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By P. R. Schmidt, N. J. Themelis

A study zvas made of the deoxidation of copper at 1170°C by injecting a jet of carbon monoxide vertically upwards into the melt. The effects of submersion depth (2 to 20 cm), orifice diameter (& to 5 in.), and gas velocity (100 to 3650 ft per sec) were examined. In the oxygen range 0.1 to 1.0 pct 0, the overall rate was conlrolled by gaseoLcs mass Lransfer. The results were interpreted in terms of a rate coefficient per unit depth which was found to be constant with distance along the jet axis and nearly proportional to the orifice Reynolds number in the range 1000 < NReo < 9100. AS the gas flow rate through an orifice submerged in a liquid is progressively increased, at least three regions of bubble formation may be distinguished. At very low rates, the formation of bubbles is practically a static phenomenon, depending on the orifice diameter, the liquid surface tension, and the densities of the two phases. In this region, the bubble size is constant while the frequency of bubble formation increases with gas flow rate.&apos;-3 At higher flows (500 < NR~, < 2100), the frequency of bubble formation reaches a steady value and the bubble size increases with gas flow rate; when the bubbles issuing from the orifice become so large that they start coalescing to form larger bubbles, the turbulence induced in the liquid by the passage of previous bubbles shatters them into small bubbles of varying size. Finally, for gas velocities in the intermediate and turbulent regions of flow (NR,, > 2100) a tangential separation surface is created around the jet and momentum transfer takes place between it and the surrounding liquid medium. The entrainment of liquid and the resulting deceleration of the gas-liquid dispersion causes the jet to expand forming a characteristic jet cone. The large velocity and density differences between the jet and the liquid result in a high degree of instability and the jet envelope fluctuates rapidly.The characteristic jet cone can be observed by means of time exposure photographs such as those shown in Fig. 1 for an air jet introduced vertically upwards in a water bath. High-speed photography has showns that the gas-liquid dispersion within the cone consists of small bubbles the size of which depends mainly on the jet orifice diameter and Reynolds number. In the laminar region of flow, the following correlation was obtained by Leibson: The results of Liebson et a1.&apos; are plotted in Fig. 2. It can be seen that the region 2000 < NReo c 10,000 is not well-defined experimentally. In the entrance to the fully turbulent region of flow (NR,, = 10,000), the mean bubble diameter decreased to about 0.4 cm and varied only slightly from there on according to the correlation:

Jan 1, 1968

PRESIDENT L. D. RICKETTS,1 NEW YORK, N. Y. PAST PRESIDENTS BENJAMIN B. THAYER,1 NEW YORK, N, Y. WILLIAM L. SAUNDERS,2 NEW YORK, N. Y. FIRST VICE-PRESIDENT SIDNEY J. JENNINGS,1 NEW YORK, N. Y. TREASURER GEORGE C. STONE,1 NEW YORK, N. Y. SECRETARY EMERITUS ROSSITER W.. RAYMOND NEW YORK, N. Y SECRETARY BRADLEY STOUGHTON NEW YORK, N. Y.

Jan 6, 1916

For the year ending February, 1918 PRESIDENT PHILIP N. MOORE ST. LOUIS, Mo. PAST PRESIDENTS WILLIAM L. SAUNDERS NEW YORK, N. Y. L. D. RICKETTS NEW YORE, N. Y. FIRST VICE-PRESIDENT SIDNEY J. JENNINGS, NEW YORK, N. Y. TREASURER GEORGE C. STONE, NEW YORK, N. Y. SECRETARY EMERITUS ROSSITER W. RAYMOND, NEW YORK, N. Y. SECRETARY BRADLEY STOUGHTON NEW YORK, N. Y.

Jan 8, 1917

For the year ending February, 1918 PRESIDENT PHILIP N. MOORE, ST. Louis, Mo. PAST PRESIDENTS WILLIAM L. SAUNDERS NEW YORK, N. Y. L. D. RICKETTS, NEW YORK, N. Y. FIRST VICE-PRESIDENT SIDNEY J. JENNINGS, NEW YORK, N. Y. TREASURER GEORGE C. STONE, NEW YORK, N. Y. SECRETARY EMERITUS ROSSITER W. RAYMOND, NEW YORK, N. Y. SECRETARY BRADLEY STOUGHTON ` . . . . NEW YORK, N. Y.

Jan 7, 1917

By F. L. Holderreed

A choosy in what they would smelt. The furnace charge had to be coarse, and it had to be rich. They discarded fines in excess of about 1/10 the total weight. They wanted 10% copper content and fussed about anything with as low as 5%. They concentrated the copper content of the charge as much as they could by prior selection. They roasted off enough sulfur to further enrich the copper content of the succeeding fall of matte (a melt of cuprous and ferrous sulfides or Cu2S.FeS). Then they desulfurized the iron and fluxed it by carefully adding silica (quartz, not silicates) for a slag of lower density than the cuprous sulfide (Cu2S or white metal). After skimming off the slag, they further desulfurized the white metal by blowing the molten bath with compressed air. The result was blister copper. Yesterday Their techniques and furnaces? Some experimented with mechanically rabbled roasters, but their standard roasting practice was burning coarse sulfide ore in 250-ton heaps. These heaps, approximately 24 x 24 x 6 ft, were burned for about 75 days down to 6-10% sulfur. The turnaround time for a given roasting position was 100 days. Assuming the base was a hearth, the calculated rate of treatment was on the order of 0.004 tpd per sq ft.

Jan 1, 1971

By E. J. KENNEDY

FEBRUARY 15-18 will be the outstanding dates of the month for members of the A. I. M. E., for then the 141st Meeting of the Institute is to be held in the Engineering Societies Building, at New York. What with 41 technical sessions, the Annual Business Meeting at 4 o&apos;clock Tuesday afternoon,, two sessions of the Section and Division delegates, minor committee meetings, and the many luncheons and dinners, the Dinner-Smoker, Informal Dance, President&apos;s Reception and the Dinner-Dance, the opportunity will be limited to do- more-than cast sheep&apos;s eyes at New York&apos;s other multitudinous attrac¬tions until the meeting is over. The technical program is diverse but well organized. The sessions are almost equally divided among the four days, with ten on Monday, Tuesday, and Wednesday, and 11 on Thursday. The meeting opens Monday morning with registration. Be sure to attend to this detail. Failure to do so may have its repercussions at the meeting and throughout the year.

Jan 1, 1932

By N. J. Olson, G. W. Toop

A regular solution is characterized by a finite molar heat of mixing and entropy due only to ideal or random mixing. The thermodynamic properties of binary regular solutions which exhibit constant atomic coordination number and constant atom-atom intefac-

Jan 1, 1967

By P. G. Winchell, M. Cohen, J. Woodilla

The kinetics of stabilization have been studied with respect to the isothermal component of the martensitic reaction in ivon-nickel alloys. Although the carbun (or nit-vogen) content may be very low in these alloys, it plays an important vole in the stabilization phenomenon. In fact, if these interstitial elements are removed by moist-hydrogen treatment, no evidence of stabilization is found. In the pvesence of 0.007 wt pct C, the activation energy for the stabilization process is comparable to that -for the diffusion of carbon (or nitrogen) in ferrite) rather than in austenitc. This suggests that the interstitial diffiision controlling the stabilization occurs within the martensitic embryos rather than in the matrix of the parent phase. The kinetics furthev indicate that the interstitial atoms tend to diffuse -from the embryos toward the suvroundings, thereby immobilizing the interface. This appears to be the origin of the stabilizing effect -found in these alloys. PHILIBERT&apos; has shown recently that interstitial elements play an important role in the stabilization of martensitic transformations in iron-base alloys. However, determination of the temperature dependence for this stabilization process has produced values (- 11,000 cal per mol) that cannot be readily identified with the activation energy for diffusion of carbon (or nitrogen) in either ferrite or austenite. In the present work, the isothermal mode of the martensitic reaction was employed to derive the activation energy for stabilization, and this was found to agree fairly well with that for diffusion of carbon (or nitrogen) in ferrite. An iron-nickel alloy with 30.8 wt pct Ni and 0.007 wt pct C was used in these experiments, the specimens being in the form of rods 0.074 in. in diam and 2 1/2 in. long. The specimens were sealed in evacuated vycor tubes and austenitized at 1100°C for 1/2 hr prior to quenching in water. A second series of specimens was decarburized (and denitrogenized) prior to the above austenitizing treatment by annealing in moist hydrogen for 182 hr at 1215°C. In order to achieve a "standard" condition in the austenitic state, all the specimens were transformed to martensite by cooling to - 195°C before the final austenitizing. Both the 0.007 pct C and the decarburized series then had an Mi temperature of about - 30°C. The isothermal martensitic transformation was carried out at a reference temperature of -88"C, and was traced by means of electrical resistance measurements. Each resistance value was normalized by dividing by the resistance of the austenitic specimen at O°C, thus giving a resist- ance ratio R. The rate of decrease of the resistance ratio (-dR/dt) provided a measure of the transformation rate. It was found that a plot of R vs log t at the reference temperature resulted in a slightly curved line which could be closely approximated by two straight lines intersecting at a time of 10 min, as shown in Fig. 1. If G = dR/dlogt is the linear slope of either straight segment, the rate of transformation at any given time is: The ratio of G for 1 less than 10 min to that for t greater than 10 min was 1.19 for the 0.007 pct C series and 1.24 for the decarburized series. These ratios made it possible to compute the transformation rate at any time greater than 10 min, knowing the transformation kinetics prior to 10 min. The stabilization treatment was introduced by up-quenching from the reference temperature, usually after 10 min of isothermal transformation: to one of four stabilizing temperatures between 0" and 22"C. After holding for various times, the specimens were down-quenched to the reference temperature for additional isothermal transformation. In this way, it was possible to compare the transformation rate (- dR/dt), immediately after stabilization with the transformation rate (- dR/dt)U in the unstabilized condition. The degree of stabilization was defined as: Ordinarily, Gs and Gu would be measured after the same time of prim isothermal transformation.

Jan 1, 1960

By G. J. Ballmer

Drilling and blasting 12-in. blastholes started about the middle of 1946 and has worked out so well that about one half of the blasting, formerly done with 9-in. holes, is now done with 12-in. holes. In most of this work the harder benches were chosen for the 12-in. size because these were the areas where the greatest difficulty was encountered in thorough fragmentation. At the start of this experimental work a 42-T Bucyrus- Erie churn drill was available whereas all other blasthole drilling was being done with 29-T rigs. The large drill was first equipped with a standard 9-in. string of tools but it could not drill quite as fast as the 29-T drills. How- ever, when the weight of the string was increased about 700 lb, or to a total weight of about 3500 lb, it was found that the 42-T exceeded the drilling speed of the 29-T by about 25 per cent. When a 12-in. bit was substituted for the 9-in. bit the 42-T rig again dropped behind the drill- ing rate of the 29-T rigs. At this stage of the experiment the 42-T was using a 12-in. bit with detachable points and the total weight of the string of tools was about 3800 lb. It took longer to change the drill points than it did the regulation bit and this accounted for some of the slower drilling rate. When a heavier stem and standard construction 12-in. bits were used it was found that the 42-T could drill a 12-in. hole slightly faster than a 29-T could drill a 9-in. hole even in the hardest rock in the pit.

Jan 1, 1949

For the year ending February, 1918 PRESIDENT PHILIP N. MOORE, ST. LOUIS, Mo. PAST PRESIDENTS WILLIAM L. SAUNDERS, NEW YORK, N. Y. L. D. RICKETTS, NEW YORK, N. Y. FIRST VICE-PRESIDENT SIDNEY J. JENNINGS NEW YORK, N. Y. TREASURER GEORGE C. STONE, NEW YORK, N. Y. SECRETARY EMERITUS ROSSITER W. RAYMOND, NEW YORK, N. Y. SECRETARY BRADLEY STOUGHTON NEW YORK, N. Y.

Jan 2, 1918

For the year ending February, 1918 PRESIDENT PHILIP N. MOORE, ST. Louis, Mo. PAST &apos;PRESIDENTS WILLIAM L. SAUNDERS NEW YORK,. N. Y. L. D. RICKETTS NEW YORK, N. Y. FIRST VICE-PRESIDENT SIDNEY J. JENNINGS NEW YORK, N. Y. TREASURER GEORGE C. STONE, NEW YORK, N. Y. SECRETARY EMERITUS ROSSITER W. RAYMOND, _ NEW YORK, N. Y. SECRETARY BRADLEY STOUGHTON NEW YORK, N. Y.

Jan 11, 1917

By Orville R. Lyons, A. C. Richardson

F. X. Ferney—We are pleased that this paper was presented at this meeting and thank Mr. Richardson and Mr. Lyons for their effort and work in preparing it. We agree with the authors that it was unfortunate that more comprehensive data were not available when the paper was prepared, this being particularly true since we had no knowledge that the paper was being written and could not make available data which were in our process files. Further, it is our opinion that because the data are not sufficiently comprehensive the results which are presented are erratic and will lead to false conclusions. As we see it, there are three Specific reasons why the data which are presented cannot be considered accurate. 1. The preparation plant was not at equilibrium while the samples were being taken. This is indicated by the fact that the percent of solids in the circulating water varied from 3.9 pct to 10.7 pct during the period when the plant was sampled. 2. We do not believe that the samples of Bird feed which were taken were representative and could indicatc the true feed to the filter. Evidence of this is shown in the data where the dewatered product leaving the centrifuge contains more coarse material than the feed to it, that is, material which is +6-mesh in size. 3. We question if the data concerning screen analysis in the fine sizes is accurate and would conclude (from the data) that these tests were made by a dry-screen method. We have found that wet screening is always necessary to obtain a true picture of the quantity of —200-mesh fines which is present. The test work described in the Lyons-Richardson paper was conducted some time ago and the tests were carried on during a period when the preparation plant had not ironed out all of their start-up problems. Since that time most of these problems have been corrected and now this is a smooth running, well-operated prep-

Jan 1, 1951

By Orville R. Lyons, A. C. Richardson

F. X. Ferney—We are pleased that this paper was presented at this meeting and thank Mr. Richardson and Mr. Lyons for their effort and work in preparing it. We agree with the authors that it was unfortunate that more comprehensive data were not available when the paper was prepared, this being particularly true since we had no knowledge that the paper was being written and could not make available data which were in our process files. Further, it is our opinion that because the data are not sufficiently comprehensive the results which are presented are erratic and will lead to false conclusions. As we see it, there are three Specific reasons why the data which are presented cannot be considered accurate. 1. The preparation plant was not at equilibrium while the samples were being taken. This is indicated by the fact that the percent of solids in the circulating water varied from 3.9 pct to 10.7 pct during the period when the plant was sampled. 2. We do not believe that the samples of Bird feed which were taken were representative and could indicatc the true feed to the filter. Evidence of this is shown in the data where the dewatered product leaving the centrifuge contains more coarse material than the feed to it, that is, material which is +6-mesh in size. 3. We question if the data concerning screen analysis in the fine sizes is accurate and would conclude (from the data) that these tests were made by a dry-screen method. We have found that wet screening is always necessary to obtain a true picture of the quantity of —200-mesh fines which is present. The test work described in the Lyons-Richardson paper was conducted some time ago and the tests were carried on during a period when the preparation plant had not ironed out all of their start-up problems. Since that time most of these problems have been corrected and now this is a smooth running, well-operated prep-

Jan 1, 1951

By H. B. Fuqua, B. E. Thompson

The area discussed herein, commonly known as the North Texas district, embraces the following 10 counties: Archer, Baylor, Clay, Cooke, Foard, Hardeman, Knox, Montague, Wichita and Wilbarger. It is underlain by two major structural features. The northernmost portion of the district, including Cooke, Montague, northern Clay, Wichita, Wilbarger, Foard and Hardeman counties, is underlain by the system of buried mountains known as the Red River uplift, which is parallel to and closely related to the Wichita-Amarillo uplift of Oklahoma and the Texas Panhandle. While the presence of a great majority of the numerous oil fields of the area is traceable to this feature, the production in Archer, southwestern Clay and southeastern Baylor counties is due to the influence of what is known as the Cisco Arch (so called because of its influence on Cisco deposition), the axis of which extends in a northwest-southeast direction across Archer County. It has been impossible for the authors to isolate the statistics for production for each of the many small pools of this district, as such statistics are not kept by the operators except for the district as a whole, therefore Tables 1 and 2 are comparatively short. The number of wells

Jan 1, 1935

For the year ending February, 1918 PRESIDENT PHILIP N. MOORE, ST. Louis, Mo. PAST PRESIDENTS WILLIAM L. SAUNDERS ? NEW YORK, .N: Y L. D. RICKETTS NEW YORK, N. Y. FIRST VICE-PRESIDENT SIDNEY J. JENNINGS . . NEW YORK, N. Y. TREASURER GEORGE C: STONE, NEW YORK, N. Y. SECRETARY EMERITUS ROSSITER W. RAYMOND, . . . NEW YORK, N. Y. SECRETARY&apos; BRADLEY STOUGHTON NEW YORK, N. Y.

Jan 6, 1917

By J. W. Spretnak, V. Kandarpa

Stress -induced ordering of carbon atoms is studied in a series of Fe-Mn-C alloys. A prominent peak is found in the vicinity of 280°C at frequencies of the order of 1.0 cps, with an associated activation energy of 37 kcal per mole. The height of the peak is linearly rekzted to the concentration of carbon in solution. The distortion of octahedral holes by manganese atoms appears to be predominant over carbon-carbon pair interactions. RELAXATION by stress-induced ordering of point defects is expected whenever the introduction of these point defects produces distortions which have a lower symmetry than that of the lattice. Under zero stress, the isolated point defects occupy the crystallographic-ally equivalent positions in the lattice, as these represent states of equal energy. However, if the defect sites are asymmetric, application of an uniaxial stress will split the energy states, and a redistribution of the defects among various states will take place. This is the case of the internal friction peak called the Snoek peak,1 resulting from isolated interstitials in bcc metals. The interstitial sites in this case have tetragonal symmetry. In the case of fcc and hcp lattices, such an effect is not expected from isolated point defects because of the symmetrical nature of the interstitial sites. However, internal friction peaks arising from interstitial diffusion have been reported both in hcp2,3 and fcc4-8 lattices. These peaks are often explained on the basis of stress-induced ordering of interstitial solutes, caused by the deviation of interstitial sites from their cubic symmetry through the presence of nearby defects. In the case of fcc lattices, evidence for interactions of both the substitutional-interstitial4,6,13 and interstitial-interstitial types5&apos;798&apos;14 have been presented by various investigators. The purpose of the present investigation was to study the internal friction peak attributed to the diffusion of interstitial carbon atoms in high purity austenitic manganese steels and to account for the peak in the light of the existing models. MATERIALS The Fe-Mn-C alloys used in the present investigation were made in two different ways, designated as Type I and Type 11. Type I alloys were made from high purity Fe-Mn alloys obtained in the form of 0.04- in.-diam wires from Materials Research Corporation, Orangeburg, N.Y. These alloys were carburized to different levels using gas mixtures of H2 and CH4 at 1000°C. Type I1 alloys were made in this laboratory starting with zone refined iron, spectrographically pure manganese, and spectrographically pure carbon. They were melted in an argon arc melting furnace and drawn into 0.04-in.-diam wires. All the wires were annealed at about 900°C for 3 hr prior to the internal friction experiments. After the measurements of internal friction, the phases in the samples were identified by X-ray diffraction and the carbon determined by the combustion method. EXPERIMENTAL PROCEDURE In the present work, a classical Ke-type pendulum was used. The details of the equipment were described previously by D. T. Peters.9 Dry helium at 40 torr was used in all the experiments. The internal friction, measured as the logarithmic decrement of the torsion amplitude of vibration was determined as a function of temperature, from ambient to about 500°C. The background internal friction was assumed to have the form of the exponential of the inverse temperature and was subtracted from the raw data. The height of the peak was measured at the position of the maximum in the plot of the internal friction versus temperature. The activation energies of the peaks were measured by the peak shift method. The internal friction values for an alloy were obtained as a function of temperature at different frequencies of vibration. The position of the peak changes with frequency, the higher the frequency the higher the peak temperature. The activation energy of the process associated with the peak is obtained using the formula

Jan 1, 1970

By Richards R. Vandervoot

T HE creep behavior of many polycrystalline metals at moderate stresses can be described by the empirical relationship: where Em is the minimum creep rate, A is a constant, a is the applied stress, E is the average elastic modulus at the test temperature, and D is the self-diffusion coefficient.&apos; This equation is generally applicable for strain rates of less than around 10-5 per sec and temperatures greater than about one-half the melting point in absolute units. Under these conditions atomic mobility plays an important role in the deformation process, and steady-state creep occurs when a dynamic equilibrium is reached between the generation and recovery of dislocation substructure. Although several theoretical mechanisms have been proposed to explain the creep of polycrystalline solids,2"4 the dislocation climb model2 is in accord with most experimental observations. The majority of creep data used to develop Eq. [1] came from metals with either the fcc or hcp crystal structures. However, on the basis of results for a and 7 iron as well as those for a and a thallium, Sherby concluded that the high-temperature deformation behavior of close-packed metals and bcc metals is probably the same.&apos; The greater creep resistance of fcc and hcp metals and alloys on a relative temperature scale was attributed to lower diffusivities in the close-packed structures. To further compare the creep properties of fcc, hcp, and bcc metals, creep data for all six bcc refractory metals were analyzed according to Eq. [I]. The results are shown in Fig. 1. The sources of information for the quantities used to prepare this figure are listed in Table I, except for high-temperature elastic moduli. The latter data were obtained from Refs. 28 and 29. The dashed lines in the figure represent the range and breadth of data analyzed by Sherby for fcc and hcp metals. In general, the deformation behavior of all of the refractory metals, ex- cept possibly that of tungsten, can be represented by Eq. [1]. This correlation is strong evidence of the similarity that exists between creep of pure close-packed metals and creep of pure bcc metals. At (Em/D) < 108, the results of Flagella and Tarr on tungsten (W-1 in Fig. 1) agree with the five-power stress law, while those of Green (W-5 in Fig. 1) show a seven-power stress dependence. Where (Em/D) > 108, the stress exponents for other data on tungsten were in the range 10 to 15. It is possible that the creep rate dependence on stress in this region is not a power law but exponential (i.e., Em - eßo). However, it was not feasible to differentiate between these two cases because of the steep slope and scatter in the data. Note the inflection point in the curve for the data of Flagella and Tarr (W-1 in Fig. 1). The slope of the line changes from 5 to around 10 at Em/D = 108. The breakdown of the fifty-power stress law at high stresses is not uncommon in other metals, and this phenomenon may result from nonequilibrium conditions in the material such as excess lattice vacancies produced by rapid straining.30 The mechanical strength of a polycrystalline metal is related to its microstructure. Attempts to establish the influence of grain size on the creep rate of metals and alloys have led to a wide variety of results. For example, the following effects have been observed: creep rate decreases as grain size increases;31&apos;32 creep rate decreases as grain size decreases;&apos;,33 creep rate is a minimum at some critical grain size and increases with either an increase or decrease in

Jan 1, 1969

By C. F. Floe, N. J. Grant, A. Joukainen

A CCORDING to Guertler,¹ Smith and Hamilton were the first to study the Cu-Ti alloy system, but because of the presence of large amounts of impurities their data are inconclusive. Hensel and Larsen² in 1930 and Kroll³ in 1931 determined the high copper end of the diagram. In 1939 Laves and Wallbaum,4 in a short summary of compound determinations in titanium binary alloys, mentioned the existence of a face-centered cubic compound, Ti2Cu, with 96 atoms per unit cell, and also a compound, TiCu3, which was said to have a deformed hexagonal close-packed structure in which ordering had been observed. The existence of a compound, TiCu, was also found but the crystal structure was not determined. Craighead, Simmons, and Eastwood determined the effect of copper on the allotropic transformation in titanium. The investigation was limited to alloys containing from 0 to 5 pct Cu, using titanium of fairly high impurity content. Experimental Procedure The methods used for determination of the diagram included metallographic examination and X-ray and thermal analyses. The system was first worked out using the higher purity "Process A" sponge titanium and oxygen-free copper. The high titanium region was next determined more accurately using iodide titanium and vacuum-melted, oxygen-free copper. Preparation of Alloys: The alloys were prepared by arc melting under prepurified helium atmos- pheres in water-cooled copper crucibles. The high purity iodide titanium alloys were prepared by melting three compositions along with a specimen of unalloyed titanium in a single charge. A multiple crucible was used which consisted of a copper plate with four cup-like depressions. The unalloyed titanium was melted first and acted as a getter for any oxygen and nitrogen in the melting chamber. Since these elements harden titanium, the hardness of the standard specimen was an index of the highest probable contamination of the alloy melts. The sponge titanium alloy melts weighed from 100 to 200 g each and the iodide titanium melts from 20 to 25 g. In order to insure greater homogeneity most of the alloys were melted, turned, and remelted twice. The larger buttons made from sponge titanium were sectioned or crushed before remelting. These alloys up to 30 pct Cu were further homogenized by forging at 925°C. They forged readily up to 20 pct Cu but numerous cracks were formed in the alloys containing from 20 to 30 pct. Above 30 pct Cu the sponge titanium alloys were homogenized by heating for 200 hr at 850°C under prepurified helium. Similarly, the iodide-grade titanium alloys containing up to 3 pct Cu were homogenized at 1000°C for 24 hr and all others at 880°C for 200 hr.

Jan 1, 1953

By H. E. Stauss, J. Hino

INTEREST in silicon has arisen again in the past decade as a result of improvements in crystal rectifiers.&apos; Although the preparation of silicon was first reported by Berzelius in 1880, the early product was of relatively low purity, and only the need for rectifiers in World War II led to the production of a 99.9+ pct pure powder. This material in crystalline form was consolidated into massive silicon for use, and the method developed was to melt it with selected added constituents as "doping" agents. Melting techniques, therefore, are of great importance. There are two basic problems in producing silicon ingots free of doping additions; one is the prevention of spitting and the other is prevention of cracking of the ingot during freezing. The most satisfactory arrangement yet developed for producing massive silicon is to melt and freeze in a cylindrical quartz crucible surrounded by a concentric heating element and concentric radiation shields or insulation. For example, use can be made of a tubular heater with a high frequency generator as the source of power and reflecting shields of alundum cylinders. The spitting of silicon is related to gas evolution, and the gas comes from two primary causes—adsorbed gas and the reaction products of silicon and the crucible. Gas is also released from bubbles contained in the quartz crucible walls. Improved removal of adsorbed gas can be achieved by means of controlled melting and freezing. The seriousness of the problem in vacuo is reduced with an electrically operated mechanical movement of the high frequency power coil. The upper portion of the powder charge is melted first and the high frequency coil lowered until the powder is completely molten. During cooling the high frequency coil is raised slowly. These means also reduce the final nonviolent extrusion of large beads of metal through the ingot top during freezing. Better control of spitting and bead extrusion is obtained when melting is done under helium at. atmospheric pressure instead of in vacuo. The problem of reaction between silicon charge and crucible in practice is confined to the reaction between silicon and quartz. This2 apparently is: Si + SiO2 + 2SiO The part that this reaction plays in spitting has not been isolated for separate study. SiO is a volatile vapor at the melting point; of silicon and is released freely during melting in vacuo, but hardly at all in helium at atmospheric pressure. The cracking of ingots is a major difficulty in melting silicon, and its prevention requires special melting techniques or the addition of "toughening" agents such as aluminum or beryllium.&apos; The cracking of the ingots has been explained as being the result of the expansion that occurs upon freezing; although direct observation of freezing ingots reveals visible cracks on the surface only after a red heat has been reached, suggesting that cracking is the result of differential contraction of silicon and quartz. Silicon wets quartz, and the ingot adheres tightly to the crucible. Therefore as ingot and crucible cool, the two either have to pull apart, or at least one must crack. Surprisingly, in spite of the relative thinness of the quartz and the thickness of the ingot, the ingot and the crucible both crack. Microscopic and X-ray4 studies fail to show any plastic flow other than twinning in the ingots. Slow cooling fails to prevent cracking. Another possible solution to cracking is to weaken the crucible. Use of thin-walled crucibles finally led to success with fused quartz crucibles with a wall thickness of 0.25 to 0.50 mm. With such thin-walled fused quartz crucibles consistently uniform success is secured in producing sound ingots 30 mm in diam from the purest available grade of silicon (99.9+) without the use of any type of addition. Melts are made in the size range of 50 to 100 g. Omission of a deliberately added doping agent is not sufficient to insure pure ingots. The reaction of silicon with crucibles and the resultant solution of impurities in the silicon is well-established." In this laboratory, the presence of Al, Be, and Zr has been found spectroscopically in ingots melted in contact with alumina, beryllia, and zircon. The best crucible materials reported in the literature are MgO and SiO2. Use of MgO in this laboratory has resulted in a heavy deposit of magnesium on the furnace walls, showing that a reduction of the magnesia occurred and the resulting magnesium removed from the melt by volatilization. In the case of quartz, the silica is reduced and SiO liberated to deposit on the equipment walls. There probably is real danger that oxygen is dissolved in the ingot when either magnesia or silica is used as the crucible material. Preliminary analyses by Dean Walter in his vacuum unit in this laboratory6 indicate the presence of oxygen in undoped silicon melted in quartz.

Jan 1, 1953

By J. P. Boisseau, C. N. J. Wagner, E. N. Aqua

An analysis ulas made of powder-paltern peaks from cold-rolled polycrystalline copper and from copper powders, compacted into briquets (1 in. diameter) with pressures up to about 106 psi. Powder-pattern peaks from both contact faces were measured with a diffractometer and CuKa radiation. Laltice-parameter measurements indicate the presence of residual stresses in the bulk specimen of the order of a - -10 kg per sq mm after 93 pct reduction in thickness, and give some evidence for the occurrence of deformation stacking faults (probability a - 0.003) in both bulk and powder samples. Fourier analyses of the line profiles were carried out on the (111) - (222) and (200) - (400) Pairs of reflections. The particle sizes decrease rapidly with increasing deformation and reach asymptotic values of De (111) = 550A and D, (200) = 350A at about 25 pct reduction in thickness or 80,000 psi pressure for compaction. The anisotropy of the particle sizes indicates the presence of microtwins and stacking faults on (111) planes. The rms strains increase also with deformation and reach limiting values of 2 x 10-3 in the [100] direction and 1 x 10-3 in the [Ill] direction at a distance L = 100A normal to the reflecting planes. THE diffraction of X-rays in cold-worked, polycrystalline, fcc metals and alloys yields Debye-Scherrer patterns in which the individual (hkl) lines may show a broadening, a shift, and an asymmetric shape.&apos; These effects can be explained by the fragmentation of the small, coherently diffracting domains, the presence of residual elastic strains in the lattice, and the formation of stacking faults. X-ray studies of stacking faults in fcc metals and alloys have been methodically performed during the last few years, but so far most of the investigators dealt with cold-worked powder specimens obtained by filing.2-8,10-19 In such specimens, the crystals are randomly oriented and the average elastic strains are assumed to be zero, so that the observed peak shifts are due to stacking faults only. The agreement between X-ray diffraction theory1,20 and experiment is generally good. On the contrary, cold-worked, polycrystalline bulk specimens (after wire drawing, rolling, plastic deformation by tension or compression, etc.) contain residual elastic strains, which may not average to zero in the surface of the specimen and show very strong preferred orientation of certain lattice planes (texture) parallel to the specimen surface. Nonzero elastic strains also produce peak shifts, the magnitudes of which depend upon the crystallographic orientation of the reflecting lattice planes in elastically anisotropic materials as well as on the type of plastic deformation and which have to be taken into account when measuring stacking-fault probabilities in deformed bulk specimens.21-23 The purpose of the present investigations was to perform a detailed X-ray analysis on a bulk specimen of a fcc metal deformed by rolling at room temperature and on powder of the same material deformed by compaction, and to compare these results with those previously obtained on cold-worked filings.18 Pure copper was chosen for this study since it is known to produce only a small quantity of stacking faults by filing at room temperature.3,16,17,19 The residual elastic strain in the surface of the bulk copper should be the predominant factor determining

Jan 1, 1965