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By G. H. Kesler, J. E. Oberele, C. E. Dryden, J. H. Oxley

Heat-transfer rates were measured in a model of a multifilament vapor-deposition bulb fo the preparation of high-purzty metals. Local transfer coefficients for heat transfer frow the filaments to the circuates process stream were determined as a functiol of gas flow rates and bulb, inlet, and filament, geowzetvies. These results a-e then convertted to n mass-t7,ansfer basis to provide a method of correlating vapor-deposition rates and to predict the performance of commercial urzits. The firm1 cor?,elating equation for mass transfer was found to be- wheve k, is the mass-transfer coefficient; D, is bze gas difficsivity : P is the system pressure; R is the gas constant; T is the gas temperature; Df, DB, and Di ave tlze diameters of the filament, bulb, and inlet, respectively; k is the gas conductivity; C, is the specific heat of the gas, M is the wzolecular zleight of the gas; Npr . N,,, NRe a7'e the Prandtl, Schmidt, and Reynolds numbem of the system, respectively; LB is the height of the bulb; and SB and Sf are the total suyiace area of the bulb and filaments, respectively. ONE of the more conventional methods of preparing very high-purity metals is the vapor deposition of the metal upon heated filaments. The reactions which can be employed in such a process generally fall into two classes: 1) Pyrolysis of a volatile metal compound. Generally because of their instabilities, metal iodides are used; however, other metal halides and hydrides have been employed. These processes are frequently carried out under vacuum conditions, and the filaments are maintained at high temperatures. 2) Hydrogen reduction of a volatile metal compound. A metal chloride is normally the preferred feed for these processes, but other halides are sometimes used under special conditions. These hydro- gen-reduction processes are usually operated at atmospheric pressure. Many of the current processes for the production of semiconductor materials are actually vapor-deposition processes. However, the vapor-deposition process itself is relatively old, and almost all metals can be prepared in a state of very high purity by the use of vapor-deposition techniques. Loonam has recently given an excellent review of the iodide process for metal deposition,' and Owen has started some detailed studies with a carbonyl system.' A more general treatment of all vapor-deposition processes has been outlined by Powell, Campbell, and Gonser.3 Despite the fact that vapor-deposition techniques have been employed since 1890, there is a surprising lack of fundamental information regarding the transport characteristics of even the simplest deposition system, the heated filament. The purpose of the investigation described in this paper was to extend some of the earlier data obtained at Battelle to predict deposition rates and the uniformity of deposition in large-diameter, multifilament deposition bulbs under forced convection conditions.4'5 A number of other investigators have already presented a simplified treatment of the deposition process under non-flow conditions, i.e., pure diffusion.6"9 To obtain information on the transport characteristics of a deposition bulb, a model of a typical plant deposition unit was constructed, and local heat-transfer coefficients from the filaments to a circulating air stream were determined under various conditions of air-flow rates and bulb, inlet, and filament geometries. These results were then converted to a mass-transfer basis, and consequently provided a method to correlate experimental vapor-deposition rates and to design commercial deposition units. EXPERIMENTAL WORK Description of Model. The apparatus which was used in this work was a scaled model of one type of deposition bulb. It was constructed of Lucite and was easily altered to give several combinations of diameter of bulb liner, inlet size and location, number of filaments, and outlet geometry. The model is shown in Figs. 1 and 2. The bulb shell was made octagonal for convenience in construction and observation, and the bulb liners were cylindrical. Air, introduced through one of several different jet inlets, was used as the test fluid in these model studies. Filaments for deposition of metal were simulated by metal rods 1/4-in. in diam. Two of the rods could be heated by passing electrical current through them ¦ while the remaining rods could not be heated. This procedure minimized the amount of heat which was

Jan 1, 1962

By John Griffen

THEORY HYDRAULIC classification as explained by Rittinger and others was largely restricted to conditions wherein the free-falling velocities of the particles were conceived as governing the separations effected (see chapter 9). The laws governing classification under free-falling conditions have been summarized by Chapman and Mott as fo1lows:l Nomenclature r represents, in a particle of irregular shape, the round-hole screen through which the particle would pass, or some other linear dimension of the particle equivalent to d, the diameter of a sphere. s, the specific gravity of the particle. 1, the specific gravity of the water used as a medium. K, a constant. W, the velocity of the water. In an Upward Current of water 1. A particle will move upward if [V > K dr(s - 1)] and, by suit- ably regulating the speed of the water current, the larger and heavier particles may be made to fall downward against the current, leaving the smaller, lighter particles in suspension in the current. 2. Particles such that [- = -] cannot be separated in an upward- current classifier with any one velocity of current. Coal particles having a specific gravity of 1.35 cannot be separated from refuse particles of [2.5 - 1 2.5 sp. gr.] unless the ratio of diameters is less than [ 4.3 to 1, 1.35 – 1] and the raw coal must be screened to size limits within this ratio if they are to be separated. Cone-shaped vessels or vessels of other shapes that allow the use of different velocities of current at different points in the flow are used to modify this limitation.

Jan 1, 1943

By J. B. Umpleby

PRoduction engineering in 1927 may be characterized by a great. clarification of fundamental conceptions, and many improvements in technique. During the year the profession has received tnarked recogni-tion by the industry and to an extent never before attained has become an integral part of it. History Petroleum production engineering is a new profession. Prior to 1925, when this Institute undertook the work, no forum existed for the open discussion of its technical problems. There was no attempt at a handbook of the subject prior to "Petroleum Production Methods by J. R. Suman, in 1921, and no textbook prior to Petroleum Production Engineering" by L. C. Uren, in 1924. As late as 1926, only six schools and universities offered special courses in petroleum production engineering. Prior to about 1923, engineers engaged by oil companies were used almost exclusively for construction and location work. Two of the leading production engineers in the Mid-Continent field, although with their respective companies more than twelve years, were not definitely assigned to production work until 1924. Both men now head large departments giving almost their entire time to production problems. Because of the newness of the profession, the leading production engineers of today have had their fundamental training in mining, civil, mechanical and electrical courses. Not unlikely this diversified training is in considerable part responsible for the amazing growth of the profession. I believe, however, that recognition is due principally to economic pressure within the industry which has directed attention more and more sharply on costs and efficiency. After all, the justification for the growth and continued development, of the profession is to recover more oil from a given unit of sand at less cost per barrel. In this new profession, it seems to me that greatest progress will result from focusing thought and effort on this single objective, and if I might offer one suggestion to the com-

Jan 1, 1928

By CARLE R. HAYWARDC

BEFORE discussing this subject it is necessary to define somewhat the meaning of the tern metallurgical.. When I was a student at M. I. T. ore-dressing was not thought of as metallurgy in any sense of the word, but it was considered as more closely allied to mining, enabling the miner to market an otherwise unmarketable product, or at least to market it to better advantage. Progress in ore-dressing has gradually allied it more closely with smelting, for at present the raw material received by the smelter is predominantly concentrates and smelting practice has been profoundly affected by the products of the concentrating mill. It is not surprising therefore that in many schools ore-dressing is frankly considered as metallurgy and although there may be some dissenting opinions it will be considered as such in this discussion. Twenty-five years ago at M. I. T. metallography was taught in a few optional lectures. This subject has developed rapidly and been expanded into the new and increasingly important field of physical metallurgy. To many metallurgists the -term metallurgy means only physical metallurgy. They know little or nothing about smelting and leaching and even less about ore-dressing. Having then broadened the scope of the term metal¬lurgy to cover ore-dressing, smelting, leaching and phys-

Jan 1, 1930

By Edward H. Robie, E. J. Jr. Kennedy

his volume records the "clay symposium" that featured the geology side of the Annual Meeting of the Institute at St. Louis, February 19-22, 1951. The symposium consisted of four sessions held under the joint sponsorship of the Geology Subdivision and the Industrial Minerals Division AIME and the Society of Economic Geologists. Its main purpose was to define or outline certain problems of clay and laterite genesis, and the papers herein, which were presented at the first three sessions, deal for the most part with individual deposits or special problems. The fourth session was a seminar concerned almost wholly with a discussion of "problems." The discussion follows the papers in the volume. The clay symposium was not the work of an appointed committee. It was thought up and inspired by John J. Collins, who so ably supervised and co- ordinated the mining, geology, and geophysics program for the 1950 annual meeting of the Institute. After requesting Dr. A. F. Frederickson to get material together on clay and laterites for the St. Louis meeting, Mr. Collins visited Dr. Frederickson and discussed this project with him in greater detail. By that time their interest and enthusiasm had spread to others in the field. The Geology Subdivision, the Industrial Minerals Division, and the Society of Economic Geologists by common consent turned over the organization of the program to Dr. Frederickson. Mr. Collins continued in active touch with Dr. Frederickson and gave him every assistance. Dr. E. C. Harder and Dr. W. D. Keller read all the material comprising the symposium, and their comment was made available to Dr. Frederickson, who did much to put papers and discussion in final shape for publication. To the Karl Eilers Memorial Fund--one of the Funds that enables the Institute to publish books of this kind, to the authors of the various papers, to the contributors to the discussion, and to Messrs. Collins and Frederickson the Institute and readers of this book are indebted.

Jan 1, 1952

By AIME

PROBABLY no greater world traveler has ever been Chairman of one of the Institute's Divisions than Henry Frederick Hebley. To begin with, he was born almost as far away as possible-in Christchurch, New Zealand, Dec. 15, 1893. There he grew up, studying mechanical engineering at the local Seddon Memorial Technical College. Then he went over to Sydney, Australia, for a bit of work before sailing for the U.S.A. in 1915. After a few months as draftsman in a San Francisco office he moved over to Clarkdale, Ariz., in the engineering department of the United Verde copper smelter, which had just gone into operation. But the war was on, and Henry thought he belonged in France with the Canadian Engineers, the United States still remaining aloof from the conflict, and that was the last the copper industry saw of him. After almost two years in France he was wounded, convalesced in England and Canada, and then went back to his native New Zealand to design concrete factory buildings. But soon the United States called again, and this time he landed in Salt Lake City with the Oregon Short Line R.R. Co. Then to Chicago in 1920. where he really got into the coal industry for good, working for the Allen K Garcia Co. on the design and operation of coal mines, beneficiation plants, and combustion equipment; and joining the Institute.

Jan 1, 1946

By R. Ward Grosz

Reasonable and timely solutions to the complicated mathematical calculations involved in the mine planning, economic evaluation and slope stability studies related to the Ruth Mine would not have been feasible without the modern digital computers. The Ruth Mine was a prosperous underground copper operation in east central Nevada from 1915 to 1948, when rising mining costs finally exceeded the value of the ore. A substantial reserve of porphyry copper remained in the ground, but until recently all economic evaluations indicated that it was at best a marginal operation and a relatively poor risk of capital. There has been a steady progress in improving all aspects of surface mining since the first steam shovel started stripping overburden; however, developments in just two rather specialized areas proved to be critical in changing the Ruth Mine from a reserve of mineralized rock to an economically attractive orebody. One involved the progress made in recent years in the science of slope stability. Applying the latest techniques in this field to mine planning resulted in reducing the stripping ratio from 6.0:l to 4. 2:l. The other major factor was the efficiency and cost performance of large capacity haulage trucks which made it feasible to go down over 1100 ft. in an open pit and recover ore with a high stripping ratio economically.

Jan 1, 1969

By Henry G. Granger

DURING upwards of three thonsand miles of canoc-travel in South America, including several mishaps, the writer has unfortunately lost his book of notes taken during the year 1894 in Dutch Guyana, or Surinam. But a year spent in a foreign country, visiting its principal mining properties, is necessarily productive of indelible memories and impressions, and some of these may be of interest to the Institute. The Guyanas include British, or Demerara, Dutch, or Surinam, French, or Cayenne, and the Disputed Territory, or that portion of Brazil on the northeast coast of South America. After passing the picturesque mountainous coasts of Colombia and Venezuela, one reaches a low, flat mud-bank which extends far out into the sea, so that from the steamer, over a couple of leagues of turbid, shallow water, one call just see the dismal outline of the pestilential "bush" that fronts the Caribbean sea, clear around to the mouth of the Amazon. Here, iii the order mentioned above, are the Guyanas. So much has been said about this out-of-the-way section during the late excitement over the Venezuela boundary question, that the historical part of the subject may be advantageously condensed. Gold-mining in the Guyanas is altogether placer-mining, and is of the same general nature throughout; hence by describing the methods in use in Surinam and the results there achieved, ail idea will be given of the work throughout the field. The product of this section is about three to four millions of dollars annually, mostly from Demerara, not because of superior richness of its placers, but as a result of its very much larger population, which exceeds twice the aggregate census returns of both Surinam and Cayenne. Mining ill all this section is of comparatively recent date, and is indirectly due to the decline of the sugar-industry. After the introduction of beet-sugar scores

Jan 1, 1897

By J. B. Clark, A. S. Yue

PfANN1 has shown that when a cylinder of molten binary alloy freezes directionally, the solute distribution can be described analytically by cg=k(l-g)k-1 [1] in which Cg is the solute concentration in the solid at the point where a fraction g of the original liquid has frozen and Co is the initial solute concentration. The term k is the effective distribution coefficient of the solute and is defined as the ratio Cx/CL where Cl is the solute concentration in the main body of the liquid. Both the slope and the intercept at -log (1 - g) = 0 of a logarithmic plot of Eq. [I.] provide a measure of k. Under conditions of freezing where diffusion in the solid is negligible and the solute concentration in the liquid is uniform, the effective distribution coefficient k, derived as above, is equal to the equilibrium distribution coefficient taken from the phase diagram. However, under ordinary freezing conditions, even though solid-state diffusion is negligible, the solute rejected from the freezing solid does not have sufficient time to diffuse uniformly throughout the main body of the liquid. A concentration gradient is formed in a boundary layer in front of the advancing solid-liquid interface as pointed out by Rutter and Chalmers.' Thus, under these conditions, the concentration of the freezing liquid in the boundary layer is higher than that predicted from the equilibrium phase diagram and consequently the effective distribution coefficient k, obtained from directional freezing experiments, is larger than the equilibrium distribution coefficient. The symbol k will designate the effective distribution coefficient in the discussion which follows. In this paper, the determination of the effective distribution coefficient is demonstrated for several dilute binary alloys and a polynary magnesium alloy. The effect of freezing rate on the value of the derived k is presented in detail. An example for the calculation of the solidus in a dilute binary solution using the experimentally determined effective distribution coefficient is given. MATERIALS STUDIED Binary magnesium alloys of copper, nickel, and zinc containing approximately 0.10 wt pct solute and a polynary alloy containing approximately 0.10 wt pct each of several elements were selected for study. The spectrographic analyses of these alloys are given in Table I. The analyses are believed accurate to within +5 pct of the stated value. EXPERIMENTAL PROCEDURE Extruded rods of the alloys, 3/8 in. in diam and 11 in. long were used for directional freezing studies. The alloy rods were melted horizontally in a high-purity graphite boat by a Nichrome-wound tube furnace which moved parallel to the length of the rod. The boat was supported inside a Vycor tube suitably connected to provide a protective atmosphere of dry SO2. For an experimental run, the following procedure was used. The alloy rod was cleaned in dilute HNO, and dried. The graphite boat containing the alloy rod was placed within the Vycor tube and the tube connected to the gas train' The 'ystem was purged for 20 min with dry argon and then a flow of dried SO, was maintained for the duration of the run. The movable furnace was positioned and either all or a desired portion of the alloy rod was melted. After attainment of steady-state temperature gradients the molten bar was solidified from one end to the other at a controlled rate by pulling the furnace along the length of the bar at the desired speed. At the conclusion of the run, the directionally frozen alloy rod was analyzed spectrographically at 1 1/4-in. intervals.

Jan 1, 1961

The meeting of the Institute of Metals Division was held in Phila-delphia from Sept. 30 to Oct. 2, inclusive. On Monday evening preceding the meeting, a dinner was held at the Ritz-Carlton Hotel at which many of the former officers of the Division and of the present officers and execu-tive committee were present. The subject of a membership committee was discussed and a motion to appoint such a committee with powers to go over the membership list for the selection of divisional members and to institute plans for additional members was passed. Mr. H. E. Howe and Dr. Johnston of the National Research Council attended the meeting and presented their plans for an Alloys Research Association. Many opinions were voiced as to the practicability of such a scheme and Mr. Howe expressed himself in appreciation of the cooperative thought and efforts given him. On Tuesday morning the Institute of Metals Division joined sessions with the American Foundrymen's Association and listened to the opening addresses. In the afternoon a boat ride was taken on the Delaware River, visiting the plants of the Cramp Ship and Engine Building Co. and the shipyard of the Emergency Fleet Corpn. at Hog Island. The launching of the boat christened "Afoundria" at 5 p.m. was witnessed by members of the party. The opening technical session was held on Tuesday evening at the Ritz-Carlton Hotel at 8 o'clock. The next session was held at the Ritz-Carlton at 10 o'clock on Wednesday morning and the final session at the same time and place on Thursday morning. The sessions were well attended and the discussion was good. The highly technical nature of some of the papers on the program was of special note. Taken as a whole the meeting was one of the most successful ever held. The follow-ing papers were presented:

Jan 11, 1919

By J. Chipman, M. N. Dastur

The importance of dissolved oxygen as a principal reagent in the refining of liquid steel and the necessity for its removal in the finishing of many grades have stimulated numerous studies of its chemical behavior in the steel bath. From the thermodynaniic viewpoint the essential data are those which determine the free energy of oxygen in solution as a function of temperature and composition of the molten metal. A number of experimental studies have been reported in recent years from which the free energy of oxygen in iron-oxygen melts can be obtained with a fair degree of accuracy for temperatures not too far from the melting point. Certain discrepancies remain, however, which imply considerable uncertainty at higher temperatures; also several sources of error were recognized in the earlier studies. It has been the object of the experimental work reported in this paper to reexamine these sources of uncertainty and to redetermine the equilibrium condition in the reaction of hydrogen with oxygen dissolved in liquid iron. The reaction and its equilibrium constant are: H2 (g) + Q = H2O (g); K1 _ PH2O / [1] Ph2 X % O Here the underlined symbol Q designates oxygen dissolved in liquid iron. The activity of this dissolved oxygen is known to be directly proportional to its concentrationl,2 and is taken as equal to its weight percent. The closely related reaction of dissolved oxygen with carbon monoxide has also been investigated:3,4,5 co (g) +O = CO?(g); K _ Pco2___ [2] K2= pco X % O [2] The two reactions are related through the wat,er-gas equilibriuni: H2 (g) + CO2 (g) = CO (g) + H2O (g); K2 = PCO X PH2O [3] PH2 X PCO2 and with the aid of the accurately known equilibrium constant of this reaction, it has been shown5 that the experimental data on reactions [1] and 121 are in fairly good, though not exact, agreement. Experimental Method Great care was taken to avoid the principal sources of error of previous studies, namely, gaseous thermal diffusion and temperature measurement. The apparatus was designed to provide controlled preheating of the inlet gases and to permit the addition of an inert gas (argon) in controlled amounts, two measures found to be essential for elimination of thermal diffusion. A known mixture of water vapor and hydrogen was obtained by saturating purified hydrogen with water vapor at controlled temperature. This mixture, with the addition of purified argon, was passed over the surface of a small melt (approximately 70 g) of electrolytic iron in a closed induction furnace. After sufficient time at constant temperature for attainment of equilibrium the melt was cooled and analyzed for oxygen. GAS SYSTEM A schematic diagram of the apparatus is shown in Fig 1. Commercial hydrogen is led through the safety trap T and the flowmeter F. The catalytic chamber C, held at 450°C, was used to convert any oxygen into water-vapor. A by-pass B with stopcocks was provided so that the hydrogen could be introduced directly from the tank to the furnace when desired. From the catalytic chamber the gas passed through a water bath W, kept at the desired temperature by an auxiliary heating unit, so that the gas was burdened with approximately the proper amount of water vapor before it was introdvced into the saturator S. All connections beyond the catalytic chamber were of all-glass construction. Those connections beyond the water bath were heated to above 80°C to prevent the condensation of water vapor. After the saturator, purified argon was led into the steam-hydrogen line at J, and finally the ternary mixture was introduced into the furnace. THE SATURATOR The saturator unit comprised three glass chambers, as shown in Fig 1, the first two chambers packed with glass beads and partially filed with water and the third empty. Each tower had a glass tube with a stopper attached for the purpose of adjusting the amount of water in it. The unit was immersed in a large oil bath, which was automatically controlled with the help of a thermostat relay to constant temperature, ± 0.05ºC, using thermometers which had been calibrated against a standard platinum resistance thermometer. The performance of the saturator over the range of experimental conditions was checked by weighing the water absorbed from a measured volume of hydrogen; the observed ratio was always within 0.5 pct of theoretical.

Jan 1, 1950

THE translators wish to record their appreciation of the help given by many individuals with whom they have discussed various details of the work. They are particularly indebted to Mrs. Anne Noble McKeachie, who initiated their collaboration; to Miss Cora Adamson, who spent many hours in making an accurate copy of a much-mutilated &st draft of the translation; and to the Yale University Library which gave access to its excellent collection of books on all aspects of the history of the sciences. The reader will share with the translators their obvious indebtedness to Mr. Carl P. Rollins, Mr. James W. Boyden, and the staff of the Printing-Office of the Yale University Press. The publication of this translation by the American Institute of Mining and Metallurgical Engineers has been made possible by a grant from the Seeley W. Mudd Memorial Fund, administered by a committee composed of Harvey S. Mudd, H. DeWitt Smith, and George Otis Smith. The translators are gratified that their work has been judged to fall within the scope of this Fund, which was established for the advancement of the sciences of mining and metallurgy by the encouragement of research and the dissemination of knowledge, and especially for the furtherance of such activities as might benefit the younger members of the profession. While Biringuccio's book would scarcely serve as a dependable text for the young mining student or metallurgist, it can give him a sense of his membership in a long-standing and honorable profession and enable him better to see his own work in true perspective. It is hoped that this English edition of a sixteenth-century Italian work will be read by the practicing metallurgist as well as by those who have already found pleasure in exploring the past of their profession. A man always feels more at home in a foreign country with men of his own craft than in his birthplace with those of different interests: As in space, so in time, and the modem metallurgist who may be unmoved by the literary and artistic Renaissance will quickly appreciate the spirit of that exciting period as he talks shop with Biringuccio on a visit to mine, smelter, forge, and foundry; as he sees in different forms the very furnaces and machines whose operation and response he knows so well; and as he discusses with this engineer of four centuries ago such topics as the best kinds of fuel or refractory for a given operation, and the importance of adequate supplies of power and material.

Jan 1, 1942

By R. B. Russell

SINCE Cahn's¹ paper on plastic deformation in orthorhombic (a) uranium an increasing amount of work is to be expected on orientation of single crystals and preferred orientation in this metal. It would seem desirable to have a table of angles between crystallographic planes (hkl) and (HKL). Table I shows these angles as distances from (loo), (0l0), and (00l), and in Fig. 1 as a standard (001) stereographic projection. Only the locations of poles whose diffracting planes produce Cu Ka reflections up to 0 = 70.5" (i.e. (154) ) are given." The relative reflection of these planes are represented by circle diameters. It is hoped that the projection may also be used in making inverse pole figures, originally suggested by Harris.' Values of 4 were calculated from the expression hH kK 1L cos = hH/a²+kK/b²-lL/c² where the lattice parameters a, b, c, and the spac-ings d were taken from the work of Jacob and Warren." (They report a = 2.852 kX (2.8578 A), b = 5.865 kX (5.8768 A), c = 4.945 kX (4.9550 A).) The parameters reported by them may be subject to revision,4,5 accordingly the interplanar angles are listed to only the nearest tenth of a degree. References ¹R. W. Cahn: Acta Metallurgica (1953) 1, p. 49. ¹G. B. Harris: Philosophical Magazine (1952) 43, p. 113. 3C. W. Jacob and B. E. Warren: Journal ACS (1937) 59, p. 2588. 4J. S. Lukesh: Acta Crystallographica (1949) 2, p. 420. ³ J. Thewlis: Nature (1951) 168, p. 198.

Jan 1, 1954

By Donald E. Meyer

High current-low voltage EB-gun evaporation in an oil-free ultra-high vacuum system was found to be necessary, though not sufficient, for stability (300°C, 106 v per on) of aluminium gate MOSFET's and MOS capacitors not stabilized by a phosphorous glaze. five characteristics of the equipment used: 1) Vacuum purification of the aluminum charge, 2) Ionization of the evaporant by the electron beam, 3) X-ray formation, 4) Residual gases during evaporation, and 5) Metal film structure were studied as Possibly significant in MOS fabrication. EVAPORATION of contact metals common to the semiconductor industry historically has been accomplished with oil diffusion pump systems and various resistance heated evaporant sources as dictated by the type of metal evaporated. To meet a need for greater reliability of semiconductor devices, other metallization methods were developed. A good example would be application of the moly-gold contact system to integrated circuits with deposition by RF or triode sputtering.' More recently, fabrication of stable metal-oxide-silicon devices and circuits has put new demands on metallization. The purity of the thin metal films composing MOS structures is critical, particularly at the metal-oxide interface, and ultra-high vacuum metallization using sputter-ion pumping and electron beam gun (EB-gun) evaporation are well suited for the task. At this laboratory aluminum has been the most common contact-gate metal for both MOS capacitors and MOSFET's. In the earliest work with MOS capacitors, aluminum was evaporated from wetted tungsten filaments using both diffusion pump and ion pump vacuum systems. In spite of clean oxide techniques these capacitors were unstable under bias-tempera-ture stressing. Only after a switch to EB evaporation of aluminum were stable capacitors produced. Using the same techniques it was possible to make MOSFET's with equivalent stability. Stability data for a discrete MOSFET is shown in Fig. 1. This is a "clean" oxide gate (no phosphorus stabilization or no etch back of a thicker gate) having a thickness of lOOO? thermally grown on the (111) plane. Gate length after diffusion was 0.24 mils, and the devices were hermetically sealed. Stressing conditions were 300°C and 106 v per cm applied alternately as a positive and negative field for 10 min, 50 min, and 4 hr for a total stress time of 10 hr. An initial shift in turn-on voltage of 0.1 v was detected for 10 min of positive bias. All evidence at this laboratory indicated that while EB-gun evaporation of ultra-high purity aluminum was not sufficient for 300°C stability, it did seem to be necessary. There may well then be something inherent in the EB-gun deposition used which enhanced stability, and probably no single factor existed but rather a series of factors. It is the purpose of this paper to report on some of the investigations carried out to learn more about EB-gun evaporation in ultra-high vacuum systems. EXPERIMENTAL DESCRIPTION The EB-gun was self accelerated, had a maximum power rating of 10 kw, and used a water-cooled copper crucible able to hold a 20-g aluminum charge. The electron beam was bent 180 deg and focused by an electromagnet which also provided movement of the beam across the crucible. Normal power conditions in this work were 9 kv and 300 to 600 mamp. The gun can be described as high-cur rent/low-voltage and was quite different in its mechanism of operation from EB-guns with much higher acceleration potentials. An oil-free vacuum system capable of 5 x 10- l0torr, a quartz crystal rate and thickness monitor and a quadruple mass spectrometer completed the evaporation system, Fig. 2. A typical evaporation cycle consisted of a 3 to 4 hr pumpdown to the upper l0-9 range and evaporation at l0? per sec with the pressure in the bell jar not rising above 1 x 10"7 torr. Thickness control was 5 pct or less and could be automatically monitored and controlled. Five phenomena associated with the EB evaporation and considered as possible contributors to Ma performance included a purification effect, ionization of evaporating aluminum, X-rays, constitution of vacuum ambient during evaporation, and film structure dependence upon evaporation rate. These phenomena are now discussed. Vacuum Purification. The design of the EB-gun permitted purification of the aluminum charge by vacuum outgassing. Particular features included an efficiently water-cooled copper hearth with a capacity of over 20 g of aluminum and the capability for sweeping the beam across the charge. Such capacity meant that aluminum had to be added only after about every fifth evaporation. A new charge was not required each evaporation as is necessary with filament evaporation. An oxide "scum" which appeared on the charge could be completely cleared from the top hemisphere of the charge by sweeping with the beam prior to opening the shutter. An indication of the purifying effect was obtained by a series of analytical measurements on incoming aluminum, after melting but with little vacuum out-gassing, after 30 min outgassing, and the evaporated film itself. Either a solids (spark source) mass spectrometer or an emission spectrometer were used for analyzing the aluminum charge. Analysis of the evapo-

Jan 1, 1970

By T. W. Atkins

ATHOUGH the magnesium industry in this country is about thirty years old, not until American industry began to amaze the rest of the world and confound our enemies with the extent and variety of our war production did the industry begin to come into its own. At the outset of the war, only three companies were producing and fabricating magnesium in this country. Today, about sixty companies are producing, casting, forging, extruding, rolling, and stamping this lightweight champion of metals. Experience in alloying, processing. and fabricating the metal gained during the war years is now being translated into hundreds of civilian peacetime applications. In no sense should magnesium be considered as a substitute for other metals. It has come into popular favor because If many unique properties in addition to is being the lightest known structural metal. These attributes are toughness, igidity, corrosion-resistance, and the ease with which it can be machined and worked. Magnesium is the third most abundant element in nature. Sea water, magnesite,

Jan 1, 1946

By Charles R. Simcoe

The stress-strain curves in the microyield region for various Fe-C solid solutions shown by Davies and Ku are typical examples of parabolic curves defined by the expression a = kEn 111 These data, when replotted on log-log coordinates, as shown in Fig. 9, exhibit three essentially parallel straight lines. It is apparent that carbon increases the flow stresses, but does not affect the exponent n. In other words, the only factor in Eq. [1] affected by in in carbon content is the constant k. As Eq. [1] is written k is the stress at a strain of 1.0. This is unsatisfactory for examining data in the microyield region. Therefore, the equation can be altered to the form: to permit the use of the authors' microyield stress at a strain of 10-6 as k. Extrapolating the curves in Fig. 9 to a strain of 10-6 gives stress values of 2000, 3200, and 5400 psi for 0.008, 0.014, and 0.02 pct C, respectively. These values do not agree exactly with the authors' measured values, but this will not affect the following discussion. The effect of carbon content on the slopes of the stress-strain curves shown in Fig. 2 of the paper by Davies and Ku can be analyzed by differentiating Eq. [2] with respect to strain. Thus: where n is always less than 1.0. Since n is essen- tially constant as a function of carbon content for the data under discussion, the slopes of the stress-strain curves depend only on k and E. If the slopes are examined at various selected Plastic strains. i.e., 10-6, 10-5, and so forth, it follows from Eq. [3] that the dif-ferent slopes for the different carbon contents depend only on the different values of ke=10-6. Thus, the larger ke=10-6, the steeper the linear stress-strain curve will rise with increasing plastic strain. This

Jan 1, 1969

By F. C. Miller

THE metallurgical fuel of Colorado, Utah, and New Mexico has been a very tardy member in the caravan of western industrial progress. The history of western coke has naturally been closely related to the development of the metallurgy of iron and steel and the precious metals, in the State of Colorado. It was at Leadville, with a population of 300 in 1877, that the Sentinel was published by Richard S. Allen. The Sentinel gave very full accounts of the various mineral discoveries at the new town of Leadville, which found their, way to the more widely circulated journals of the East, and attracted the attention of many people. At the close of 1878, a census showed a total of 5040 persons. The first smelter was established in 1877, at Malta, two miles from Leadville, by A. R. Meyer, but was not successful. It was succeeded by the Harrison Reduction Works, in 1878. The La Plata began with one furnace in June, 1878, and in 1879 had four furnaces in active operation. These furnaces used charcoal for fuel, and, because of hot tops, suffered a tremendous loss in lead and silver. This difficulty was overcome by the erection of 50 single-bank 10-ft. beehive ovens at Crested Butte, Colo., in 1880. The slack coal sent to these ovens was very pure, and yielded a coke carrying as little as 4.5 per cent. ash. Among the pioneers in the Leadville district were Grant, Eddy, James, Billings, Eiler, and Dickson. To these men the West owes the present expansion of its mining industry, and the erection of metallurgical processes for the treatment of precious metals.

Jan 8, 1918

By R. A. Wagstaff

THE method of charging a reverberatory furnace has changed many times since smelting was introduced in this country from the old smelters of Swansea, England. The cause of the latest change at the Garfield plant has been the excessive fineness of the charge due to fine grinding in the concentration of the crude copper ores. The many desirable features of deep-bath smelting as now used at Garfield have been proved. The old method of dropping the charge through holes in the arch (known as center-feed method) causes excessive dusting which makes heavy slag and causes flue-dust losses, also rapid deterioration of the silica brickwork of the furnace through fusion .with the iron oxides from the dust. The purpose of this paper is to describe a gun feeder that was designed to overcome the disadvantages of the older methods of center feeding and still maintain the good features of deep-bath smelting with the hot finer charge. A gun feeder was designed to introduce the finely divided hot calcines under the moving gas stream of the combustion zone and still have them spread in a uniform blanket over the highly heated matte bath. The temperature of the furnace was so great that it was impossible to maintain a stationary feeder, so a movable feeder was designed that could be introduced into the highly heated zone and be withdrawn after the charge had been dropped. It was necessary to protect the nozzle of the gun with a water-cooled coil. Many different types of protected nozzles were tried, such as air jackets, water jackets and heat-resisting steel alloys, but none proved satisfactory.

Jan 1, 1932

By Y. L. Yao

The solubility limit of oxygeu in a titanionn at 850°C has been determined by magnetic measurements as 12.5 + 0.5 pct (29.0—30,9 at. pct). Also in the susceptibility-co~centmtion curve, there is n distinct but not sharp maximum at 19.0 * 0.5 z~t pet (40.5--42.1 at. pct), which indicates the presence of the 6 phase. The magnetic susceptibilities of the alloys of the titanium-oxygen system were determined byEhrlich in 1939.' is alloys were prepared by sintiring mixtures of titanium and its oxide at high temperatures. On the titanium-rich side, despite the fact that the alloy compositions he measured crossed two phase boundaries, the limited results obtained

Jan 1, 1960

September 1 to 6, 1918 COMMITTEE IN CHARGE Spencer Penrose, Chairman. George M. Taylor, Vice-Chairman. A. E. Carlton, Chairman. Finance Committee J. Dawson Hawkins, Secretary DENVER COLORADO SPRINGS CRIPPLE CREEK Finance Finance Thomas B. Crowe T. B. Stearns A. E. Canton , E. P. Arthur, Jr. Richard A. Parker Spencer Penrose N. S. Greensfelder T. B. Burbridge George M. Taylor A. E. Carlton. A. L. Blomfield, Treasurer B. F. Hill Arrangement I F. G. Willis Dave G. Miller Registration Norris E. Eads Frank Bulkley Loren C. Lennox 1V. E. Ryan Geo. E. Collins Horace F. Lunt Fred Jones .1. M. Tippett F. D. Smale Entertainment J. H. Haynes F. H. Bostwick Arrangement and Entertainment L. W. Lennox F. E. Shepard George M. Taylor A. L. Blomfield M. R.. Valentine Howland Bancroft J. D. Hawkins Thomas B. Crowe B. P. Morse A. E. Carlton E. P. Arthur J. G. Perry G. H. Clevenger Etienne A. Ritter Ladies Ladies , PUEBLO Mrs. T. B. Stearns, Mrs. C. M. Taylor, Mrs. C. H. Clevenger J. F. Welborn Chairman. Chairman H. B. Carpenter Mrs. C. Loughridge Mrs. S.-Penrose Mrs. A. E. Carlton L. B. Eames Mrs. H. Bancroft Mrs. J. D. Hawkins Mrs. A. L. Blomfield F. Robinson Mrs. G. Bancroft Mrs. L. C. Lennox Mrs. J. M. Tippett . Mrs. W. D. Leonard Mrs. H. F. Lunt -Mrs. E. C. van Diest Mrs. C. Chase Mrs. E. A. Ritter Mrs. AV. Strieby Mrs. F. H. Bostwick Mrs. L. S. Harner Mrs. C. L. Bailey Mrs. F. Bulkley Miss F. Dickerman Mrs. E. P. Shove Mrs. C. L. Tutt Mrs. F. C. Peck Mrs. F. D. Pastorius

Jan 10, 1918