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By C. E. Berry

Natural stone or manufactured porcelain pebbles are used as the grinding elements in pebble mills and the mills are lined with stone or porcelain blocks. Steel balls usually form the grinding medium in ball mills, and the mills may be lined with steel. Pebble mills are used to avoid contamination by metal of the material being ground, to avoid rapid wear due to corrosion, and for other specialized reasons. Belgian silex (silica) blocks formerly were used widely for lining pebble mills, because of their good resistance to wear, light color, and low cost, but the importation of these blocks was suspended early in the war. The stocks of Belgian silex diminished so rapidly that it was found desirable to compare the properties of a number of domestic substitutes for use in critical operations. Accordingly, a study was made to determine the best substitutes for fine grinding of white pigment and for certain heavy-chemical process work such as the disintegration of phosphate rock in weak phosphoric acid solution. A comprehensive survey of substitute lining materials was not contemplated. It was stipulated at the beginning of the investigation that only materials on the market, available in large quantities, would be tested and that these should be reasonable substitutes from a wear-resistance viewpoint as determined from known physical characteristics. Marble and limestone, for example, could be eliminated immediately. Quartzite, granite and porcelain were selected as likely substitutes for Belgian silex and were subjected to quality tests. Materials Tested 1. Belgian Si1ex.—Sample blocks of a standard grade were taken from crates in which they had been imported. The stone was light gray in color and contained inclusions of small clusters of quartz crystals as well as light colored portions that might be calcite. This was a siliceous rock which appeared to be of igneous origin. 2. Quartzite.—Samples of quartzite were obtained from a quarry in Minnesota. The blocks exhibited a crystalline fracture. The stone was pink in color and composed of fine quartz crystals bound together with a siliceous cement. 3. Granite A was a fine-grained granite quarried in South Carolina. 4. Granite B was coarse-grained granite quarried in South Carolina. 5. Granite C was a coarse-grained granite quarried in North Carolina. 6. Porcelain A.—Sample blocks of the pebble-mill lining material were obtained direct from the manufacturer. It was white in color and of lower specific gravity than the natural materials. It did not have a crystalline structure. 7. Porcelain B.—Sample pebble-mill lining blocks of the porcelain were received direct from the manufacturer. It was white

Jan 1, 1947

By C. E. Berry

NATURAL stone or manufactured porcelain pebbles are used as the grinding elements in pebble mills and the mills are lined with stone or porcelain blocks. Steel balls usually form the grinding medium in ball mills, and the mills may he lined with steel. Pebble mills are used to avoid contamination by metal of the material being ground, to avoid rapid wear due to corrosion, and for other specialized reasons. Belgian silex (silica) blocks formerly were used widely for lining pebble mills, because of their good resistance to wear, light color, and low cost, but the importation of these blocks was suspended early in the war. The stocks of Belgian silex diminished so rapidly that it was found desirable to compare the properties of a number of domestic substitutes for use in critical operations. Accordingly, a study was made to determine the best substitutes for fine grinding of white pigment and for certain heavy-chemical process work such as the disintegration of phosphate rock in weak phosphoric acid solution. A comprehensive survey of substitute lining materials was not contemplated. It was stipulated at the beginning of the investigation that only materials on the market, available in large quantities, would be tested and that these should be reasonable substitutes from a wear-resistance viewpoint as determined from known physical characteristics. Marble and limestone, for example, could be eliminated immediately. Quartzite, granite and porcelain were selected as likely substitutes for Belgian silex and were subjected to quality tests. MATERIALS TESTED I. Belgian Silex.-Sample blocks of a standard grade were taken from crates in which they had been imported. The stone was light gray in color and contained inclusions of small clusters of quartz crystals as well as light colored portions that might be calcite. This was a siliceous rock which appeared to be of igneous origin. 2. Quartzite.-Samples of quartzite were obtained from a quarry in Minnesota. The blocks exhibited a crystalline fracture. The stone was pink in color and composed of fine quartz crystals bound together with a siliceous cement. 3. Granite A was a fine-grained granite quarried in South Carolina. 4. Granite B was coarse-grained granite quarried in South Carolina. 5. Granite C was a coarse-grained granite quarried in North Carolina. 6. Porcelain A.-Sample blocks of the pebble-mill lining material were obtained direct from the manufacturer. It was white in color and of lower specific gravity than the natural materials. It did not have a crystalline structure. 7. Porcelain B.-Sample pebble-mill lining blocks of the porcelain were received direct from the manufacturer. It was white

Jan 1, 1946

By C. E. Berry

Natural stone or manufactured porcelain pebbles are used as the grinding elements in pebble mills and the mills are lined with stone or porcelain blocks. Steel balls usually form the grinding medium in ball mills, and the mills may be lined with steel. Pebble mills are used to avoid contamination by metal of the material being ground, to avoid rapid wear due to corrosion, and for other specialized reasons. Belgian silex (silica) blocks formerly were used widely for lining pebble mills, because of their good resistance to wear, light color, and low cost, but the importation of these blocks was suspended early in the war. The stocks of Belgian silex diminished so rapidly that it was found desirable to compare the properties of a number of domestic substitutes for use in critical operations. Accordingly, a study was made to determine the best substitutes for fine grinding of white pigment and for certain heavy-chemical process work such as the disintegration of phosphate rock in weak phosphoric acid solution. A comprehensive survey of substitute lining materials was not contemplated. It was stipulated at the beginning of the investigation that only materials on the market, available in large quantities, would be tested and that these should be reasonable substitutes from a wear-resistance viewpoint as determined from known physical characteristics. Marble and limestone, for example, could be eliminated immediately. Quartzite, granite and porcelain were selected as likely substitutes for Belgian silex and were subjected to quality tests. Materials Tested 1. Belgian Si1ex.—Sample blocks of a standard grade were taken from crates in which they had been imported. The stone was light gray in color and contained inclusions of small clusters of quartz crystals as well as light colored portions that might be calcite. This was a siliceous rock which appeared to be of igneous origin. 2. Quartzite.—Samples of quartzite were obtained from a quarry in Minnesota. The blocks exhibited a crystalline fracture. The stone was pink in color and composed of fine quartz crystals bound together with a siliceous cement. 3. Granite A was a fine-grained granite quarried in South Carolina. 4. Granite B was coarse-grained granite quarried in South Carolina. 5. Granite C was a coarse-grained granite quarried in North Carolina. 6. Porcelain A.—Sample blocks of the pebble-mill lining material were obtained direct from the manufacturer. It was white in color and of lower specific gravity than the natural materials. It did not have a crystalline structure. 7. Porcelain B.—Sample pebble-mill lining blocks of the porcelain were received direct from the manufacturer. It was white

Jan 1, 1947

By C. E. Berry

Natural stone or manufactured porcelain pebbles are used as the grinding elements in pebble mills and the mills are lined with stone or porcelain blocks. Steel balls usually form the grinding medium in ball mills, and the mills may be lined with steel. Pebble mills are used to avoid contamination by metal of the material being ground, to avoid rapid wear due to corrosion, and for other specialized reasons. Belgian silex (silica) blocks formerly were used widely for lining pebble mills, because of their good resistance to wear, light color, and low cost, but the importation of these blocks was suspended early in the war. The stocks of Belgian silex diminished so rapidly that it was found desirable to compare the properties of a number of domestic substitutes for use in critical operations. Accordingly, a study was made to determine the best substitutes for fine grinding of white pigment and for certain heavy-chemical process work such as the disintegration of phosphate rock in weak phosphoric acid solution. A comprehensive survey of substitute lining materials was not contemplated. It was stipulated at the beginning of the investigation that only materials on the market, available in large quantities, would be tested and that these should be reasonable substitutes from a a ance viewpoint as determined from known physical characteristics. Marble and limestone, for example, could be eliminated immediately. Quartzite, granite and porcelain were selected as likely substitutes for Belgian silex and were subjected to quality tests. Materials Tested 1. Belgian Si1ex.—Sample blocks of a standard grade were taken from crates in which they had been imported. The stone was light gray in color and contained inclusions of small clusters of quartz crystals as well as light colored portions that might be calcite. This was a siliceous rock which appeared to be of igneous origin. 2. Quartzite.—Samples of quartzite were obtained from a quarry in Minnesota. The blocks exhibited a crystalline fracture. The stone was pink in color and composed of fine quartz crystals bound together with a siliceous cement. 3. Granite A was a fine-grained granite quarried in South Carolina. 4. Granite B was coarse-grained granite quarried in South Carolina. 5. Granite C was a coarse-grained granite quarried in North Carolina. 6. Porcelain A.—Sample blocks of the pebble-mill lining material were obtained direct from the manufacturer. It was white in color and of lower specific gravity than the natural materials. It did not have a crystalline structure. 7. Porcelain B.—Sample pebble-mill lining blocks of the porcelain were received direct from the manufacturer. It was white

Jan 1, 1948

By H. I. Aaronson, C. Laird

Although the past results of X-ray experiments indicate that the broad faces of 0' plates are coherent with their matrix, dislocations lying in arrays have frequently been observed at these boundaries by transmission electron microscopy. Critical experiments employing the latter technique have been carried out in order to determine the origin of these dislocations. It is concluded that 8' plates are essentially coherent with the matrix at their broad faces throughout the aging temperature/time envelope studied. Virtually all of the dislocation arrays observed are deduced to have been formed by plastic deformation accompanying transformation. The proportion of dislocations arising from convexity of the plates is shown to be negligible by comparison with that from plastic deformation. At the higher aging temperatures, a[001] dislocations appeared in moderate numbers. These dislocations were traced directly, however, to the ledgewise dissolution of 0' occasioned by the formation nearby of 0 crystals. On the other hand, since there is a parametric difference normal to the broad faces of the ?' plates, mismatch dislocations do form at their edges. A previous conclusion that these dislocations have Burgers vectors of type a[001] was confirmed directly. The edges of 0' plates were observed to develop octagonal shapes when growing, but circular shapes during dissolution. 1 HIS paper presents the results of an investigation of the interfacial structures of plates of the transitional phase, 8', formed in an A1-4 pct Cu alloy. In a companion paper, Part 11, the effects of these structures upon the migration kinetics of a:?f boundaries are reported. This work is pa.rt of a general program designed to establish the basis of precipitate morphology. The present authors in Al-Ag,1 and whitton2 previously in U-C alloys, have used transmission electron microscopy to examine directly the vander Merwe3-6 networks of dislocations anticipated7 to compensate the small amount of lattice misfit normally founda at the broad faces of Widmanstatten plates. Since the broad faces of 0' plates are considered to be perfectly coherent with the corresponding habit planes in the a matrix,' no dislocations should be present at these faces. Many reports have been published, however, giving evidence to the contrary.10-18 The primary objective of this investigation was therefore to ascertain the nature of these dislocation structures. An attempt to do this is described in the first three sections of this paper. Inspection of the matching of the a and 8 ' lattices at the orientations of the 0:0' boundary corresponding to the edges of 0' plates raises the possibility that these edges may be made up of rather closely spaced edge- type misfit dislocations oriented so as to be sessile with respect to the lengthening or shortening of the plates. Since this structure should severely inhibit migration of the plate edges (Ref. 7, Part II), a situation not originally anticipated,' an experimental determination of the interfacial structure of the edges of 8' plates was clearly in order, and is reported in Section III. Those aspects of the experimental procedure applicable to both Parts I and I1 are presented in the next section. Specific procedures applicable to individual aspects of each investigation, and also the relevant surveys of the literature, are then individually reported in the appropriate sections. I) GENERAL EXPERIMENTAL PROCEDURE The material used in both parts of these studies was the same as that of a previous investigation:" strips of A1-3.93 pct Cu, 0.009 in. thick, prepared as before, solution-annealed at 548°C for 6 hr, and quenched. Details of subsequent aging, and in some cases deformation treatments, are given in the Experimental Procedure sections of the individual parts of both papers. Specimens of the heat-treated strips were electro-thinned as beforeLg and examined in a Philips EM 200 microscope equipped with a goniometer stage. A commercial hot stage, of the grid-heater type and capable of * 30-deg tilt about one axis in the plane of the specimen, was also used for kinetic studies. The usual precaution of calibrating for the additional heat supplied by the electron beam was taken.19 A 16-mm cine cam-I era mounted outside the viewing window was frequently used to record the transformations. Conventional selected-area diffraction and dark-field viewing techniques were used to identify the precipitates in the foils. Normal bright-field images corresponding to two-beam diffracting conditions or dark-field images were employed to characterize the dislocations observed at the interfaces of the precipitates. The application of these techniques to the study of an interphase boundary, and the interpretation of the images,20'21 has been fully described in a previous paper.'

Jan 1, 1969

By E. W. Dewing

The nature of solid solutions of sodium in non-paphitic carbon at temperatures near 1000°C has been investigated by an electrolytic technique. The activity coefficient is found to vary strongly with the heat-treatment temperature of the carbon, and an analysis of the energy terms involved suggests that this is due to variations in the Fermi level. The diffusion coefficient for sodium is in the range implying that the sodium atoms (or ions) are not bound to specific sites on the carbon, in agreement with lack of evidence for specific compounds in the activity -composition curves. In the light of These results phenomena occurring in aluminum reduction cell linings are dis-cussed. It is concluded that sodium migrates by diffusion through the carbon lallice and not the pores, and that A14C9 is formed within the lining hy The excess of NaF invariably found in used linings is formed by this reaction and by air oxidation: There has recently been much interest in the swelling of carbon which occurs when it is made cathodic in an aluminum electrolysis cell, and there is general agreement that the phenomenon is due to the penetration of sodium atoms, derived from the reaction on the carbon lattice. (NaF and AlF3 are constituents of the fused-salt electrolyte.) The low-temperature lamellar compounds of potassium with graphite are well-known, and one compound between sodium and graphite has been reported.4 There is, however, virtually no information on the basic chemistry of the interaction of sodium with nongraphitic carbon at high temperatures, although Dell3 has made some fundamental studies of rates of penetration. At the time the present work was carried out these were not available. Rapoport and samoilenkol had measured rates of physical expansion in a dilatometer, using the fractional increase in length of a carbon specimen after electrolysis in a cryolite bath for 2 hr as an index of susceptibility to cathodic swelling. Work here with a similar apparatus showed that expansion (of a 1.5-in.-diam cylindrical specimen) ceased in less than 20 hr, and that the final expansion was much more reproducible than the value at some intermediate time. This suggested that an equilibrium was being set up, and that a thermodynamic approach was required. The results obtained are not as accurate as had been hoped, but they are the only ones of their type available and have enabled useful conclusions to be drawn. The experimental work was divided into two parts: an investigation of the activity-concentration diagram for sodium in carbon, and a rough determination of the diffusion rate. For the former, most of the experiments were made with petroleum coke even though this is not a form of carbon used in cell linings. It has the advantages, however, that it is a homogeneous material, that it is low in ash, and that its structure is reasonably well understood. Anthracites and coal cokes gave results of the same type as obtained with petroleum coke, but the reprodu-cibility from specimen to specimen was extremely poor. EXPERIMENTAL 1) The Activity-Composition Diagram for Sodium in Carbon. The petroleum coke was ground, pressed at 40,000 psi into plates 19 by 9 by 2 mm without added binder, and heat-treated. The sodium activities were established by an electrolytic technique. The carbon was made anodic in a cryolite bath with an aluminum cathode, and a controlled potential, E, applied so that the sodium activity at the anode was given by ln Na = 1n asa - EF/RT [21 where as, is the sodium activity generated by Reaction [I]. The relative activity is sufficient for many purposes and is simply given by The value of Na not at present known, but when the thermodynamics of the Na-A1 system have been worked out it can be derived from the equilibrium

Jan 1, 1963

By Joachim J. Hauser

Experiments on latent hardening were peyformed by compressing single crystals along a direction perpendicular to the tension axis. The slope and length of easy glide in the tension test were found to depend only on prior deformation in the same slip plane. Prior deformation on a different slip plane changes the stress level of the resulting stress-strain curve. The yield points appearing upon reloading after prior extension and unloading were related to the end of easy glide. SEVERAL researchers have studied the latent hardening due to deformation of a crystal by slip on a slip System after prior deformation. These experiments can be divided into those in which the prior deformation was on the same plane as the subsequent and those in which the two deformation processes were in different planes. In the former category are the experiments of Buckley and Entwistle,1 Parker and washburn,2 and Haasen and Kelly.3 The latter case has not been studied systematically; it was the main purpose of this investigation to produce this type of latent hardening and explain the results in terms of the existing theories of work hardening. In general, tension producing slip on a certain slip system can be preceded by tension, transverse compression or longitudinal compression, each with predictable dislocation movement and intersection. The intersection of dislocations can lead to glissile or sessile jogs, Cottrell-Lomer locks and other sessile dislocations. The effect on the stress-strain curve could depend on which combination of the former mechanisms is operating. Haasen and Kelly3 have studied the yield points which occur in aluminum and nickel single crystals upon reloading after prior unloading in a tension experiment. They attributed this effect to the anchoring of dislocations occurring during unloading. As Cottrell and stokes4 have shown that dislocations cutting through the "forest" could only lead to reversible changes, they attributed the anchoring to the formation of sessile dislocations during unloading. However, different kinds of sessile dislocations could be formed during unloading, and it was the purpose of this experiment to determine whether Cottrell-Lomer locks are responsible for the yield effect and for the end of easy glide. The case where a longitudinal compression is followed by tension along the same axis is commonly referred to as a Bauschinger test. This type of effect was studied by Buckley and Entwistle1 on aluminum single crystals and by Parker and washburn2 on zinc single crystals. In such a test, the tension and the compression activate the same slip plane with opposite slip directions. The use of sideways compression in the present experiments permits the activation of different types of slip systems and the study of their effect on the easy glide region and on the transition between the elastic and easy glide region. The theory of seeger5 for the flow stress in fee materials is applied to explain the latent hardening. EXPERTMENTAL PROCEDURE All the single crystals used in this investigation had an axial orientation close to <210>, called the "0.5" orientation. This is the orientation for which the tensile axis is 45 deg from both the slip plane and the slip direction. The single crystals were grown from the melt under a helium atmosphere using milled graphite boats,=at a rate of 8.6 mm per min. The silver used in the experiment was 99.98 pct pure. The single crystals had a square cross section about 0.9 by 0.9 cm and a length of 14 cm. The orientation of the specimen was determined within ±2 deg by the Laue back-reflection method. The specimens were annealed at 940&apos; ± 2°C in a helium atmosphere for 24 hr and then furnace cooled over a period of 7 hr. The specimens were electropolished in a solution of 9 pct KCN in water. The specimens were tested in a soft-type tensile machine (the load is prescribed) up to 3 pct strain. The stress was increased continuously at approximately 30 g per mm2 per min. The strain was measured over a 5 cm gage length with a mechanical extensometer employing an optical lever. The strain and stress were measured with accuracies of i 2 X 10-5 and ± 2 g per mm2, respectively. The remainder of the stress-strain curve up to 20 pct strain was obtained in a hard-type tensile machine (the strain rate is prescribed). The strain and the stress were measured in that machine with an accuracy of ±2 pct. The compression tests were performed in the hard-type machine using accurately machined steel blocks without lubrication. The blocks were used so as to apply a uniform compression over a length of 13 cm. The strains were measured on the hard-type machine and with a micrometer.

Jan 1, 1962

By W. L. Hill, W. H. Armiger, S. D. Gooch

The physical properties, chemical behavior under thermal treatment, and fertilizer value of fluorine-containing pseudowavellite (hydrous calcium aluminum phosphate) that occurs as phosphate clay admixed with quartz sand in an extensive deposit near Bartow, Fla., were determined by experiments in laboratory, pilot-plant, and greenhouse. When the mineral was heated at 500°C, 80 pct of the phosphorus become citrate soluble. The heated product, however, deteriorates markedly under moist conditions such as obtain in the soil. EXTENSIVE beds of a soft aluminiferous phosphate lie in the Bartow-Pembroke region of Florida. Although the extent of the deposit is unknown, it is thought that the equivalent of at least five million tons of material containing 25 pct P,Os exists on one large mine property alone, and soft phosphates similar in nature are known to occur elsewhere in the state. This aluminum phosphate, unlike fluorapatite, is rendered fairly soluble in neutral ammonium citrate solution merely by heating it at a temperature below 600 °C, a property made the basis of a process patent by the junior author.&apos; The possibility of producing an available form of phosphorus from what has hitherto been a worthless natural phosphate prompted the Bureau of Plant Industry, Soils, and Agricultural Engineering to make a brief study of the Pembroke phos- phate during the war years with a view towards determining the optimal temperature for heat treatment and the reactions involved in the process. The results of this study supplemented by data and information furnished by the junior author are presented in this paper. Description of Natural Phosphate: The phosphate with admixed quartz sand and siliceous matter occurs as a low-grade (8 to 9 pct P2O5) clay-like material that can be beneficiated cheaply by making a water separation of the very fine material from the sand, floating off the fine material, settling the suspension to a thick slurry, and finally de-watering the slurry by vacuum filtration followed by drying. The product dried at 100 °C contains about 16 pct water and 25 pct P2O5, about 1/12 of which is citrate soluble. Partial analyses of representative samples of the crude ore and corresponding concentrate are given in table I. The concentrate is light yellow in color and even after being dried at 100°C sticks very noticeably to laboratory grinding and screening equipment. Under the microscope the ground material is predominantly light brown crystalline aggregates with index of refraction near 1.61. The principal phosphate mineral constituent was identified as pseudo-wavellite with admixed phosphosiderite.2 Pseudo-

Jan 1, 1951

By W. L. Hill, W. H. Armiger, S. D. Gooch

The physical properties, chemical behavior under thermal treatment, and fertilizer value of fluorine-containing pseudowavellite (hydrous calcium aluminum phosphate) that occurs as phosphate clay admixed with quartz sand in an extensive deposit near Bartow, Fla., were determined by experiments in laboratory, pilot-plant, and greenhouse. When the mineral was heated at 500°C, 80 pct of the phosphorus become citrate soluble. The heated product, however, deteriorates markedly under moist conditions such as obtain in the soil. EXTENSIVE beds of a soft aluminiferous phosphate lie in the Bartow-Pembroke region of Florida. Although the extent of the deposit is unknown, it is thought that the equivalent of at least five million tons of material containing 25 pct P,Os exists on one large mine property alone, and soft phosphates similar in nature are known to occur elsewhere in the state. This aluminum phosphate, unlike fluorapatite, is rendered fairly soluble in neutral ammonium citrate solution merely by heating it at a temperature below 600 °C, a property made the basis of a process patent by the junior author.&apos; The possibility of producing an available form of phosphorus from what has hitherto been a worthless natural phosphate prompted the Bureau of Plant Industry, Soils, and Agricultural Engineering to make a brief study of the Pembroke phos- phate during the war years with a view towards determining the optimal temperature for heat treatment and the reactions involved in the process. The results of this study supplemented by data and information furnished by the junior author are presented in this paper. Description of Natural Phosphate: The phosphate with admixed quartz sand and siliceous matter occurs as a low-grade (8 to 9 pct P2O5) clay-like material that can be beneficiated cheaply by making a water separation of the very fine material from the sand, floating off the fine material, settling the suspension to a thick slurry, and finally de-watering the slurry by vacuum filtration followed by drying. The product dried at 100 °C contains about 16 pct water and 25 pct P2O5, about 1/12 of which is citrate soluble. Partial analyses of representative samples of the crude ore and corresponding concentrate are given in table I. The concentrate is light yellow in color and even after being dried at 100°C sticks very noticeably to laboratory grinding and screening equipment. Under the microscope the ground material is predominantly light brown crystalline aggregates with index of refraction near 1.61. The principal phosphate mineral constituent was identified as pseudo-wavellite with admixed phosphosiderite.2 Pseudo-

Jan 1, 1951

By R. J. Wasilewski

The resistivity of single crystal and of polycrystalline metal has been determined between 77° and 1500°K. At comparable purity, the resistivity of the poly crystalline metal differs from that calculated from the axial resistivity values. The observed anisotropy is briefly discussed. A zone refined titanium rod was obtained from F. J. Darnell.1 The hardness of this material varied between 52 and 64 Bhn, indicative of its high purity. Single-crystal specimens were cut out from a few large grains, elongated predominantly along <1120>. Resistance measurements were taken with specimens immersed in liquid nitrogen, solid CO,, and acetone, and at ice point, and then recorded continuously between room temperature and 1200" to 1250°C, throughout at least one full heating and cooling cycle at a rate of l° to 3°C per min. Four probe measurements were taken using spot-welded Pt wire 0.003 in. in diam as potential terminals, and the electromotive force drop was determined poten-tiometrically. A standard resistance, in series with the specimen, served to determine the dc current (generally about 80 ma) in the circuit. In order to eliminate spurious thermal electromotive forces, the circuit polarity was automatically reversed at 5-min intervals, and the mean of the two adjacent readings taken as the true electromotive force value. The discrepancy between the readings at reversed polarities was generally of the order of a few µ v, as all the spot-welded joints were contained within a volume of some 5 mm cube. The relative resistance (R T/R 273o) variation with temperature is tabulated below, and shown in Fig. 1, as measured during the first heating run. The discontinuous drop in resistance, corresponding to the a — ß transformation, started for both initial orientations at 1170°K; i.e., some 15°K above the accepted value of 882°C (1155°K). Judging by the temperature ranse of transformation—some 30°K for the single crystal and 20°K for the polycrystal-line specimen—this difference is believed caused by the solution of the oxygen present initially on the surface of the specimens. The general trend of the resistance vs temperature shown in Fi,;. 1 is in qualitative agreement with that previously reported for polycrystalline titanium metal. 2,3 Significant anisotropy is, however, indicated by the crossing over of the curves for <1120> and <0001> orientations at 273°, 650°, and 1000°K. This difference is most startlingly shown in Fig. 2, where instantaneous temperature coefficients (l/R273 x dR /dT) are plotted for both the first heat-

Jan 1, 1962

D. J. DEMOREST,* Washington, D. C. (written discussion ?).-This paper is a real contribution to technical science; it will make it&apos; easier to think accurately about the inner workings of a blast furnace. I was rather surprised to read that the authors regarded as a new discovery the idea that a molten mixture of CaO, A1203, and Si02 is a molten solution of the compounds of these oxides rather than of the oxides in each other. Surely no. chemist with an active respect for the known facts of chemical affinity could believe that these oxides could be melted together without forming compounds, and that these compounds would then dissolve in one another. This work does, however, help to establish what it was supposed must be true. I think it is worth while, in the light of the work of the Geophysics Laboratory, this work of the Bureau of Mines, and that of previous investigators, to visualize what happens as a charge passes down through a blast furnace, thinking especially of the slag-forming materials. These are chiefly kaolin (Al203.2SiO2.2H2O), quartz, and limestone. These substances do not undergo much change until the limestone decomposes at about the middle of the furnace, whereupon the chemical affinities of CaO and SiO2 must begin to he active; especially if there is any amorphous Si02 present. This forms CaSiO3, and the SiO2, CaSi02 and Al2-032SiO2 then come together to form the binary and ternary eutectics so well located by the work of the Geophysics Laboratory. No matter how much lime has been charged into the furnace, the formation of this eutectic will start it about the same height in the furnace and the gangue will start to get pasty at the same height. If the charge is such that the

Jan 4, 1918

The Inspiration ore body was discovered in 1904, but a 50 -ton mill which was installed to treat the disseminated copper ore promptly failed. The original Inspiration Company then gave way to another, backed by W. B. Thompson, which found 40 million tons of ore. Control then passed to Anaconda and Dr. Louis Ricketts took charge as consulting engineer. He abandoned the mill which had been partially built (to the horror of the stockholders, according to Ira Joralemon) and spent a year and a million dollars experimenting with flotation. The first large copper flotation plant was then built and recovered 50% more copper than had previous gravity mills. It, of course, was highly successful and became the forerunner of modern flotation plants. Inspiration is distinctive as the first fully integrated copper operation in the United States. Three open pits supply sulfide ore to the concentrator and mixed oxide and sulfide ore to a vat leaching and electrowinning operation with leached ore also being sent to the concentrator. In addition, dump leaching supplies pregnant solution for scrap iron precipitation. Inspiration has recently constructed an electric furnace smelter and also operates a continuous casting and rod plant. The new primary 54 in. by 74 in. crusher was completed in May of 1972 and replaced an older unit which was in the way of the open pit development. It is of an unusual circular silo design, which permits dumping 0 from two positions at 90 from each other. One dumping position is in line with the spider, while the other one is at right angles to it. A box girder splitter bar hung from the dump pocket slopes downward from the second dump point, across the spider cap, and rests on the pocket bottom. This splitter was not installed to protect the spider but was to aid in distributing wet ore being dumped from that position to both sides of the spider. Any large amount of wet ore delivered to one side of the spider would pack in the crusher cavity. The round front wall of the 18 ft (5.5 m) deep pocket is unlined except for light steel protection at the top, while the straight back wall is lined with vertically positioned railroad rails. Water for dust suppression is sprayed into the pocket through a cluster of 3/8 in. (9.5 mm) nozzles at the back of the pocket. About 5 gpm (19 lpm) of water are mixed with 90 psi (620 kPa) air upstream of the nozzles to produce a fog which is effective in dust control. The 54 in. Allis -Chalmers gyratory is placed mostly within one quadrant of the circular enclosure to permit placement of the apron feeder on the lowest level in the proper position to transfer crushed ore to the

Jan 1, 1978

By R. Hogg

INTRODUCTION As mineral particles are made smaller and smaller, it follows that their surfaces assume a greater and greater importance. In the extreme, the colloidal systems are characterized by the complete dominance of surface over bulk properties. Surface characteristics and properties will clearly influence any fine-particle processing operation. Comminution, for example, is a process of creating new surface. Agglomeration, on the other hand, may involve the reduction of surface area and the forces involved are generally surface forces. All mineral separations, solid-solid as well as solid-fluid, involve the treatment of two or more phases (solid plus liquid and/or gas). As the interfacial area increases, so will its effects on processing. Both physical and chemical separations are influenced by interfacial phenomena. Gravity separations are usually performed in a liquid phase and may be affected, for example, by the wetting characteristics of the solids. Flotation processes, of course, are based on the exploitation of differences in surface properties. Hydrometallurgical processing usually involves interfacial chemical reactions, e.g. leaching. The rates of such reactions depend on surface area and may be influenced by electrochemical effects in the electrical double layer at the solid-liquid interface, or by adsorption of reactant and/or product species from solution. In characterizing a mineral surface, it is important to consider first the surface area, since this determines the relative importance of the interfacial effects. The structure and chemical composition of the surface, which may depend on segregation of impurities within the solid and on adsorption from the external environment as well as on the bulk composition of the solid, will generally determine such

Jan 1, 1980

By A. C. Fraker, H. H. Stadelmaier

WIENER and Bergerl reported the existence of the nitrides Fe3NiN and Fe3PtNwith a cubic L1&apos;2 structure. The present note shows that a similar nitride Fe3PdN can be observed and that the composition range between the iron nitride Fe4N and the nitrides Fe3NiN, Fe3PdN, and Fe3PtN is occupied by single-phase cubic nitrides with structures intermediate between L1&apos; and L1&apos;2. The materials used in this investigation were electrolytic iron of 99.9 pct purity, carbonyl nickel of 99.7 pct purity, sponge platinum of 99.95 pct purity, and palladium sheet of 99.8 pct. purity. Binary alloys of the transition metals were induction-melted in a crucible of fused alumina, powdered, and screened to a particle size of - 200 mesh. The powders were nitrided at 600°C in a gas mixture of ammonia and hydrogen, and the crystal structure was determined with the aid of a Wilson powder camera. The results are compiled in Table I together with information from the paper of Wiener and Berger.1 The compound at the nominal composition Fe3PdN has a diffraction pattern with prominent reflections of a face-centered cubic lattice (h2 + k2+l2 = 3, 4, 8, 11, 12, 16) and weaker superstructure lines (h2 + k2 + 12 = 1, 2, 5, 6, 9, 10, 13, 14). With decreasing palladium content the superstructure lines become weaker and approach the intensity of those of Fe4N. No analysis was made of the intensities, but it can be assumed that the structure is that found by Wiener and Bergerl in Fe3NiN and Fe3PtN, namely L1&apos;2 (perovskite structure) with both palladium and the interstitial nitrogen fully ordered. The dependence of the lattice constant upon the solute atom (Ni, Pd, Pt) content can be explained tolerably well by simple lattice expansion due to subsequent work confirms this suggestion, it will be of significance to order-disorder theory. The author is grateful to Lester Guttman for discussions on this topic.

Jan 1, 1961

By Benjamin C. Craft, Frank Perkins

The wall-building properties of salt-water muds can be maintained at high temperatures by additions of gum karaya, gum ghatti, gelatinized starch, or commercially prepared starch. A germicide should be used to prevent fermentation. Introduction The behavior of drilling mud has received special attention from the petroleum industry within the past few years in numerous research projects dealing with such subjects as chemical treatment, gelation, and filtration characteristics. The importance and control of filtration, or water loss, is readily apparent* It affects the analysis of side-wall cores and interpretation of electric logs; it controls to a large extent the work of primary cementing, reduces the amount of expensive fishing, and permits the running of long strings of casing. It has been found that among the many factors that have an adverse effect on filtration, the presence of electrolytes, in general, and of salt, in particular, is outstanding. The effect is one of flocculation of the colloids due to neutralization of the negative charges on the clay particles. This reaction is further increased on the Gulf Coast because high temperatures reduce dispersion, to a minimum, causing increased flocculation in both fresh-water and saltwater muds. The problem of reducing water loss in salt-water muds by the addition of gums and starch at atmospheric temperature has been investigated,&apos; and many successful field tests in West Texas indicate its solution. From the work of Byck2 it is concluded that no existing method will permit an approximate determination of the filtration rate at high temperatures from data taken at room temperatures. Filtration should be measured at the ternperature actually anticipated in the well, or at least at a number of lower temperatures and extrapolated over a small range. A laboratory study has been made of the chemicals available for the filtration characteristics of salt-water muds at high temperatures, and the use of germicides to prevent fermentation. Laboratory Investigations Procedure Since the purpose of this investigation was to compare several different gums and starches at elevated temperatures, mud from the same source was used for all the tests. Viscosity was measured in a Stormer viscosimeter at 600 r.p.m. and water loss was determined with a Baroid High-pressure and High-temperature Wall-building Tester3 at temperatures from 80&apos; to 250°F. and at a pressure of 500 lb. per sq. in. for 30 minutes. The samples tested consisted of 150 grams of commercial Louisiana mud, 50

Jan 1, 1943

By Benjamin C. Craft, Frank Perkins

The wall-building properties of salt-water muds can be maintained at high temperatures by additions of gum karaya, gum ghatti, gelatinized starch, or commercially prepared starch. A germicide should be used to prevent fermentation. Introduction The behavior of drilling mud has received special attention from the petroleum industry within the past few years in numerous research projects dealing with such subjects as chemical treatment, gelation, and filtration characteristics. The importance and control of filtration, or water loss, is readily apparent* It affects the analysis of side-wall cores and interpretation of electric logs; it controls to a large extent the work of primary cementing, reduces the amount of expensive fishing, and permits the running of long strings of casing. It has been found that among the many factors that have an adverse effect on filtration, the presence of electrolytes, in general, and of salt, in particular, is outstanding. The effect is one of flocculation of the colloids due to neutralization of the negative charges on the clay particles. This reaction is further increased on the Gulf Coast because high temperatures reduce dispersion, to a minimum, causing increased flocculation in both fresh-water and saltwater muds. The problem of reducing water loss in salt-water muds by the addition of gums and starch at atmospheric temperature has been investigated,&apos; and many successful field tests in West Texas indicate its solution. From the work of Byck2 it is concluded that no existing method will permit an approximate determination of the filtration rate at high temperatures from data taken at room temperatures. Filtration should be measured at the ternperature actually anticipated in the well, or at least at a number of lower temperatures and extrapolated over a small range. A laboratory study has been made of the chemicals available for the filtration characteristics of salt-water muds at high temperatures, and the use of germicides to prevent fermentation. Laboratory Investigations Procedure Since the purpose of this investigation was to compare several different gums and starches at elevated temperatures, mud from the same source was used for all the tests. Viscosity was measured in a Stormer viscosimeter at 600 r.p.m. and water loss was determined with a Baroid High-pressure and High-temperature Wall-building Tester3 at temperatures from 80&apos; to 250°F. and at a pressure of 500 lb. per sq. in. for 30 minutes. The samples tested consisted of 150 grams of commercial Louisiana mud, 50

Jan 1, 1943

THE committee in charge of arrangements for the meeting of the Institute in September has com-pleted its program. The headquarters of the meeting will be at the Palace Hotel, San Francisco, and the registration committee will be at the hotel all day on Sunday, Sept. 24, and from 8 a.m. until noon on Monday. On Sunday afternoon, automobiles will be available for sightseeing trips around the city. Monday will be devoted to technical sessions. In the morning, there will be sessions on Mining and on Iron and Steel; in the afternoon, sessions on Mining and Milling. At these sessions, in addition to the papers mentioned in the tentative list printed in August, there will be presented three papers on the geology, mining and milling of the Comstock lode; one on the Aztec mine, Baldy, N. M.; one on the Colombian oil fields; and one on charcoal precipitation of cyanide solutions. The luncheon on that day will be Dutch Treat, for men only, at the Engineers Club. On Monday evening, there will be an informal buffet supper at the home of F. W. Bradley. On Tuesday morning, a party of 50 men will leave for Hetch Hetchy. During the four days of the trip, the party will see the Priest tunnel and earth dam under construction by steam-shovel and hydraulic-fill methods, the Big Creek shaft and tunnel, early intake power plant and tunnels and the Hetch Hetchy dam under construction. For those who remain in San Francisco, Tuesday will be "San Francisco Day." There will be motor trips to the Presidio, Cliff House, Golden Gate Park, and other points of interest, and shopping trips to Chinatown. On Wednesday, "University of California Day," the party will be guided through the university by members of the Mining Association, the affiliated stu-dent society, and will see the Greak Theatre and not-able buildings. Thursday will be "Leland Standford, Jr. University Day." Automobiles will leave the Palace Hotel at 10 a.m., and will return from the university at 4.30 p.m. Friday has been reserved for trips to the Selby Smelter, to Mt. Tamalpais, or to other points of interest. Arrangements will be made to visit the mines or gold dredges in California, if members desire to do so, but such trips must of necessity be considered special trips and arrangements will have to be made to suit the convenience of the individual or party. The Golf Committee will make arrangements for those who wish to play golf.

Jan 9, 1922

By Earl C. Herkenhoff

Publication of the article "The Flotation Behavior of Digested Asphalt Ridge Tar Sands" by R.J. Smith and J.D. Miller has confirmed and again spotlighted a most significant and important development in the field of tar sand and heavy oil mining. This is the ability to recover 95% of the bitumen in dry tar sands by a hot water process. The initial investigation by Miller and Sepulveda in early 1978. "Separation of Bitumen from Dry Tar Sands," was the first blockbuster. It is disappointing that there has been so little scientific and industry ackowledgement that the authors laid to rest the long entrenched belief that the sand grains had to be "water wetted" for a hot water process to be applicable. Dr. Miller and his researchers at the University of Utah used slightly different mineral dressing terminology in describing their process but it is essentially the old, established technique of high &lids attrition scrubbing at elevated temperatures with a conditioner or modifier, followed by dilution and froth flotation. Similar techniques were described in detail for other nonmetallic minerals in the mid-1940s by Stuart Falconer of American Cyanamid Co. The authors used a 15-minute "scrub" period (or in their terminology "digester step") at 73% solids and 95OC (203°F) in a 0.3 m solution of sodium carbonate-about 4 kg/t (8 lb per st) of tar sand. Flotation was at 10% solids. Obviously, the scrub is an expensive step with respect to energy input but the high recovery of bitumen appears to justify it. Two basic questions then arise: What are the effects of shorter scrubbing time, lower temperature, and less sodium carbonate? Would a two-stage approach be advantageous? That is, could you get the major proportion of the bitumen with a mild scrub and apply the high power and temperature only to the refractory portion? These variables should be evaluated. Apparently, all results were only for rougher flotation. What would the grade and recovery of bitumen be if multiple cleaner flotation steps were employed? We must concede that a 60.62% grade of bitumen leaves considerable room for upgrading. Finally, it should be noted by all executives who approve funds for heavy oil recovery schemes, most of which are variations of in-situ methods, that mining can yield a 95% recovery of bitumen. That is correct, 95%. Imagine what that does to the total barrels recovered from a heavy oil resource compared with the scrawny 30-35% maximum recovery we are getting now. The conclusion-let&apos;s mine heavy oil and tar sands.

Jan 1, 1983

By P. Shahinian, H. H. Smith, M. R. Achter

Crack growth rates are measured at elevated temperature in a resonant fatigue machine from vibration frequency decreases calibrated in terms of crack depth. Crack growth rates in Type 316 stainless steel at 500º and 800°C show a sharp increase with oxygen pressure in an intermediate pressure range and little or no change at high and low pressures. At 500°c, I torr of oxygen reduces the fatigue life by almost a factor of 100 in comparison to that in vacuum and raises the growth rate of shallow cracks by the same At At 800°C the effects are smaller. Changes in slope in the crack growth rate curves are discussed in terms of a model in which rates of surface production and of surface coverage by gas are compared. The use of a calculation method in which the surface exposure time is equal to X/v, where x is the interatomic spacing and v is the growth rate, makes it possible to obtain order of magnitude agreement at 500°C between the observed pressure and the predicted pressure at these slope changes. At 800°C oxidation becomes a .factor and the data cannot be treated by simple adsorption theory. THE decrease in the fatigue life of metals as a function of gas pressure usually follows a stepped curve with virtually all of the decrease concentrated in a sharp drop in a transition zone at intermediate pressures and little or no change at low and high ranges. A number of models, differing in the details of the mechanism, have been offered to explain the shape of the curve. Measurements of crack growth in aluminum as a function of gas pressure by Bradshaw and Wheeler&apos; and Hordon2 demonstrated opportunities for quantitative comparison to evaluate the proposed models. Since comparable data were lacking at high temperatures, in the present work rates of crack propagation were measured in Type 316 stainless steel at 500" and 800°C as a function of oxygen pressure. Choice of this material was dictated by two considerations; it is stiff enough at these elevated temperatures to resonate with the regenerative drive on our fatigue machine and it is known to display a large effect of environment. A new method of calculation is described to predict the gas pressure at the critical point. EXPERIMENTAL PROCEDURE Because of the difficulty of measuring crack depths directly at high temperatures, an indirect method was developed based on the decrease in the resonant frequency with the growth of a crack. A reversed bending, constant amplitude fatigue machine, described previously,3 vibrates a specimen at its resonant frequency, automatically records any changes in it and shuts itself off after it has reached a preset value of frequency decrease. The record of frequency change is used to determine the rate of crack growth. Sheet type specimens of Type 316 stainless steel, Fig. 1, incorporated a sharp, shallow notch to localize the formation of a single crack. After machining, they were annealed in a vacuum of l0-6 torr either at 1066" (lot A) or 871°C (lot B) and then electropolished in an acetic-chromic acid solution. Bending strains were measured at 500" and 800°C by an optical technique4 and reported as total strain without correction for the notch. At 500°C, the 0.141 pct strain was 0.085 pct elastic and the remainder plastic. At 800°C the 0.062 pct strain was all elastic. To convert frequency decrease to crack length, calibration curves were obtained by interrupting the vibration at stated intervals of frequency decrease. The crack depth was measured microscopically at a magnification of X400 and reported as the average of the measurement on each edge. Some specimens were sectioned for crack measurement while others were returned to the machine and fatigued further. There was good agreement between the two methods. Before beginning the vibration, the vacuum chamber was first evacuated cold to 1 x 1O-6 torr, then heated to the operating temperature and held there until the pressure was again reduced to 1 x10-6 torr at which time oxygen was introduced to the desired pressure. In this investigation the vibration frequency was nominally 10 cps and a decrease of 0.6 cps was taken as the failure point. The choice of the frequency decrease to represent failure has no appreciable effect on the fatigue life because the crack is growing very fast at this point.

Jan 1, 1970

By H. S. Rankin, E. C. Houston

OLIVINE is considered a valuable potential source of metallic magnesium in the chloride electrolytic process. Treatment of olivine with hydrochloric acid can be carried out under conditions that prevent the formation of gelatinous silicic acid, which would inhibit the reaction by forming a covering around the ore particles. It is our hypothesis that the formation of gelatinous silicic acid is avoided by the dehydrating action of the magnesium chloride, which takes up water to form a series of hydrates and leaves the silicic acid in granular condition. Leaching serves to separate the magnesium chloride from the silicic acid and unattacked ore, which can be treated with fresh acid in successive steps until extraction is essentially complete. The leach solution can be purified by the addition of caustic magnesia and the precipitated impurities removed by decantation or filtration. The resulting magnesium chloride contains: Fe, less than 0.001 per cent; Mn, 0.012 per cent; Ni, none. Chlorinationt of olivine has two major defects: (I) a large part of the chlorine goes to form silicon and iron chlorides, (2) the anhydrous magnesium chloride is held by absorption in the finely divided silica. SUPPLY It is well known that olivine, a silicate of magnesium and iron, is present in large amounts in several localities in the United States. The largest deposits occur in the southeast and on the Pacific Coast.1 The southeastern deposits were surveyed by Lewis2 in 1896 and by Hunter3 in the period 1933-1940. It is estimated that high-grade olivine, conveniently located with regard to transportation and power, is present in excess of 230 million tons above local drainage level in western North Carolina and north Georgia. PREVIOUS TECHNICAL WORK In the past few years, olivine has attracted considerable attention in the refractory field. In the chemical processing industry, however, it has long been thought axiomatic that the cost of processing silicates is an economic barrier to their utilization, especially where more reactive minerals, such as carbonates, oxides or salts, are available. This attitude is not entirely justified in connection with olivine. Unlike most silicates, olivine is readily attacked by acids, chlorine and other reagents without resorting to fusion to break down the silicate structure. Olivine has been suggested as a raw material for making epsom salt by roasting with pyrites.4 Other processes include acid treatments and digestion with calcium chloride.6 Recently a small plant was built near Webster, N. C., for making epsom salt from olivine by treatment with sulphuric acid. This plant is now in commercial operation, producing approximately two tons per day. Olivine is also receiving attention from the fertilizer industry as an inexpensive source of soluble magnesium.

Jan 1, 1942