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By P. de Vitry, Oliver Bowles

The conventional wire saw, introduced in the slate district of Pennsylvania by the Bureau of Mines in 1927, and used thereafter with remarkable success, consists of a three-strand steel cable having a diameter of 93/16 or 54 in. The equipment, methods used, and accomplishments have been described in previous reports.'-I Similar wire saws have been used extensively in Europe, in quarries and in shaping blocks and slabs. During the period 1932-1937, competition in European marble quarries was keen, prices were declining, and orders were not abundant. When orders were received, there was generally an urgent call for speedy delivery. Because of the diversification of demands, it was impossible to maintain in stock marbles of the color, size, and thickness called for, therefore the material generally had to be fabricated after the order was received. The wire saw enabled stone mills to fill such orders promptly. With skillful handling, 7/8-in. slabs could be cut accurately and rapidly with this equipment. It was found, however, that, as the three-strand wire became worn, the cutting speed dropped rapidly and the cut became less accurate. To overcome these difficulties the junior author of this paper, after much experimentation, developed a new type of wire consisting of a single ribbon-shaped strand, twisted as shown in Fig. I. To ensure straight sawing, the twist of the ribbon is reversed from right to left and vice versa every 25 ft. The reversal of the twist is shown in Fig. 2. This is not a new feature; it has been used to advantage with the three-strand wire both in Europe and America for several years. However, some difficulties arise in splicing the three-strand reverse-twist wire, and the claim is made that cutting is less accurate as the wire becomes worn. To make an endless belt, the ends of the single-strand wire are brazed together with Pyrophyllite is a hydrous aluminum silicate (A1²Si4O10(OH)²)1 that, occurs in both the foliated and the massive forms. The foliated variety resembles talc in that it has a greasy feel, a pearly luster, perfect basal cleavage, and usually is white, although in some deposits apple green, gray, brown, russet, and nearly black specimens may be found. The massive deposits of pyrophyllite yield pearl gray to light tan aggregates, some of which are so friable that they may be crushed with the hands into a fine gritty powder. Frequently specimens of the massive variety are studded with crystals of radial structure. The mineral has a specific gravity of about 2.7 and a hardness of 1 on Mohs' scale.' The chemical composition of commercial pyrophyllite reflects the mineralogy of the deposits, which, according to Stuckey12 contain pyrophyllite and quartz, together with chloritoid, sericite, and a few other minerals of negligible importance. The latter, he says, ('are noticed in but small quantities to the extent they might occur as accessory constituents of an igneous rock or as products of regional metamorphism or weathering. . . . Quartz is abundant everywhere except in the very best grades of pyrophyllite." Analyses of specimens from several deposits are listed in Table 1, showing that the silica content varies from 57 to 73 per cent and the alumina from 22 to 33 per cent. Oxides of iron and the alkaline metals are collectively present, with one exception, to an extent of about 1 to 1.5 per cent. Sources At present, North Carolina is the only commercial source of pyrophyllite, although the mineral has been found in small quantities in many parts of the world. The North Carolina deposits are in the "Carolina Slate Belt," which traverses the center of the state in a southwesterly direction. This belt varies from 8 to 50 miles in width. Two major deposits of pyrophyllite lie along its eastern boundary, in what is known as the Deep

Jan 1, 1942

By P. de Vitry, Oliver Bowles

The conventional wire saw, introduced in the slate district of Pennsylvania by the Bureau of Mines in 1927, and used thereafter with remarkable success, consists of a three-strand steel cable having a diameter of 93/16 or 54 in. The equipment, methods used, and accomplishments have been described in previous reports.'-I Similar wire saws have been used extensively in Europe, in quarries and in shaping blocks and slabs. During the period 1932-1937, competition in European marble quarries was keen, prices were declining, and orders were not abundant. When orders were received, there was generally an urgent call for speedy delivery. Because of the diversification of demands, it was impossible to maintain in stock marbles of the color, size, and thickness called for, therefore the material generally had to be fabricated after the order was received. The wire saw enabled stone mills to fill such orders promptly. With skillful handling, 7/8-in. slabs could be cut accurately and rapidly with this equipment. It was found, however, that, as the three-strand wire became worn, the cutting speed dropped rapidly and the cut became less accurate. To overcome these difficulties the junior author of this paper, after much experimentation, developed a new type of wire consisting of a single ribbon-shaped strand, twisted as shown in Fig. I. To ensure straight sawing, the twist of the ribbon is reversed from right to left and vice versa every 25 ft. The reversal of the twist is shown in Fig. 2. This is not a new feature; it has been used to advantage with the three-strand wire both in Europe and America for several years. However, some difficulties arise in splicing the three-strand reverse-twist wire, and the claim is made that cutting is less accurate as the wire becomes worn. To make an endless belt, the ends of the single-strand wire are brazed together with Pyrophyllite is a hydrous aluminum silicate (A1²Si4O10(OH)²)1 that, occurs in both the foliated and the massive forms. The foliated variety resembles talc in that it has a greasy feel, a pearly luster, perfect basal cleavage, and usually is white, although in some deposits apple green, gray, brown, russet, and nearly black specimens may be found. The massive deposits of pyrophyllite yield pearl gray to light tan aggregates, some of which are so friable that they may be crushed with the hands into a fine gritty powder. Frequently specimens of the massive variety are studded with crystals of radial structure. The mineral has a specific gravity of about 2.7 and a hardness of 1 on Mohs' scale.' The chemical composition of commercial pyrophyllite reflects the mineralogy of the deposits, which, according to Stuckey12 contain pyrophyllite and quartz, together with chloritoid, sericite, and a few other minerals of negligible importance. The latter, he says, ('are noticed in but small quantities to the extent they might occur as accessory constituents of an igneous rock or as products of regional metamorphism or weathering. . . . Quartz is abundant everywhere except in the very best grades of pyrophyllite." Analyses of specimens from several deposits are listed in Table 1, showing that the silica content varies from 57 to 73 per cent and the alumina from 22 to 33 per cent. Oxides of iron and the alkaline metals are collectively present, with one exception, to an extent of about 1 to 1.5 per cent. Sources At present, North Carolina is the only commercial source of pyrophyllite, although the mineral has been found in small quantities in many parts of the world. The North Carolina deposits are in the "Carolina Slate Belt," which traverses the center of the state in a southwesterly direction. This belt varies from 8 to 50 miles in width. Two major deposits of pyrophyllite lie along its eastern boundary, in what is known as the Deep

Jan 1, 1942

By Pol Duwez

The effect of the rate of cooling on titanium, zirconium, and thallium has been measured. For titanium-molybdenum alloys, it has been shown that for molybdenum concentration up to 8 pct the rate of cooling has no effect on the transformation temperature, but this temperature decreases progressively with increasing molybdenum content. HIGH strength to weight ratio and remarkable corrosion resistance have often been advanced as the main reasons for the present widespread interest in titanium. For the physical metallurgist, the existence of an allotropic transformation in titanium is another important factor. As in the case of iron, an allotropic transformation may be the fundamental property upon which the response of Ti-base alloys to heat treatment will depend. It is therefore important to study the mechanism of the allotropic transformation in pure titanium and the effect of alloying elements on this transformation. The existence of an allotropic transformation in titanium was reported in 1931 by Schulze.' Later, De Boer et al.' determined the transformation temperature from a discontinuity in the electrical resistivity at 882"42O°C. According to recent work," the transformation temperature is 882.5"&1°C. The crystal structure of the room temperature a phase is hexagonal close-packed and the high temperature fi phase is body-centered cubic.' It is well known that the high temperature /3 phase of pure titanium cannot be retained by quenching to room temperature. Several investigators'-' have shown that in alloys of titanium with metals which are soluble in the @ phase (for example, nickel, molybdenum, chromium, or manganese), the /3 structure can be retained, providing the concentration of the alloying element is greater than a certain critical value. Below this critical value, the alloys transform during quenching, at least partially, into a supersaturated solid solution having the a. structure. This behavior is very similar to that found in some iron binary alloys (Fe-Ni and Fe-Mh, for example) and is an indication that the transformation might occur by means of a shear mechanism analogous to that observed in the austenite-martensite reaction. The present investigation is mostly concerned with the effect of the rate of cooling on the /3 to a transformation. In the first portion of this paper, the results obtained on pure titanium are described. Two other pure metals, zirconium and thallium, were also investigated, because they both have an allotropic transformation like titanium, from an hexagonal close-packed to a body-centered cubic structure. For purposes of comparison, the effect of rate of cooling of the y to a transformation of iron was included in the experimental program. The second part of this paper deals with Ti-Mo alloys. The equilibrium phase boundaries involving the solid state reactions on the Ti-rich side of the system were determined and a study was made of the effect of the rate of cooling on the transformation of the high temperature /3 solid solution. Experimental Procedure Since the main object of the present investigation was the determination of the effect of the rate of cooling on a transformation temperature, the best technique available was that used by Greninger" in his study of the martensite arrest in carbon steels. This method consists of heating a very small sample of metal to which fine thermocouple wires are .attached, cooling the sample rapidly by means of a blast of helium, and recording the temperature vs. time curve on an oscillograph. The apparatus used in the present experiments was very similar to that described by Greninger, except that the heating coil was made of molybdenum wire (0.040 in. in diam) and the assembly was placed in a bell jar under vacuum of 10" mm Hg or less. The specimen con-

Jan 1, 1952

By Jack Washburn, E. R. Parker

Kinking in zinc single-crystal tension specimens was observed under conditions of low stress and high temperature. Kinking is discussed in relation to other plastic bending phenomena on the basis of dislocation theory. Experiments on the stress-induced motion of small angle boundaries are reported. KINKING was first reported by Orowan1 as a new deformation mechanism. He observed the phenomenon in cadmium single crystals loaded in compression. Glide lamellae in a local region of the rod were observed to snap over suddenly to a tilted position, resulting in a sudden shortening of the specimen. Between the tilted portion and the rest of the crystal there were fairly sharp boundaries, with the slip plane assuming approximately mirror image positions on opposite sides of these boundaries. Orowan considered the boundaries to be regions where dislocations had concentrated. Hess and Barrett' observed the formation of kinks in critically oriented zinc compression specimens. It was found that the sudden snapping over of the tilted region was not an essential part of the kinking phenomenon but rather was associated with the method of loading. Kinking was explained on the basis of the accepted mechanisms of slip and flexural glide. It was also suggested that a kink can be considered as a special type of deformation band. During a recent investigation of the effect of surface condition on creep of zinc single crystals," a similar phenomenon was observed in crystals which were loaded in tension. The specimens were 0.4 in. diam cylindrical rods with a free length of 4 in. between end connections. All of the crystals were tested at a constant load. adjusted to give an extension rate of approximately 0.05 pct per hr. Kinking, as shown in Fig. 1, occurred in some of the tests performed at temperatures above 200°C. Kinking was observed in specimens varying widely in initial orientation, scattering about a 45" angle between the slip plane and the specimen axis. The condition leading to kinking in tension appeared to be non-uniform distribution of flow along the gage length combined with the restraint imposed by the tensile load. At low temperatures and fast strain rates, the distribution of strain throughout the midsection of tension specimens was generally quite uniform; therefore, bend planes developed only near the ends as described by Miller.4 However, at high temperatures under creep conditions it was difficult to obtain specimens in which the distribution of flow was uniform. Some of the factors which may have caused differences in flow stress along the length of the crystals are: Nonuniform distribution of impurities, accidents of growth (lineage structure), slight bending or other damage during handling, surface conditions, and strain-aging characteristics due to dissolved nitrogen." Plastic flow, once started in a local region, often continued to a relatively large strain before other parts of the gage length became active. Under these conditions a series of kinks, such as those in Fig. 1, were produced. Fig. 2 illustrates how a nonuniform distribution of slip produces bending moments which- are responsible for kink formation. If no plastic bending were to occur while the rod extended by pure slip in two separate sections of the rod, it would assume a shape such as that in Fig. 2a. A specimen having this shape and being subjected to a tension load would have concentrations of stress at the concave surfaces C and lower than average stress would exist at the convex surfaces D. Therefore a bending moment is superimposed on the average stress in the regions between C and D. The positions of potential bend planes under these conditions are shown as dotted lines. Actually no such shape as Fig. 2a develops because plastic bending in the region C-D occurs simultaneously with pure slip in the intervening regions. The observed structure of a tension kink is indicated by Fig. 2b. Perhaps the best approach to an understanding of kinking as well as other related plastic bending phenomena, such as the bend planes discussed by Miller,' cell formation studied by Wood et al.,6 and polygonization,7 is consideration of the dislocation model of a bent lattice. Current theories of the slip process postulate generation or multiplication of dislocations at certain lattice imperfections. The mechanism proposed by Frank and Read8 results in continuous generation of concentric dislocation loops which spread out

Jan 1, 1953

By W. B. Morrison

The principal factors influencing the total percent elongation of a lead-tin eutectic and several low-alloy steels which exhibit superplasticity were investigated. These factors are: a) Strain-rate sensitivity of the stress (m). b) Specimen geometry; in particular, diameter-to-length ratio (d0/l0), and surface irregularity (e.g. notches). A feature of the tensile deformation of a superplastic alloy is the early appearance of a neck which continues to extend throughout the test. As a result the total elongation is directly related to the diameter-to-gage-length ratio. The strain-rate sensitivity of the stress varies during extension, mainly because of microstruc-tural changes. A satisfactory correlation exists between the minimum strain-rate sensitivity and total elongation, as indicated in the equation shown below. Notches cause a considerable reduction in total elongation and their effect is greatest at high values of strain-rate sensitivity. An initial notch depth exists below which there is no appreciable effect on elongation. An equation relating elongation to strain-rate sensitivity and specimen geometry is proposed, THE total percent elongation of a tensile specimen is usually regarded as a measure of superplasticity. However, little attention has been given to the fact that total elongation is also a function of specimen diameter and gage length, even though the importance of geometry has long been recognized in the tensile testing of materials in which elongations are relatively small.* In the present study, the effect on superplas- tic extension of the ratio of specimen diameter to length was investigated and an analysis was made of strain distribution along the gage length. Superplastic alloys are characterized by having a flow stress sensitive to strain rate but relatively insensitive to strain.2"' In an earlier study,5 it was found that the strain-rate sensitivity of several low-alloy steels changed during the test and that the minimum value correlated best with total elongation. In the present study, the variation of strain-rate sensitivity during the straining of a lead-tin alloy was investigated. EXPERIMENTAL PROCEDURE Lead-tin eutectic alloy (32 pct Pb 68 pct Sn), made from high-purity lead and tin, was cast in the form of 1-in. diam rod. The rod was cold-rolled in stages to 0.25 in. diam and then swaged to 0.125 in. diam. Samples were cut from the rod at various stages of the mechanical working process. Tensile test specimens were then made by attaching threaded steel ends to the rods by an epoxy-base thermosetting adhesive which required a setting treatment of 2 days at room temperature. The rods were seated in the steel ends in holes approximately 0.01 in. oversize. The test pieces thus made were of various diameters and gage lengths. These were stored at a temperature of about -70°C (-94°F) until required for testing. The distribution of strain along the gage length of a specimen was determined at various stages of the tensile test. The lead-tin alloy was superplastic at room temperature and direct observations during testing were simple. The gage length was divided by reference marks into five initially equal units. These reference marks were made with ink and were reinforced during the test when the initial marks became faint. Photographs were taken, at intervals, of the deforming specimen and measurements of the elongation in each of the gage units were made on these photographs. Tests were also done on several superplastic low-alloy steels whose properties were described earlier.5 The chemical compositions of these steels are given in Table I. A diagram of the notched tensile specimen used in the steel tests is shown in Fig. 1. The specimens were tested at 900°C (1650°F) in a furnace through which a mixture of He + 2 pct H was continuously circulated.5 RESULTS Strain Distribution. Approximately 20 tests on lead-tin alloy specimens were conducted to determine the strain distribution during the test. An example is shown in Fig. 2 of the strain distribution in the gage

Jan 1, 1969

By H. L. Marcus, C. D. Turk

Titanium was physically vapor-deposited by electron beam high rate evaporation. Rates of 50,000 and 85,000Å per min at deposition temperatures of 480°, 535°, and 595°C were used. Deposited thickness ranged front 0.004 to 0.010 in. The evaporated titanium had a high degree of basal Plane texture. The specimens were tested in tension at temperatures ranging from 78° to 520°K. From the data, the yield stress, thermal component of the yield stress, and work hardening characteristics were found as a function of temperature, deposition rate, and deposition temperature. It was found that Taylor's equation, best fit the work hardening data with m = 1/2. MANY investigations have been made on the tensile deformation characteristics of commercial- and high-purity titanium.1"7 The data obtained from these experiments emphasize the fact that the mechanical properties are generally related to the method of production. The correlation of mechanical properties to production history arises from the dependence of impurity concentration on the extraction and melting technique used. Additional effects are derived from crystallographic texturing which can result from fabrication history. Lee and Backofen8 and other investigators9 have shown that crystallographic texturing in titanium sheet has a significant effect on the deformation characteristics. Bunshah and Juntz10 prepared high-purity titanium by high rate physical evaporation techniques. These authors found the deposited material to have a columnar structure with grain sizes ranging from 12 to 104 µ, depending upon the substrate temperature. The room-temperature strengths of the coarse-grained distillate were similar to arc-melted, rolled. and annealed crystal bar titanium. Commercial-purity titanium was also produced experimentally in our laboratory using high rate physical vapor deposition techniques. The commercially pure material has a finer structure than the high-purity distillate,10 and is highly textured. Since the method of preparation and degree of texturing affect the mechanical properties, a research program was initiated to determine the temperature dependence of the yield stress and work hardening characteristics as a function of high rate deposition parameters. This paper relates the results of the investigation. EXPERIMENTAL A) Material Preparation. The titanium was received in the form of commercial-grade 0.096-in.-diam wire which has a composition of 0.016 pct C, 0.0037 pct N, 0.110 pct 0, 0.011 pct H, 0.05 pct Mn, 0.051 pct Fe. balance Ti. The wire was continuously fed into a vacuum evaporation unit as shown schematically in Fig. 1. The deposition chamber was evacuated, purged with argon, and reevacuated to a pressure of 10-5 Torr which was maintained during deposition. A focused electron beam was used to evaporate the titanium from a water-cooled copper crucible. The titanium vapor was condensed onto a preheated titanium substrate. The temperature of the substrate was controlled within ±5°C for the deposition temperatures of 480°, 535°, and 595°C. Control of the input power enabled the use of two deposition rates. 50,000 and 85,000Å per min. The evaporated titanium had a final analysis similar to that of the input titanium, within experimental limits. B) Testing. The evaporated titanium was physically stripped from the titanium substrate and machined into tensile specimens with 1-in. gage lengths. In addition, tensile specimens of as received annealed 35-A titanium sheet with a 20 µ grain size and 45 pct cold-rolled 35-A were also prepared. All specimens were tested in tension in an Instron at a strain rate of 3.3 x 10"4 in. per in. per sec. Proportional limit has been used as a measure of yield strength. Tests were conducted at 78°, 220°, 300°, and 520°K. Metallography, X-ray diffraction, and electron microscopy were used to correlate structure with the deposition parameters and mechanical properties. Room-temperature X-ray measurements were made to determine the phases present. Pole figures and a scans were made to determine deposition texture. Because the vapor deposition was symmetrical about the normal to the substrate, there was no preferred di-

Jan 1, 1969

By C. S. Finney, John Mitchell

The growing popularity in the United States of the vertical-flue even was emphasized when in 1905 the United States Steel Corp. chose the Koppers oven as the type which best suited their requirements. Heinrich Koppers was born on November 23. 1872. at a small farm in Walbeck near Geldern on the lower Rhine. When young Koppers was eight years old, however the family moved away from the farm to the industrial city of Bochum in the Ruhr. Here Koppers attended public school and subsequently served an apprenticeship to a tinsmith before taking a job as a lathe operator with a local steel company. He had ambitions to be much more than a machinist, however, and used his week-ends and evenings to improve his theoretical background by taking courses at a vocational-training school in Bochum. After winning the highest honor the school could bestow (the silver Staats-medaille), Koppers went on to continue his education at the Rheinisch-Westfalische Hüttenschule in Duisberg. One of his teachers there, Fritz Wüst who later became a professor at the Technische Hochschule at Aachen, recognizing Koppers' unusual abilities, predicted for him a great future. In 1894 Heinrich Koppers joined the firm of Dr. C. Otto and Co. in Dahlhausen, and in 1899 while superintendent of the Mathias Stinnes mine he built his first battery of ovens for Hugo Stinnes, the German industrialist. Two years later he started his own organization, and in 1902 he made Essen his headquarters. It was to Essen that a group of engineers from the United States Steel Corp. went in 1906 with an invitation to Koppers to design and supervise the construction of four batteries of ovens at the Joliet works of the Illinois Steel Co. Each battery was to consist of 70 ovens. Arriving in the United States in 1907, Koppers established a branch of his firm in Joliet, and construction began. The first battery was fired on July 27, 1908. Rugged and simple, these ovens incorporated basic design features which were to make the Koppers oven and its future modifications the choice of a very large segment of the by-product coking industry of America. The 280 ovens at Joliet were 35 ft long, 8 ¾ ft in height, and tapered from 21 to 17 in. The total daily capacity of the four batteries was 2240 tons of coke. The ovens were of the new cross-regenerative type; that is, instead of longitudinal regenerators serving an entire battery, as in the older Koppers ovens, cross regenerators for each separate oven were employed. Fuel gas was supplied from the side of the battery through ducts in the brickwork known as gun flues, which reached to the center of the battery under the vertical heating-flues. Removable, ceramic gas-nozzles fitted at the top of each gun flue helped to insure good control over the distribution of the fuel gas, and uniform heating conditions were also promoted by regulating the air supply to, and the suction in, each heating flue. A different refractory w& used for each battery. One was built of American silica brick, one of American quartzite, and two of imported German quartzite. The installation at Joliet proved to be very successful, and in 1911, 490 additional' Koppers ovens were built for the Illinois Steel Co. at the great new steelworks at Gary, Ind. By 1912 the H. Koppers Co. had established its headquarters in Chicago and was rapidly extending its business to include construction for such iron and steel companies as the Woodward Iron Co. at Woodward, Ma. (80 ovens in 1912); the Tennessee Coal, Iron and Rail- road Co. at Fairfield, Ala. (280 ovens in 1912); the Inland Steel Co. at Indiana Harbor, Ind. (86 ovens during 1913 and 1914) ; and the Republic Iron and Steel Co. at Youngstown, Ohio (68 ovens in 1913). In 1914 a group of men in Pittsburgh bought a major shareholding in the H. Koppers Co., and moved the headquarters of the organization from Chicago to their own city. Under its new management the company was highly successful in obtaining a large share of the contracts for by-product installations built during World War I. In 1917 the remaining German interests in the company were

Jan 1, 1961

By Don M. Jackson, Robert W. Howard

Techniques for the epilaxial growth of single -crystal silicon carbide films on silicon were developed. The vapor-phase decomposition and bydrogen reduction of silicon tetrachloride (SiC14) and Propane (C3H8) resulted in clear films of silicon carbide, lip to seveval microns in thickness. The growth took place in a horizontal . silicon epilaxial reactor at 1100°C (pyrometer) at a rate of- 3000Å per minute. Electron diffraction and X-ray diffraction studies demonstrated that the films were single-cyrstal, ß -phase, or cubic silicon carbide. SiO2 film were used to mask areas of the silicon sur-lace in order that the silicon carbide might be grown in controlled geometries. Both n- and p-type films were grown on p-type silicon waters.. Heavily doped silicon films of the same conductivity type as the silicon carbide films were deposited over the silicon carbide in order to affect better probe contact to the structures. when n-type silicon carbide mesas were grown on p-type silicon substrates the de vollage-current relationships between films and substrates were that of junction diodes. These diodes showed a sensitivity to while light ill that the incident light increased forward- and reverse-satro,ation currents, P-type silicon carbide mesas grown on p-type silicon were ohmic rather than rectifying in their voltage -current relationship. No conclusions could he reached concerning heterojunc-tiou rectification in the structure. SILICON carbide is a semiconductor with many interesting properties. It decomposes at temperatures above 2200°C.1 It occurs in two general crys-tallographic forms—hexagonal (a Sic) and cubic (ß Sic)—with the cubic form having a forbidden-gap energy of 2.32 ev and the hexagonal form (specifically the 6H polytype) a gap energy of 2.86 ev.3 It behaves as an extrinsic semiconductor at temperatures approaching 5003C. It has been shown to have a high resistance to radiation damage4 and p-n junctions formed in Sic have been shown to radiate visible light under forward- or reverse-bias conditions. Epitaxial silicon carbide on silicon carbide has been successfully grown through the use of a variety of techniques, such as gaseous cracking of SiCL4 and CC4, nearly all of which require a deposition temperature above 1500°C.6 This paper will cover very recent work on the gas-phase deposition of highly ordered films of silicon carbide on high-quality silicon single-crystal substrates. The films have been shown to ex- hibit junction-rectification properties when geometrically isolated regions are electrically biased with reference to the silicon substrate. There will be no discussion of the mechanism of heterojunction rectification, but the methods of film fabrication, geometry control, and structural evaluations will be covered in detail. Electron diffraction, X-ray diffraction, and diode electrical properties were used to characterize the films and the junctions. GAS-PHASE DEPOSITION OF Sic The techniques for the deposition of silicon carbide films were a logical outgrowth of the standard silicon epitaxial process. The major premise followed was that, for any film to nucleate in an ordered fashion where there is considerable mismatch in lattice parameters (in this case 22 pct), an extremely clean, damage-free substrate surface must be presented to the gas stream. Thus a standard gas-phase HCl etching step was used to prepare the substrates for growth. A minimum of 5 µ of substrate-surface material was removed prior to the deposition of Sic overgrowth films. The techniques used for growing silicon carbide films were those of growing silicon alone, with the added injection of a hydrocarbon gas into the hydrogen and silicon tetrachloride gas stream. The hydrocarbon gases used thus far have been research-grade (99.99 pct) methane (CH4) and propane (C3H8). Propane ultimately gave the best results. The gas flows were controlled through a panel shown schematically in Fig. 1. A hydrogen main stream of 30 liters per min passed through the horizontal quartz-tube epitaxial reactor, while SiC14, C3H8, HC1, and doping gases were injected as side streams. The

Jan 1, 1965

By W. F. Mullen, C. W. Stickler

WITH few exceptions, unit operations in the Pennsylvania slate industry in 1950 did not differ appreciably from production methods described by Behrel and Bowles2-4 several decades ago. Many traditionally picturesque but relatively inefficient hand operations continued to contribute to high operating costs in an industry in which the margin of profit, for various reasons, was admittedly low. As part of a general program in which the Pennsylvania State College has been assisting the slate industry to solve some of its problems, time and method studies were used in an effort to determine the bottlenecks of production flow. The results are as applicable to other stone industries as they are to slate. A study of the basic elements in the production of roofing slate, structural slate, and slate blackboards among selected slate producers revealed comparatively few refinements. Any marked difference in operating method was characterized largely by the available equipment, a noticeable difference in the working properties of the rock quarried by a particular company, and by either the habit thinking or ingenuity of the individual operators. With the hope that significant economies in manufacture might result, all the unit operations were broken down into elements for study and analysis. The greater part of the study encompassed those operations from the quarry rim to the finished product; however, to obtain a reasonable synthesis of time allotments per operation, several analyses of quarrying from the finish of the wire saw cut are included for reference. The complete study of quarrying made by Bowles several years ago resulted in the introduction of the wire saw into the operation; there appears to be a need for as fundamental a change in the processing of finished slate as the wire saw was in the quarrying process. Fig. 1 illustrates the flowsheet of quarried rock from the parent bed to the quarry rim with the basic elements which contribute to the difficulty of removing slate from the ground. In Pennsylvania roofing slate is produced by one of three procedures, many operations of which are quite similar. In the traditional or classical method the quarried rock is reduced by sculping and auxiliary manual treatment to workable size and then is split and dressed (trimmed to size) in the conventional shanty. Archaic as this method might appear, there are several elements that result in substantial savings over more mechanized operations. In a modified version of this method, the block is reduced by sawing and gouging preparatory to splitting and dressing in indoor stations. This method is particularly adaptable to rock which fractures unevenly by conventional sculping methods. In the third and more modern method, reduced block received from the block maker is diamond-sawed to length and finished on a production line. Fig. 2 illustrates the flow pattern in each case. In the modified and more modern plans, dressing is done on mechanically-operated trimming machines, which appreciably reduce the fatigue factor of the operator. However, it should be noted that it is advantageous for the operator to be able to control the speed of the knife to prevent breakage of certain classes of stock. In the classical plan the splitter and dresser normally act as blockmakers also and carry their eighter slabs (equivalent in thickness to eight shingles) into the shanties themselves, all of which adds to fatigue and reduced efficiency. The extremely low investment and operating expense of the classical method has undoubtedly been of paramount importance in its continuation. Production of Mill Stock The production of mill stock is accomplished by less picturesque methods than enter into the production of roofing slate but it is, in the main, relatively more efficient because of the increased use of machinery for handling and for finishing. Mill stock can be classified into two categories as far as difference in production method is concerned: structural slate and blackboards. The significant difference in operation is caused largely by the nature of the rock used for each product with the best and easiest cleaved rock being reserved for blackboards to permit the splitting of large slabs to as little as 1/2 in. in thickness. Structural stock, on the other hand, is split into panels no thinner than 11/2 in. and

Jan 1, 1952

T.B.King (Depaytment of Metallurgy, Massachusetts Institute of Technology)— A valuable contribution of the authors is in the factual information which they have been able to gather; this type of information is quite difficult to obtain. In many respects, however, it would have been better if they had not subsequently embarked on a discussion of the chemistry of the converter process. It seems inconceivable that the authors do not refer to the papers of Schuhmann and his associates14 which have set the thermodynamic foundation for the whole copper smelting operation. In addition, a very useful review on the physical chemistry of copper smelting by Ruddle 5 appeared as long ago as 1953. An examination of this literature would have convinced the authors that there is no cause to be surprised at a correlation between the magnetic content and the silica content of converter slags, though they rightly point out that one should distinguish between the total magnetite content of the slag and the amount of magnetite which may be considered to be in solution. It is not true that the lowest melting converter slag is that corresponding to the eutectic between ferrous oxide and silica. The simplest slag system which can be considered is a three-component system, since both ferric and ferrous iron are present. As Schuhmann, Powell, and Michal have shown, there are lower melting compositions than this eutectic in the ternary system. The most unfortunate impression given by this paper is that the driving force for chemical reaction is determined by the heat of reaction: of course the entropy change must be taken into account. It would have been more correct to list, in Table VI, values for free energies of formation. Nor can it be said that the data in Table VI represent the "best available data." They do not corregtond with any of the recent, acknowledged sources. F. E. Lathe and L. Hodnett(author's reply)— We are pleased that Dr. King finds the factual information in our uawer of some interest. Dr. King suggests that it would have been better if our analysis and discussion of the data had been omitted, largely because our list of references is so. incomplete. If he will carefully read our introduction, he will see that the questionnaire was sent out in the hope of obtaining data which would throw light on certain questions relating to the use of converter refractories. We did not attempt (nor would the AIME have published!) a complete review of the literature on copper converting, as Dr. King has apparently assumed, nor indeed a complete analysis of the data submitted, but tried only to find a sound basis for the choice of refractories, taking into consideration common variations in converter practice. We hope our paper indicates that, by raising the silica content of the converter slag and operating at a higher temperature, the normal circulating load of magnetite can be greatly reduced, and the whole reverberatory-converter operation improved to a major degree, with resultant important savings. Under such operating conditions, chrome-magnesite brick may be expected to stand up better than those of straight magnesite. Regardless of the choice as between these brick types, however, we find the cost of converter refractories to be so low in comparison with other converter costs as to justify operation under the more severe conditions suggested. Valuable as are the papers by Schuhmann and associates and the book by Ruddle, we make no apology for omitting reference to them, nor for using heats of reaction without mention of entropy changes or free energies of formation. Our primary object was to interest the practicing copper metallurgist, with whose language we may claim to be fairly familiar; we think it would have been unwise to include the highly theoretical phases of the subject which Dr. King suggests. The interest shown in our preliminary paper presented at the New York meeting in 1956, and the trends in practice whtat we have observed since that time, suggest that we did not wholly miss the target. In conclusion, we sincerely hope that Professors King and Schuhmann will independently review the data obtained in our questionnaire and submit a paper giving their own recommendations as to the choice of refractories and the particular converter operating conditions which will result in the lowest overall cost of copper smelting and converting.

Jan 1, 1960

By Jack Parker, Bert Caverson

More than 6000 resin-anchored bolts have been installed at the White Pine mine, and their performance has proven excellent in both pull tests and "beam" building. With its improved reliability, resin anchorage will permit a more scientific approach to the design of roof bolting systems, and this should ultimately result in both better support and reduced costs. The White Pine mine lies five miles south of Lake Superior in Ontonagon County. Mich. The orebody occurs in gently dipping upper Keweenawan sediments midway between the Porcupine Mountains and the Bergland Hills, both of which are ranges of steeply dipping Keweenawan extrusives and intrusives.

Jan 1, 1971

By B. C. Mariacher

EXTRACTION of uranium from ores is being ac-complished by processes which. for the most part, subject the entire ore to acid or carbonate leaching. Ore deposits with a U 3 O 8 content below 0.10 pct U 3 O 8 are seldom considered suitable for treatment by leaching. A preliminary concentration that would enrich the uranium content of an ore by a simple, low cost process based on physical properties of the ore might result in some low grade deposits becoming commercial ores. In addition, the process might be employed in existing operations to reduce transportation and leaching costs and to increase capacity of existing leaching plants. A study to attempt the development of a preliminary concentration process for primary uranium ores was undertaken by the Colorado School of Mines Research Foundation under sponsorship of the U.S. Atomic Energy Commission. The objective of this work was to produce concentrates containing 0.25 pct U3O8 from the low grade ores tested. Ores Tested: The main effort was devoted to the low grade primary uranium ores from northwestern Saskatchewan. Samples were obtained from the Beaverlodge operation of the Eldorado Mining & Refining Ltd. Additional primary ores, obtained from deposits in Gilpin County, Colo., contained from 0.07 to 0.10 pct U3O8. Summary of Concentration Tests: The Beaverlodge ore was tested to determine amenability of the ore to concentration by magnetic, electrostatic, gravity, and scrubbing processes. None of these produced satisfactory results. Both gravity and magnetic processes produced fairly good concentrates when closely sized fractions of the ore were treated, but on the basis of treating the total ore, recovery was poor. Preparation of sized fractions and the low capacity of equipment for suitable concentration made these methods impractical. As flotation offered the advantage of treating the total ore without intermediate sizing, the main effort was in this direction. A flotation process was developed that fulfilled the concentration objectives as set by the AEC. Pilot plant testing was used to verify results obtained from laboratory batch testing. Mineralogy: A petrographic examination of the Beaverlodge ore included a study of polished sur- faces and identification of the radioactive mineral by autoradiograph and X-ray diffraction. Approximate quantitative mineral identification was as follows: quartz, 60 pct; orthoclase feldspar, 20 pct; chlorite, 10 pct; carbonates, 5 pct; and miscellaneous minerals, 5 pct. Included in this last group were plagioclase feldspar, pyrite, mica, chalcopyrite, pyroxene, sericite, magnetite, galena, and uraninite. The most general occurrence of uraninite was in the form of crusts and thin coatings on limonite-stained grains of pyrite, quartz, and pyrite-quartz intergrowth. At least 90 pct of the uraninite was still attached to other minerals in a 100 by 200-mesh size fraction. The uraninite crusts were as small as 10 to 20 µ diam, and 5 to 10 µ thick. The Flotation Process Petrographic examinations of the Beaverlodge ore had indicated the impracticability of attempting to concentrate the uranium by floating individual grains of uraninite. Liberation of the uraninite required grinding to sizes below those suitable for flotation. However, there was preferential association of the uraninite with some minerals while others were free of uraninite attachment. The approach to the development of a flotation process was, therefore, based upon an attempt to concentrate the uraninite by floating carrier minerals. The following paragraphs discuss the various stages of the process with regard to the factors tested and the conditions under which best results were obtained. Grinding: The most effective size range for flotation was —150 mesh + 13 µ. The —13 µ material in the final concentrate had a higher U3O8 content than the total ore, but not as high as the average concentrate; however, rejection of slimes before flotation was prohibitive because of the loss in uranium carried in the —13 µ fraction. Grinding techniques which contributed to a minimum production of fines, such as stage grinding, were then employed. Quartz and Silicate Depression: These minerals represented approximately 80 pct of the ore and were free to a large degree of uraninite attachment. Significant improvement in the grade of the concentrate was obtained by depression of these minerals with hydrofluoric acid or sodium fluoride. Promoter: Selective stage flotation of uraninite carrier minerals was simplified by development of a single promoter mixture. The mixture consisted of an emulsion of a fatty acid, fuel oil, and a petroleum sulfonate and was selected after a comprehensive series of tests. It contained three parts by weight of an oleic and linoleic acid such as Emersol 300,

Jan 1, 1957

The pressure of the gas in equilibrium with sphalerite has been determined in the temperature range of 680' to 825°C, using the Knudsen orifice method. A comparison of these experimental pressures with those calculated from thermal data and from other equilibrium measurements shows that the vapor above sphalerite is predominantly dissociated ZnS. Equations have been given for correctly calculating dissociation pressures using the Knudsen orifice method. It has been shown that the experimentally determined pressure is the same, whether the zinc sulphide is sphalerite or not, or a mixture of wurtzite and sphalerite. CONFLICTING points of view appear in the literature on the constitution of the vapor in equilibrium with solid zinc sulphide in the vicinity of 800°C. By comparing the dissociation pressure calculated from thermodynamic data and the vapor-pressure determination of ZnS by Veselovski,1 Lumsden2 has concluded that the vapor consists largely of dissociated ZnS. Sen Gupta,' however, concludes from his spectroscopic determinations that the vapor is largely ZnS molecules. In view of the fact that the thermodynamically calculated' dissociation pressure is higher than that experimentally measured by Veselovski, it seemed in order to repeat Veselovski's measurements. Experimental Procedure The method used for the determination of the pressures in this papel- is the Knudsen effusion cell. The apparatus and procedure were described in a previous paper- from this laboratory on the determination of the vapor pressure of silver. The only difference is that the Knudsen cell in this work is made from platinum and there is no external cover around the cell. The cell is an ordinary platinum crucible of 2.2 cm top diameter with a capsule cover. It was thought that platinum might stand up at these temperatures to the solid and gaseous ZnS, since it was found that the weight of the platinum cell itself did not change appreciably on heating ZnS in it at the working temperatures. To insure that reaction of the zinc sulphide with the cell was not giving' a false value, a stabilized zirconia cell was employed for check runs. Fig. 1 shows the comparison, which is satisfactory. Veselovski previously had measured the vapor pressure of ZnS using a silica Knudsen effusion cell. On repeating his experiment in this laboratory, it was found that ZnS at-tacked the silica cell, giving it a marked frosty appearance. This led to the belief that Veselovski's result:; may be in error. Also, he was operating at pressures above the range ordinarily considered safe for the Knudsen method. The effusion rate was measured by weighing the cell before and after each run. The weight loss during heating to temperature and cooling down was measured and subtracted from the weight loss during the actual run. The zinc sulphide used in this investigation was from two sources: Fisher cp grade, and a sample of pure sphalerite supplied by Mr. E. A. Anderson of the New Jersey Zinc Co. Before and after the series of runs with Fisher ZnS, X-ray analysis showed that both wurtzite and sphalerite were present. However, the ratio of sphalerite to wurtzite increased. All measurements were made below the transition temperature which has been reported" to be 1020°C. The data obtained in this investigation are tabulated in Table I. The pressure was calculated by the usual Knudsen formula" on the assumption that ZnS molecules were effusing. From these data, using pure sphalerite in the platinum Knudsen cell, the vapor pressure of ZnS, in mm of Hg, as a function of temperature is given by the solid line in Fig. 1. The best straight line, as determined by the method of least squares, is given by 14405 logpzns =-14405/T +11.032. A comparison of these results with Veselovski's shows that his results are about 50 pct lower. Discussion The vapor in equilibrium with solid zinc sulphide in the temperature range of this study will consist of Zn, S2, and ZnS mol, since other species of zinc and sulphur' are relatively unstable. The question to be settled is whether or not ZnS is largely dissociated. The derivation8 which follows gives the method of calculating the pressure of zinc and sulphur over solid ZnS, assuming complete dissociation, from Knudsen cell data. The free energy of the reaction 2 ZnS(solid) ? 2 Zn(gas) + S2(gas) is given by ?F?° = -RT In K = —RT In p12p2 where p1 is the zinc pressure and p is the sulphur pressure. If dissociation occurs in a closed system,

Jan 1, 1955

By Robert B. Hoy

If the reader finds that the basic information in a commodity chapter is insufficient, he can consult the appropriate sources in this chapter to find more detailed or more up-to-date information. In these days, technology develops so rapidly that this 5th edition will be somewhat out of date even by the time it is distributed. A comparison of this edition with the 4th edition (1975) of Industrial Minerals and Rocks will clearly demonstate how rapidly the scene changes. One of the best sources of new information, of course, is attendance at technical meetings. For example, the papers presented at the national and sectional meetings of AIME usually discuss new developments in the respective divisions of the society. Frequently this information is available in Preprints. In addition some are printed in Mining Engineering and/or the Transactions of the Society of Mining Engineers of AIME. Furthermore, other professional and trade journals contain articles pertinent to the field. A journal introduced in 1967, Industrial Minerals, published by the Metal Bulletin, Ltd., London, is an excellent source of information. The Mining Journal, Ltd., also in London, publishes a weekly journal, a Mining Magazine (monthly), and a Mining Annual Review. The latter covers the field from three aspects: (1) by commodities, (2) through technical developments, and (3) geographically. The Industrial Minerals Directory 1977, 1st ed., Metal Bulletin Books, Ltd., London, provides addresses of organizations in the field. Other useful magazines and periodicals include Engineering and Mining Journal, Pit and Quarry, Rock Products, and World Mining, all published in the United States. In addition many new books related to industrial minerals have been published since the 4th edition of Industrial Minerals and Rocks. Most of these are included in the bibliography of each chapter in this volume. Another excellent information source is the proceedings of the Forum on Geology of Industrial Minerals. This group, which held its 18th annual meeting in 1982, is sponsored by a state geological survey or another mineral agency on a rotational basis. The proceedings have been published by the various sponsors and are available as indicated in Table 1. Two major sources of basic industrial mineral and rock data in the United States, and also a good source for many foreign countries, are the US Geological Survey and the US Bureau of Mines. The two agencies publish many reports and maps on a variety of geological and mining subjects. In addition, each agency has an indexed list of all their publications with a free service announcing new publications: New Publications of the Geological Survey, US Geological Survey, 329 National Center, Reston, VA 22092 and New Publications-Bureau of Mines, Publications Distribution Branch, US Bureau of Mines, 4800 Forbes Ave., Pittsburgh, PA 15213. The US Bureau of Mines (USBM) publishes annually Minerals Yearbooks which provide statistical data on mineral products including production, consumption, imports and exports, as well as information on new developments. Another very useful USBM series is called Mineral Facts and Problems. Editions were published in 1960, 1965, 1970, and 1975. Four major series of publications by the Bureau are Information Circulars, Reports of Investigations, Mineral Trade Notes, and Minerals and Materials. The last two are particularly good for news of foreign developments. The Bureau of Mines Employee Directory, available at all USBM offices, lists addresses and telephone numbers for all offices as well as same for all commodity and area specialists.

Jan 1, 1983

By Y. A. Topkaya

The placer gold occurrences at Sart Çayl, Manisa, Turkey, the legendary River Pactolus of King Croessus, were evaluated in this study to determine if this deposit contains sufficient recoverable value to justify development and exploitation. The gold occurs both in the upper Neogene conglomerates and the alluvium derived from these conglomerates. The total reserve in the whole region is estimated to be 500 million cubic metres. Samples were taken of the upper conglomerate and in the alluvium in an attempt to determine the amount and the physical nature of the gold. The gold in samples was recovered by screening out barren oversize followed by washing the sand and gravel through riffled sluices. The resulting sluice concentrate was later panned and amalgamated at site. Laboratory cyanidation testing of some samples for control purposes was also done. The average calculated free gold was found to be about 90-100mg/m3 and the size of gold flakes found was quite small. The field as well as laboratory testing of the samples of Sart Çay1 indicated that the potential reserves in this region could only be developed as a sand and gravel operation and the gold could be recovered together with the heavy minerals as a byproduct.

Jan 1, 1984

By Jasper L. Stuckey

GEOGRAPHICALLY, North Carolina consists of three divisions, the coastal plain on the east, the piedmont plateau in the center, and the Appalachian mountain region on the west. Geologically, the State may be divided into two main divisions, an eastern or coastal plain region, and a western or piedmont plateau and mountain region. The eastern region is underlain with unconsolidated sands, clays, marls, and shell limestones varying in age from Cretaceous to Recent. The western region is, in general, underlain with gneisses, schists, slates, sheared volcanics, and igneous intrusives of Pre-Cambrian age. In the mountain and upper piedmont portion of the western region are several areas of irregularly metamorphosed sediments of early Paleozoic age. Throughout the piedmont plateau and a part of the mountain portion of the western region, important areas are underlain with igneous intrusives of late Carboniferous age. Along the eastern edge of the piedmont plateau are two narrow belts, trending northeast-southwest, underlain with sediments of upper Triassic age. Although North Carolina contains a

Jan 1, 1947

By P. Martinez, A. F. Hoyte, F. E. Senftle

The possibility of applying a neutron activation technique for silver exploration is considered. A mobile positive-ion accelerator type neutron source is used to irradiate a small area of rock or soil in situ. By using a short period of irradiation and gamma ray spectral analysis, a technique is shown for silver exploration. Two different mobile units are described. Laboratory and preliminary field tests both indicate that a sensitivity of less than 1 oz of silver per ton of ore can be achieved. The increasing consumption of silver for industrial uses and also for coinage has caused a serious shortage of silver in this country. The silver shortage has been reviewed and analyzed by kiilsgaard1 who concludes that, "The best hope for meeting future demands for silver is through accelerated exploration for precious ores." As almost all the exposed "bonanza" type silver deposits evidently have been found, it is urgent that some sensitive geophysical technique be found to detect large, extended, but generally low-grade, secondary ores, as well as hidden vein deposits. Silver is easily made radioactive by exposure to slow neutrons; hence a neutron activation method appears promising for locating silver deposits. The principles of mineral beneficiation using neutron activation techniques were discussed some years ago.2-4 Using the same approach, a preliminary description5 has been published of neutron activation as a mineral exploration tool. An exploration technique is described in which silver is made radioactive in situ and detected with a gamma radiation counter. The technique is similar to the well-known method used for uranium exploration. THEORETICAL CONSIDERATIONS Elemental silver consists of two isotopes, Ag107 and Ag109, having naturally occurring isotopic abundances of 51.4% and 48.6%, respectively. For short periods of irradiation of silver by thermal neutrons, the long-lived 250 day, half-life isotope, Ag110m, is not produced in significant quantities. However, significant quantities of 2.3 min half-life Ag108 and 24.5 sec half-life Agl10 are formed by the following reactions. Ag108 and Agl10 emit a 0.44 Mev (million electron volts) and a 0.66 Mev gamma ray, respectively. Ag107 + n + Ag108 (2.3 min) Ag109 + n + Ag110 (24.5 sec). Because of the large capture cross section (110 barns) of Ag109, and short half-life of Ag110 (24.5 sec), the 0.66-Mev gamma ray is the most prominent emission from silver for neutron activation periods of about a minute's duration.* The 0.44-Mev gamma ray from Ag108 will also be present, but will be one or two orders of magnitude lower in intensity. The decay scheme of Ag110 is shown in Fig. 1. If the neutron irradiation time is limited to about 100 sec, the Ag110 activity will essentially reach saturation and can be used to detect the presence of silver. In a neutron flux of 10 8 neutrons/cm2/set, the induced 0.66-Mev activity in 1 g of silver will be about 2 x 107 disintegrations per sec. This is about 1000 times the measurable gamma activity of 1 g of uranium in equilibrium with all its decay products; hence there is ample activity for detection. Under the same conditions of activation, most of the other elements do not reach this relatively high disintegration rate. Although this is in favor of the proposed technique, other problems must be considered. For mobile operation, it is desirable to obtain the largest neutron flux to weight ratio. Hence we have used a small 150-kev accelerator-type neutron source rather than an isotopic source such as an americium-beryllium neutron source. By use of remote control system, an accelerator-type neutron source can be safely used without the massive shield required for an isotopic source. Moreover, an accelerator-type source is more versatile in that it allows one to use a flux of either 14-Mev or 3-Mev neutrons, depending on whether a tritium or a deuterium target is used. With a 14-Mev generator, one can obtain a flux of 10 9 neutrons/cm 2/sec, and with a 3-Mev generator, the flux is generally two orders of magnitude less. Although silver will become activated with either generator using proper moderation, detection may be

Jan 1, 1968

By Robin O. Williams

The increase in internal energy as the result of deformation has been measured for lead, aluminum, silver, nickel, iron, and zirconium by using rapid, adiabatic compression. The stored energy increase is roughly Proportional to the strain; the propor-tionality constant increases rapidly with increasing melting point. The fraction of the mechanical energy which is stored increases more slowly, since the strength of the metals also increases with melting point. The values of the stored energy are considered accurate to about 10 pet. The present values appear about 50 pet larger than the more reliable published results where comparisons are possible. It is possible that this difference is due to the high strain rate used in this investigation. Immediately after deformation all these metals release energy at a rate roughly proportional to (time)-'. This release is considered to be associated with dislocation motion but in aluminum (and copper) some additional process seems to be present. This release can represent 20 pet or more of the stored energy. WHEN pure metals are plastically deformed, most of the mechanical energy is converted into heat. The energy remaining within the metal is significant in that it is the energy of the disorder produced and thus detailed knowledge of this energy is a powerful tool in understanding the nature of deformational disorder. While much effort has been expended on this problem, the amount of information available is limited. The situation as of 1958 has been carefully reviewed by Titchener and ever.' The present results have been obtained by a new experimental approach to this problem. The method necessitates high-strain rates which make comparisons with published results less certain, but a high-strain rate is an advantage in that the energy release immediately after deformation can be followed. EXPERIMENTAL PROCEDURE In the experimental method used, the internal (stored) energy is given as the difference between the mechanical work used in deforming the sample and the heat which is released (the first law of thermodynamics). The work is supplied by two identical hammers swinging freely from a fixed height, the available energy being the product of the mass, the gravitational constant, and the distance through which the center of gravity moves. The initial temperature rise of the sample represents the heat produced by the deformation. The sample temperature is determined by a small thermocouple embedded in and supporting the sample. This process can be repeated over and over to produce increased strains. Most samples are run through about five cycles to a total strain of around 0.7. Further details are covered elsewhere. The determination of the heat is dependent upon the sample weight, its specific heat, the rise in temperature, and any gains or losses to the surroundings. One is dependent on published results for specific heals (the values were taken from a collection).3 The values must be accurate to about 0.1 pet in order that they not affect the results. The best values thus do not contribute to the uncertainty, but this is probably not always the case. The accuracy of the temperature rise is limited primarily by knowledge of the thermocouple characteristics over short temperature intervals, but careful calibration eliminates this as an important factor. One can calculate readily the heat flow between the sample and hammers if the time of contact and the sample temperature are known and if there were no oil at the interface. Assuming the maximum temperature difference, upper values for this interchange have been calculated (the time of contact is determined from the decrease in sample length) and it may or may not be significant. However, no correction is colnsidered necessary because of the presence of a thin oil film which has a thermal conductivity much less than the metals. Except for the possible uncertainty in specific heat, the heat is considered to be adequately known. The mechitnical losses which are recognized as important are: 1) friction between the sample and the hammer:;, 2) the kinetic energy in the hammer suspension system which may not be entirely usable, 3) the rebound energy of the hammers, and 4) the vibration of the hammer heads. All these have been covered in detail elsewhere2 and only the more significant points are made here. The friction turns out to be small except for soft materials (lead)

Jan 1, 1962

By R. H. McLean

Jet impingement produces two mechanisms to clean the bottom of a borehole during jet-bit drilling operations. One is an impact-pressure wave in the immediate area of jet impingement. The other is crossflow, which spreads across the bottom away from the pressure wave. Measurements of the vertical distribution of the cross-flow at several positions beneath a 4 3/4-in. tricone jet bit in a laboratory model show that the maximum velocity in the crossflow is directly proportional to the square root of the product of the rate of flow and the velocity of the jets through the nozzles (QV). Other measurements in the laboratory model show that gradients in the impact-pressure wave are directly proportional to the jet QV if the diameters of the nozzles are held constant. Consistency of the basic relationships through changes in the Reynolds numbers of the jets from 31,000 to 93,000 suggests that the laboratory results should be representative of typical flow in field operations having higher Reynolds numbers. Estimates of the impact-pressure waves under conditions other than those in the jet-bit model may be made by comparison with a less complex model—impingement of a jet against an unrestricted flat surface normal to the jet. Equations derived from current jet technology describe the wave in this simple system for a wide range of conditions. INTRODUCTION The efficiency of rotary drilling operations is strongly linked to the efficiency with which cuttings are removed. Cuttings remaining on the bottom of the borehole will impede further penetration by the bit until they are removed. Wasteful regrinding is prevented if the fluid circulated past the bit removes cuttings as rapidly as they are made. Most investigations of bottom-hole cleaning under bits have been concerned with the rate-of-penetration effects of bit type, nozzle configuration, fluid properties, pressure gradients and utilization of hydraulic horsepower. These investigations have shown that drilling muds, weighted to keep the pressure in the borehole greater than in adjacent formations and carrying material which forms a filter cake, apparently plaster cuttings against the bottom, making them difficult to remove. In addition to a demonstration of the factors causing poor cleaning, the most significant result of these previous investigations has been the increased use of jet bits accompanied by better hydraulic programs and better selection of drilling fluids. Undoubtedly, these practices have improved bottom-hole cleaning, but rates of penetration when drilling with muds are still often lower than would be expected with perfect cleaning." Although there is general agreement with the concept that increasing hydraulic energy at a jet bit often increases the rate of penetration by improving cleaning, research workers have differed as to the best criterion for evalyating hydraulics. Some lean toward maximizing the product of the rate of flow and the velocity through the nozzles (QV) others prefer to maximize the hydraulic horsepower at the bit;'"-' "till another says that neither criterion is universally suitable."' This controversy shows that conclusive field evidence has not established the superiority of either of these criteria. Analysis of the fluid flow which cleans the bottom should contribute to resolving the controversy. Impinging jets clean the bottom by creating two mechanisms capable of dislodging cuttings. One is the impact from the momentum of the jet and the other is the flaw parallel to the bottom away from the area of impingement. The impact force appears in the form of a pressure wave on the bottom and, in this paper, is called the impact-pressure wave. The flow parallel to the bottom is called crossflow. Fig. 1 illustrates these two mechanisms. This paper describes crossflow and the impact-pressure wave beneath jet bits and relates them to controllable parameters. Through these relations, criteria for use in designing hydraulics to achieve maximum use of the mechanisms of cleaning are derived. PROPERTIES OF CROSSFLOW CONCEPTS DEVELOPED IN PREVIOUS INVESTIGATIONS Concepts of scavenging the bottom by crossflow have been well discussed by Bobo, et al." They examine the means by which crossflow may create forces on cuttings and conclude that the cleaning action of crossflow can be increased by increasing the velocity of the flow stream close to the bottom. Using boundary layer theory, they indicate that a reduction in the viscosity of the drilling

Jan 1, 1965

By R. A. Greenkorn

This project originated in a practical problem—we needed five tracers that could be used together to locate flow paths in a pilot flood. While tracers for subsurface liquids have been used since the turn of the century,1-15 none of those reported in the literature appeared to be either consistent or quantitative enough for our purposes. Most were used in field systems without controlled experiments to determine the accuracy and precision of analysis, and many were tracers that could not be used collectively. The ideal tracer, of course, would follow the fiuid of interest exactly, traveling at the same velocity as the fluid front. But the ideal is impractical to attain because adsorption-desorption effects cause the tracer to lag behind the front; these effects, plus diffusion-dispersion effects, cause the tracer front to spread more than the fluid front. Thus, our objective was not to locate a tracer that would be ideal for all circumstances but rather, to find one that would approximately follow the fluid, or one that under controlled conditions could be corrected to calculate the movement of the fluid front. We considered tracers satisfactory—(1) if they were easy to analyze; (2) if their breakthrough-elution curves were not too different from those for the chloride ion, a tracer believed to follow the fluid front closely; and (3) if we could calculate from the curves a material balance, at 1.25-PV (pore volume) injected, within 5 per cent of that calculated from chloride curves. Of a possible 35 materials, we selected 13 tracers that could be quickly and easily identified and whose analysis was claimed to be accurate within 5 per cent. Only one of these, tritiated water, was a radioactive tracer. Radioactive tracers are easy to detect even in small quantities, but they require special handling and special equipment. Also, those that can be used together are limited because special equipment is required to separate emissions from the various tracers. Two of the original 13 tracers were eliminated in static tests to determine how accurately and precisely they could be analyzed, and to check on gross adsorption. The remaining 11 were flowed through a 9-ft linear sandstone model, and breakthrough-elution curves were obtained. Finally, three tracers were field-tested as breakthrough tracers. These tests are described in the following sections. The 13 tracers considered in these experiments were EDTA (ethylene diamine tetra acetic acid), fluo-rescein, picric acid, salicylic acid and ammonium, boron (as borate), bromide, dichromate, iodide, nitrate and thiocyanate ions, plus chloride ion and tritiated water. All but the chloride ion and tritiated water were subjected to static sand tests to eliminate the tracers that could not be analyzed quickly and accurately and to eliminate those that showed excessive adsorption. All but two of the tracers, EDTA and salicylic acid, qualified for flow tests on this basis. The procedures used in the static tests (see Appendix A for analytical details) were as follows. Each tracer (in the amount shown in Table 1) was dissolved in 1,000 ml of water. Then, 800 ml of this solution was added to 500 gm of sand, and the remaining 200 ml was reserved as a control standard. The sand-tracer mixture was agitated once a day over a 10-week period, and during this period we analyzed five duplicate samples from this mixture, along with five duplicate samples from the control solution. From the control-sample analyses, we constructed a control chart on which the sand-tracer analysis results were plotted. The control chart, and its use to determine accuracy and precision of analytical results, as well as the amount of adsorption, is described in Appendix B. The results of the static tests are summarized in Table 1, which lists the concentration c (concentration at time t) divided by c, (initial concentration). If there was no adsorption, c/c, = 1. The acceptable deviation from this value varied from tracer to tracer, depending upon the limits of analytical precision established for the different tracers. The best results were obtained with boron, bromide and dichromate, with all values falling within limits of accuracy and precision. Ammonium, iodide, nitrate and picric acid also were satisfactory, although the ammonium results were erratic. Flourescein and thiocyanate were unsatisfactory ini-