powder in an agate mortar; however, needle-shaped solid specimens were used when the alloy was sufficiently ductile to permit their preparation. Diffraction patterns were taken with a Straumanistype Debye-Scherrer camera using filtered Cu or Co radiation. The lattice parameters were obtained in A by plotting the calculated a0 values against the cos29/sin 0 + cos2?/? function and extrapolating linearly to ?= 900. Metallographic control specimens were polished on cloth wheels with diamond paste and etched with various phosphoric and nitric acid reagents. RESULTS The eighteen equiatomic alloys listed in Table I gave evidence of a cubic structure with two atoms in the unit cell, although two of these cubic structures exist only at elevated temperatures and transform to a tetragonal structure on quenching. Nine of these eighteen alloys gave diffraction patterns with super-lattice lines showing that the structure is of the CsC1-type. The lack of superlattice lines in patterns of the other nine alloys may be attributed to the small difference in atomic scattering power of the components. Metallographic study indicates the occurrence of nine narrow single-phase fields at the AB composition. Any or all of these nine may also have a CsC1-type structure. The VFe alloy was found to have a CsCl-type structure by Philip and Beck2 through the use of CrKa radiation (for which the scattering factor of V is anomalously low), whereas the Cu radiation used

Jan 1, 1960

By K. W. Smith, E. A. Thomas

Various grades of synthetic mullite have been developed in recent years to replace or supplement natural sources of mullite deriued from the mullite group of minerals consisting of sillimanite, kyanite, and andalusite. Raw materials and heat treating processes used in making synthetic mullite are described. Chemical and physical data are given for typical grades and crystalline structure is illustrated with micrographs. Use of synthetic mullite as a refractory material in the glass and metallurgical industries is discussed. Mullite (3A12O3.2siO2), the only stable compound formed in the alumina-silica system, is usually present to some degree in all aluminum silicate ceramic products. The formation of mullite is considered beneficial to give rigidity to the structure and is dependent upon the ratio of Al2O3 to SiO2 in the original composition, particle size, degree of mixing, firing temperature, cooling rate, and the presence of auxiliary glass-forming fluxes. Mullite may also be formed at the reaction interface of fire clay or alumina-type refractories in contact with glass or slag melts. The term synthetic mullite is commonly used today to identify a class of sintered and fused aggregates or grains in the alumina-silica system having a highly developed mullite structure but derived mainly from raw materials other than the sillimanite group of minerals. Within the past 15 years extensive research has been done to develop economical processes to form sintered synthetic mullite aggregate to replace calcined Indian kyanite in super-refractories. Severa1 brands of such mullite are now being produced in commerical quantity and finding extensive use in refractories. Based on the service results of such refractories in many applications throughout the metallurgical, ceramic, and glass industry these developments have been considered successful and suitable substitutes for Indian kyanite now appear assured. EARLY DEVELOPMENT The conversion of kyanite, sillimanite and anda-lusite minerals of the sillimanite group to mullite and their use in refractories and porcelain have been discussed quite extensively in the literature by peck,' Grieg,' Riddle and Foster,3 Bowen and Grieg,4 and others and will only be mentioned here for reference to compare properties with synthetic mullite. In 1928, curtis5 reported on the development of a high temperature gas-converter process for forming synthetic mullite. The raw materials were derived mainly from lumps of high alumina clay of the correct natural composition or blends of clays and alumina that was interground and briquetted to form a suitable charge to maintain a surface combustion firing within the converter. Curtis was, no doubt, the first to illustrate by micrographs in natural color the crystalline structure of mullite derived from kyanite and mullite derived by sintering clay and alumina mixtures at temperatures above cone 32 (3123°F) and by electric fusion. In 1937, sei16 was issued a patent covering the use of a mixture of alumina-silica minerals and alumina in the proportion to form a mullite-yielding material at temperatures in excess of 3100' F. During the period from 1930 to 1940, economic conditions were not favorable for the production of synthetic mullite mainly due to an adequate supply of good grades of Indian kyanite ore suitable for conversion to mullite. Uncertain conditions on availability of the Indian kyanite during the early stages of World War II fostered further study on the development of synthetic substitutes. In 1943, McVay and wilson7 reported on an extensive investigation of domestic substitute materials. Their work covered essentially the use of mixtures of electric furnace mullite, calcined topaz, and calcined domestic kyanite. Compositions were found that gave equivalent or better hot load strength than Indian kyanite in mullite-type brick compositions; however, the calcining of the topaz presented certain physical and chemical problems on the disposition of silicofluoride and hydrofluoric acid while the high cost of electric furnace mullite was a limiting factor. In this work it was pointed out that water-quenched fused mullite was found to be unstable on reheat and gave poor hot load strength due to excessive glass present whereas the slow cooled or annealed mullite contained large crystals of mullite and corundum with little glass and gave superior results.

Jan 1, 1961

Jan 1, 1900

By David L. Holt, Walter A. Backofen, Anwar-uI Karim

Specimens of a hydrided Mg-0.5 Zr alloy were strained in tension at 500°C and constant rates of 2 x10-3 5 x 10-3, and 2 X 10" min-1. Hydride-denuded zones formed at grain boundaries normal to the tensile-stress direction as a result of magnesium transport during difusional flow. The width of the zones could be measured and the measurement used for calculating the diffusional component of the imposed tensile strain. The strain from diffusional flow was found to increase with imposed strain at a diminishing rate, tending to saturate at approximately 12 pct. Strain rate sensitivity of flow stress was low. The apparent non Newtonian character of the diffusional flow is attributed to a non Newtonian process acting in parallel with it which could be boundary shear. Fracture grows out of voids that form in the denuded zones. DEFORMATION of a grain by diffusion of atoms from boundaries stressed in compression to boundaries stressed in tension is Newtonian viscous,1-3 and evidence has accumulated in recent years that such a process may be responsible for the high strain-rate sensitivity of the flow stress of super-plastic alloys.4"7 One piece of evidence is that experimental stress: strain-rate relationships can be quantitatively explained.5-7 There is also metallo-graphic evidence of diffusional flow in superplas-ticity, but in a limited amount. The formation of striated bands on the surface of superplastically deformed specimens has been attributed to diffusional flow.5"7 The basis of that attribution came from experiments on a coarse-grained, nonsuperplastic and hydrided Mg-½ wt pct Zr alloy which formed hydride-denuded, light etching zones at tension-stressed boundaries when strained in tension at 270?C.6 The origin of these zones had already been traced to the diffusional flow of magnesium atoms to the boundaries.' The particular observations in the more recent work were of striated-band formation on the surface and denuded-zone formation internally, with both the bands and zones having the same width and appearing at tension-stressed boundaries. It was argued that the bands were a surface manifestation of the zones and hence of diffusional flow. Of course in superplastic alloys which do not contain internal metallographic "markers", the surface bands can be the only metallographic indication. In the present work, denuded-zone formation was utilized, as it has been by others,9-11 to extend the observations of diffusional flow and to measure the strain, ed, resulting from it. Grain size had to be large to measure ed with accuracy. The grain size chosen for this study was -30 , and with that a strain of 10 pct from diffusional flow produces a denuded zone only 3 µ in width. The large grain size naturally precludes superplasticity. The observations of diffusional flow were complemented by determining the strain from the other operative deformation modes: slip, e,, and grain boundary shear, egb. An incremental specimen extension is the sum of increments from slip, and grain boundary shear as well as diffusional flow. Division by a common length is required to convert to strain. If this length is taken as the initial specimen length, then imposed engineering strain, e, is given in terms of the component engineering strains by e = ed + es + egb [1] Stress:strain-rate relationships are determined by the way in which this "strain balance" is made up. EXPERIMENTAL Material. Zirconium hydride markers were introduced into the Mg-0.5Zr alloy by annealing in hydrogen at 450°C for 30 min. The hydride concentration was particularly high at zirconium rich stringers, which was fortunate in that the transverse boundaries at which denuded zones form lie perpendicular to the stringers. Grain size after annealing was 30 µ. Photomicrographs of unstrained and strained material are shown in Fig. 1. Procedure. Specimens were strained in tension with an Instron machine at crosshead velocities of either 2 x 10"3, 5 x X or 1 x 10-2 in. min-'. Specimen length and diameter were 1.0 and 0.2 in., respectively, so that initial strain rates in tests at constant crosshead speed were 2 x 10"3, 5 x X and 1 X l0-2 min-1. Tests were made at 500°C which is a compromise temperature at which diffusional flow is still measurable but grain growth is not active enough to interfere with metallographic measurements. The tests were made in a hydrogen atmosphere. Strain Balance. An equation additional to [I] is eg = ed + es [2] where eg is strain measured from grain elongation. Measurement was made of ed, eg, and, of course, e, which enabled all the strains in Eq. [I] to be determined. For this purpose, strained specimens were sectioned longitudinally, polished, and etched. The strain from diffusional flow, ed, was computed by measuring on photomicrographs the width in the tensile direction of denuded zones at either end of a grain XI, X2, adding them, and dividing by twice the initial longitudinal grain dimension L0, Fig. 2. Reported values are the results of measurements on seventy randomly selected grains; 95 pct confidence limits on ed were +1.5 pct strain. To measure eg, the maximum length, L, and the maximum width, W,

Jan 1, 1970

By Lester Uren

Beginning with theoretical concepts of oil drainage, this paper demonstrates that the flow of petroleum into a well from a stratum of oil-saturated sand of uniform texture increases with the diameter of the well. This conclusion is supported by experimental evidence. It appears that if a well may be reamed to a diameter of 20 ft. within the oil sand, its production will be approximately doubled. A novel method is proposed for forming and supporting a cavity of such proportions within the oil-producing stratum. PETROLEUM occurs, in nature, as a fluid saturating the pore spaces between the grains of porous rocks or aggregations of rock particles such as sand, sandstone, conglomerate, shale, limestone, etc. The oil, under the influence of gas pressure, hydrostatic pressure, gravity, earth pressure, and, perhaps, other natural forces, is caused to flow through the porous "reservoir rock" into wells penetrating the stratum in which the oil occurs. The principal moving force is the pressure of dissolved or occluded natural gas within the oil, though this;, force is assisted by gravity and by the hydrostatic or buoyant pressure of ground water about the edges of the "pool." The wells, providing outlets to the surface, are centers of reduced pressure and the flow of rock fluids into a particular well is usually an expression of the difference in pressure existing between the space within the well and that of the stored oil .within the reservoir rock. The greater this differential pressure, the more rapidly will oil flow from the source rock into the well. Opposing movement of the oil from the reservoir rock into the well are certain natural forces related to the rock structure, such as pore friction and capillarity, and certain others related to the physical properties of the oil, such as viscosity and adhesion. The differential pressure between the well and the boundaries of the area drained by it must be sufficient to overcome the forces opposing flow if there is to be movement of oil into the well. If by any device the resistance to movement of the oil may be reduced, the oil will flow into the well at a more rapid rate and the effective area of drainage will be increased.

Jan 10, 1924

By Harvey T. Kennedy, Charles R. Olson

In many investigations of the performance of petroleum reservoirs the assumption is made that the liquid, if below its bubble-point pressure, is at all times in equilibrium with gas. On the other hand, observations by numerous investigators have indicated that gas-liquid systems including hydrocarbon systems, may exhibit supersaturation to the extent of many hundred psi in the laboratory. Up to the present, there has been no reliable data on which ti judge the actual extent of supersaturation under conditions approaching those existing in petroleum reservoirs. The work reported here deals with observations and measurements on mixtures of methane and kerosene in the presence of silica and calcite crystals. Bubbles were observed to form on crystal-hydrocarbon surfaces in preference to the glass-hydrocarbon interface or to the body of the liquid. Statistically, it was found that the number of bubbles formed per second per square centimeter of crystal surface was a function of the supersaturation only. and the function was evaluated graphically. Supersaturations were observed up to 770 psi, under which condition bubbles formed quickly and with considerable violence. With decreasing degrees of supersaturation, the frequency of bubble formation became less, until at 30 psi supersaturation and lower, no bubbles were observed to form, even though the observation at 30 psi was continued for 138 hours. It was found that silica and calcite crystals had identical effects, within experimental error, in accelerating the formation of bubbles, and that small amounts of water and crude oil had no effect on the results. It is shown that the maximum supersaturation that can exist in a reservoir may be calculated from the data presented and from the area of the rock surface. It is also shown that the number of bubbles formed in the reservoir, in order of magni- tude, may be calculated for any rate of pressure decline imposed on the reservoir by production. The bearing of the number and distribution of bubbles on reservoir performance is discussed. INTRODUCTION A liquid system is supersaturated with gas when the amount of gas dissolved exceeds that corresponding to equilibrium at the existing pressure and temperature. The degree of super-saturation may be conveniently expressed as the difference between the bubble-point of the mixture and the prevailing pressure. Thus, if a mixture having a bubble-point of 1,000 psi at a given temperature exists in single liquid phase at 700 psi at the same temperature. it is supersaturated to the extent of 300 psi. There are many examples of high supersaturations, mostly in aqueous solutions, reported in the literature. Thus, Kenrick, Wismer and Wyatt1 showed that water may be saturated with oxygen, nitrogen or carbon dioxide at 100 atmospheres, and the pressure reduced to one atmosphere without producing bubbles immediately. When liquids are in a state of tension, they may be considered as supersaturated at least to the extent of the tension. The tensile strength of water has been reported as 30 atmospheres by Meyer,1 60 atmospheres bv Budgett. 30 to 50 atmospheres by Temperley and Chambers,4,5 200 atmospheres by Dixon6. and 223 atmospheres by Briggs.7 Vincent8,9 determined the tensile strength of a mineral oil as 45 psi. Gardescu1 maintained pressures for short times in a model reservoir at 115 psi below the bubble-point. It should be noted that the high supersaturations observed were obtained on systems carefully purified to remove particles or surfaces which might promote the formation of bubble; These "nuclei" were considered as contaminants which interfered with the determination of a property of the liquid. In

Jan 1, 1952

By F. Twyman, D. M. Smith

THOSE chemists (they are still greatly in the minority) who use the spectroscope, use it very often, and find it almost indispensable. As a means of detecting minute quantities of the metals it is unrivalled. A metal can be readily distinguished in the presence of any other element, compound, or mixture without the necessity of separation. The qualitative analysis of the metallic constituents of a substance, which the spectroscope gives so easily, is a sure basis for planning a chemical analysis. As the determination of each element proceeds the purity of precipitates may be checked as often as desired. If, possessing these advantages, the spectroscope has been neglected in general chemistry, it is not surprising that it was neglected in metallurgical chemistry; for many of the impurities which are of industrial interest, even when they are present in a metal or alloy in small quantities, are not then always easily detected by the examination of their visible spectrum. The history of the development of the art has been given in Bureau of Standards Scientific Paper No. 444.

Jan 1, 1928

By J. T. Eash, E. M. Wise

Platinum and palladium are the most generally useful, most ductile and least rare members of the platinum family. They have many important applications in the pure state but for other applications it is frequently desirable to harden them and otherwise modify their properties by alloying small amounts of the other platinum group metals with them. These alloys are frequently required to withstand very drastic forming operations and to possess certain mechanical properties to fulfill specific requirements. For these reasons a knowledge of the tensile properties and annealing characteristics of pure platinum and palladium as well as their more useful commercial alloys is important to the user and the fabricator. The present work was undertaken to fill this need. Rather brief (5 min.) annealing treatments were employed to render the data of maximum practical value and all tests were conducted upon 0.050-in. dia. wire, initially reduced 50 per cent in area by cold drawing, for the same reason. Conclusions 1. Pure (thermocouple grade) platinum reduced 50 per. cent by cold drawing exhibits the following tensile properties: ultimate tensile strength, 36,000 lb. per sq. in.; proportional limit, 27,000 lb. per sq. in.; elongation, 2.5 per cent in 2 in.; reduction in area, 95 per cent. When fully annealed by treatment at 1100°C. its properties are: ultimate tensile strength, 20,700 lb. per sq. in.; elongation, 30 per cent in 2 in.; reduction in area, 93 per cent. 2. The addition of alloying elements in moderate amounts markedly increases the strength and annealing temperature without much detriment to the ductility. The behavior and properties of variously hardened platinum alloys are considered in some detail. The behavior of a 20 per cent iridium

Jan 1, 1935

By J. T. Eash, E. M. Wise

Platinum and palladium are the most generally useful, most ductile and least rare members of the platinum family. They have many important applications in the pure state but for other applications it is frequently desirable to harden them and otherwise modify their properties by alloying small amounts of the other platinum group metals with them. These alloys are frequently required to withstand very drastic forming operations and to possess certain mechanical properties to fulfill specific requirements. For these reasons a knowledge of the tensile properties and annealing characteristics of pure platinum and palladium as well as their more useful commercial alloys is important to the user and the fabricator. The present work was undertaken to fill this need. Rather brief (5 min.) annealing treatments were employed to render the data of maximum practical value and all tests were conducted upon 0.050-in. dia. wire, initially reduced 50 per cent in area by cold drawing, for the same reason. Conclusions 1. Pure (thermocouple grade) platinum reduced 50 per. cent by cold drawing exhibits the following tensile properties: ultimate tensile strength, 36,000 lb. per sq. in.; proportional limit, 27,000 lb. per sq. in.; elongation, 2.5 per cent in 2 in.; reduction in area, 95 per cent. When fully annealed by treatment at 1100°C. its properties are: ultimate tensile strength, 20,700 lb. per sq. in.; elongation, 30 per cent in 2 in.; reduction in area, 93 per cent. 2. The addition of alloying elements in moderate amounts markedly increases the strength and annealing temperature without much detriment to the ductility. The behavior and properties of variously hardened platinum alloys are considered in some detail. The behavior of a 20 per cent iridium

Jan 1, 1935

By J. J. Jonas, J. L. Uvira

Equipment was constructed which permitted the hot compression of 99.8 pct Armco iron and 2.8 pct Si steel at constant true strain rates of 0.05 to 1 per sec over the temperature range 600" to 1000°C. A maximum true strain of 1.9 could be attained, followed by immediate quenching or by isothermal annealing. True stress-true strain curves were obtained, and the steady-state flout stress, a, strain rate, i, and temperature, T, were found to fit the following expression: The constants A, a, n', and AH were determined for the two ,materials. The activation energies obtained for Arrnco iron and silicon steel are 66 and 80 kcal per mole, respectively, and approximate those for seu- diffusion and for creep. This indicates that hot compression is a diffusion-controlled thermally activated process. THE hot compression of iron and steel is usually carried out in the austenite temperature range,1"7 as this is the one of greatest interest with respect to industrial hot working. However, a disadvantage of testing in the austenite range is that the hot-worked structure is destroyed by the phase transformations taking place during cooling. The present study was therefore carried out in the ferritic temperature range, and the hot-worked substructures were preserved by rapid quenching after deformation. The substructural results will be described in a separate paper, and the present communication is restricted to the strain rate/stress/temperature relationship observed during hot working. The results of hot-compression testing are usually given in the form of true stress/true strain curves, with a different curve for each temperature/strain rate ~ornbination.',~,~ Sometimes simple algebraic equations are fitted to the curves, so that certain extrapolations or interpolations can be performed.1'2'5 These equations are, however, devoid of mechanistic interpretations. The present study was undertaken to show that hot compression can be described by an equation of the type used in creep studies. That is, it will be shown that the temperature dependence of the strain rate in hot working is well-represented by an Arrhenius term, with an activation energy similar to that for creep. Also it will be seen that the stress dependence of the strain rate is similar to that for creep EXPERIMENTAL METHOD AND MATERIALS The investigation was carried out with the following three ferrous materials: 1) Armco iron; 2) Armco iron with 0.26 pct Mn; 3) 2.8 pct Si steel. The first two materials were utilized for investigations performed in the temperature range 600" to 800°C; the last one was used for tests at temperatures from 600" to 1000°C. The materials were of commercial purity,* as shown in Table I. Cylinders of five different sizes were prepared by strain annealing. The resulting mean grain diameter was 3 mm in the 1-in. Armco iron and 2 mm in the other sizes and grades. Different ratios of diameter/height were used to enable the determination of the coefficient of friction. The specimen faces were provided with concentric grooves, which acted as lubricant holders during compression, as recommended by English and ~ackofen' and others.2'9 Powdered glass lubricants were applied to the samples before hot compression to decrease friction and barreling, following the practice of previous investigator~.~~~~~~~~ Different mixtures of glass powder were used for each temperature, after the determination of suitable compositions by experiment.'' Equipment for Hot Compression. Hot-compression tests were carried out on an adapted 150-ton vertical hydraulic extrusion press and also on a modified high-temperature creep machine. The modified extrusion press was used for temperatures up to 800°C. The following items were added to the press: a) a high-temperature furnace with built-in upper and lower platens; and b) a transmission assembly, which permitted the attainment of logarithmically decreasing crosshead speeds. These accessories are described in detail in Ref. 11.

Jan 1, 1969