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Discussion of the paper of DOUGLAS BUNTING, presented at the New York meeting, February, 1915, and printed in Bulletin No. 97, January, 1915, pp. 1 to 21. ARTHUR HOVEY STORRS, Scranton, Pa.-I know something about accidents Nos. 4 and 8. At the Fuller mine there was no disturbance of the surface in connection with either of those accidents, there was no surface settling, nor signs of sand in the mine, and seemingly the water all came from a subterranean basin or water-bearing stratum overlying the Six Foot vein. A similar thing was shown, in an accident not referred to in Mr. Bunting's table, at the Avondale, where we had an inflow of water, as high as 12,000 gal. a minute, for a considerable period. Regarding the second accident (No. 8) at the Fuller mine: after the first inflow of water (No. 4 of the table), the mining was abandoned in the Six Foot vein. A long slope was. driven in an underlying seam, and when this had reached a point about 2,000 ft. southeast of the place where the first inflow of water occurred, and where the bore holes show there was apparently sufficient rock covering for the Six Foot vein, a rock plane was driven up to the upper vein (Six Foot) and one afternoon this exposed the coal. During the following night the inflow of the water occurred. There were absolutely no workings at this point so that no disturbance of the overlying rocks could have occurred. The result of the inflow of water was to fill up the entire lower-vein workings in about two or three clays and caused the abandonment of the mine. After several years, considerable time and money were spent in an effort to hoist the water from the shaft and mine workings, with varying, but in the main rather indifferent, success until, clue to the breaking of one hoisting rope, the engineer pulled the other hoisting tank up through the tower and down on to the engine, making a complete wreck of the whole plant. It was then decided to allow the mine to soak and it is still doing so, other portions of the property being mined from adjoining collieries.

Jan 5, 1915

By William B. Harris, Leonard Greenburg, Gustav Werner

Haulage in tunneling operations generally has been done with electric locomotives. As a rule, on short hauls the source of electricity is a storage battery mounted on the locomotive, which, of course, must be removed and recharged periodically. Where the distance from the recharging point to the tunnel face is very long, and where loads are heavy, trolley-driven locomotives are used. Diesel engines have been used in mining and tunneling operations in Europe for a number of years. The recent reports of studies in Belgium1 and by the Bureau of Mines in this country2-4 have indicated the potentialities of this form of power for haulage, mucking, bulldozing and many other underground operations. The hazards attending the use of Diesel engines in more or less closed spaces have long been known. The exhaust constituents that may create a harmful or objectionable environment are carbon monoxide, oxides of nitrogen and sulphur, carbon dioxide, aldehydes and smoke. Lack of precise information regarding the concentration of these gases and the ventilation requirements to reduce them to safe levels has to some extent suppressed their general acceptance in tunneling and mining work. Not until the work of the Bureau of Mines referred to above, and certain experience gained in the construction of the Delaware Aqueduct, ‡ has there been available the requisite information regarding the conditions under which their use may be permitted. This paper concerns itself with the successful operation of Diesel engines underground in the construction of certain parts of the Delaware Aqueduct, and describes the conditions under which Diesel engines have been found to operate with a minimum production of noxious gases. The test data reported were obtained during the operation of Diesel engines over a period of two years.* Studies by the New York State Department or Labor Exhaustive tests were made by the Division of Industrial Hygiene, of the composition of the exhaust gases given off by a Diesel engine mounted on a test block. These tests showed that certain' quantities of the gases are discharged from the exhaust. On the basis of these figures, preliminary requirements of design and control

Jan 1, 1943

By Gustav Werner, Leonard Greenburg, William B. Harris

Haulage in tunneling operations generally has been done with electric locomotives. As a rule, on short hauls the source of electricity is a storage battery mounted on the locomotive, which, of course, must be removed and recharged periodically. Where the distance from the recharging point to the tunnel face is very long, and where loads are heavy, trolley-driven locomotives are used. Diesel engines have been used in mining and tunneling operations in Europe for a number of years. The recent reports of studies in Belgium1 and by the Bureau of Mines in this country2-4 have indicated the potentialities of this form of power for haulage, mucking, bulldozing and many other underground operations. The hazards attending the use of Diesel engines in more or less closed spaces have long been known. The exhaust constituents that may create a harmful or objectionable environment are carbon monoxide, oxides of nitrogen and sulphur, carbon dioxide, aldehydes and smoke. Lack of precise information regarding the concentration of these gases and the ventilation requirements to reduce them to safe levels has to some extent suppressed their general acceptance in tunneling and mining work. Not until the work of the Bureau of Mines referred to above, and certain experience gained in the construction of the Delaware Aqueduct, ‡ has there been available the requisite information regarding the conditions under which their use may be permitted. This paper concerns itself with the successful operation of Diesel engines underground in the construction of certain parts of the Delaware Aqueduct, and describes the conditions under which Diesel engines have been found to operate with a minimum production of noxious gases. The test data reported were obtained during the operation of Diesel engines over a period of two years.* Studies by the New York State Department or Labor Exhaustive tests were made by the Division of Industrial Hygiene, of the composition of the exhaust gases given off by a Diesel engine mounted on a test block. These tests showed that certain' quantities of the gases are discharged from the exhaust. On the basis of these figures, preliminary requirements of design and control

Jan 1, 1943

Jan 1, 1920

By G. P. Moore

BOLIVIA still remains among the oil countries that have proved oil acreage but no production which is being marketed. No steps have been taken during the past year to provide facilities for transport of Bolivian oil to market nor are any known to be contemplated for 1930. The only active operator to date is the Standard Oil Co. of Bolivia, subsidiary of the Standard Oil Co. of New Jersey. The potential production from completed wells is practically unchanged from the 1928 figure of 6000 bbl. daily. As far as is known, there has been only one completion during the year 1929. This is the Machareti well, which is about 50 km. north of Villa Montes along the road to Charagua. The well is reported at about 250 bbl. daily initial production. The gravity of the oil is not known but is presumed to be about 40" Bé., the average for the region. The Standard Oil Co. of Bolivia has five strings working on various parts of its concession. No new locations have been made definitely. Company Activities There was no change in the situation of American holdings in Bolivia during 1929. The oil rights of an English company, acquired under a special colonization contract with the Bolivian Government, are being negotiated in New York and may mean the entrance of another of the large American oil companies in Bolivia. The Sucre Syndicate sold its holdings to the Standard Oil Co. of Bolivia during the past year. .A local company called the "Aguila Doble" was formed during 1929 to drill a well or wells near the town of Cochabamba on structures mapped by a local geologist. It is reported that the Government is buying about one-fourth of the capital stock of this company for 500,000 Bolivianos (about $180,000). The company has not yet raised sufficieht funds to buy drilling equipment so that no operations have been started. According to the statements published in La Pas, this company has acreage on seven anticlinal structures near Cochabamba. This area lies about 8500 ft. above sea level on the eastern Hank of the Andes Moun-

Jan 1, 1930

By Jei Y. Choi, P. G. Shewmon

The surfrrce-diffusion coefficients (DJ for Aulg8 on (100) and (111) surfaces of copper have been determined between 1050" and 780°C using a new avuzlysis imd experimental procedure. The results are: D, has also been determined fm cua4 at 870°C, and the values found are 4.5 times larger than those measured by the grain boundary grooving technique for the same surface orientations. This difference is felt to result from the approximate nature of the mathematical solution used in the present work. Attempts to measure D, for silver on copper and silver surfaces indicated a means of matter transport different from surface diffision was dominant in moving tracer from the source out over the surface. Cnlculations and experiment both indicate that this is the flow of silver through the vapor phase which completely masks the much smaller flow due to surface diffusion. The previous self-difhsion studies of D, for silver and copper are discussed in terms of our own analysis and found to yield values of D, factors of lo5 or more greater than those found by the grain boundary grooving tech -nique. UNTIL about 5 years ago it was widely believed that the activation energy for surface diffusion, AH, , was less than that for grain boundary diffusion, AHb,, which in turn was less than that for diffusion through the lattice, AHz.' This was concluded from various evidence that D,> Db>Dl, and one tracer study of D, for silver on silver from which AH, was inferred.2 In 1959 Mullins and Shewmon demonstrated that D, could be determined from the kinetics of the growth of grain-boundary grooves.3 Using this procedure, Gjostein measured D, on copper between 800" and 1050°C and found that the activation energy was roughly equal to AHl .4 Subsequent work on copper,5" silver,',' and goldg between the melting temperature T, and 0.87 T, confirmed that AH, as determined using the grain boundary grooving or scratch-relaxation technique was equal to or greater than AHz. During the same period, Drew and Pye again determined AH, for silver on silver using a tracer techniquelo and a mathematical solution similar to that of Nicker son and arker.' Though the values of D, Drew and Pye measured at any given temperature were about 200 times smaller than those reported by Nickerson and Parker, they again found a low activation energy of about 10 kcal, or about one fifth that found at the higher temperatures with the mass transport technique. A distinguishing characteristic of these two previous tracer studies is that they have worked at low temperatures (-1/2 T,) where they felt volume diffusion was negligible and then analyzed these data as if all tracer atoms leaving the source flowed out into and remained in a homogeneous high-diffusivity surface layer of undefined thickness. This is totally different from the model used in the mass-transport studies or the studies of grain boundary diffusion, which assume the high-diffusivity surface layer to be only a few angstroms thick. If this latter model is applied to the earlier tracer studies, it is shown that the tracer has really pe!etrated into the lattice a mean distance of 1000A. Thus the tracer distribution observed after an anneal is thought to be due to the combined effects of surface and volume diffusion. Independent of the relative validity of the two models, it seems evident to us that any comparison of the values of D, as determined in these two ways is meaningless and misleading, since the values of D, and AH, obtained in these two ways would be totally different for the same physical distributions of tracer. Once the fundamental difference in the approaches of the two techniques is established, we are faced with the question of which model better approximates physical reality. Here all the evidence seems to be on the side of the ''thin surface layer" analysis. In fact, the authors of Refs. 2 and 9 do not argue for the "thick-layer model" we have described; they simply invoke it through the equation they use to calculate D, . The primary evidence for the thin-film approach is: a) grain boundary grooves and scratches widen in proportion to tU4 and Mullins' rigorous analysis shows that this is only valid for a surface layer which is quite thin relative to the width of the groove;11 b) all accepted or seriously discussed models of solid-vapor interfaces and high-angle grain boundaries assume that the disturbed region of the interface is at most a few a0 thick. With the above in mind, it was desirable to determine D, using a radioactive tracer and a "thin-

Jan 1, 1964

By W. F. Guenther

The usual hand-operated drilling outfit consists of a 4-in. post-hole auger with 3/4,-in. pipe for drill stem, in 4-ft lengths, with a turning handle fitted to a top pipe T. The auxiliary tools are: a chisel-bit drill made from 3/4 or 7/8-in. tool steel welded to a 4-ft length of 3/4-in, pipe, so that the regular pipe string can be used; also a churn or "mule foot" made from 3-in. pipe, slotted on one side, belled to a 4-in. tempered cutting edge on the bottom, all welded to a 3/4-in. coupling by a yoke. Other tools required are pipe wrenches and cleanout tools made from old auto springs (Fig I). A 4 1/2 or 5-in. collar welded to a plate is often used to protect the mouth of the drill hole. In general the auger is used in the typical clay overburden and brown phosphate matrix, which is relatively soft. The churn or "mule foot1' is used in hard pan, lump phosphate or cherty ground. The drill is used for breaking flint, often found loose in the overburden. The drill with the chisel bit is used for trimming sides of the hole, sounding for lime bottom and breaking through hard lumps. Holes have been drilled to a depth of 80 ft, but the limit of efficient operation is about 50 ft. In deep holes it is necessary to unscrew the string in 20-ft lengths, to

Jan 1, 1948

By W. F. Guenther

The usual hand-operated drilling outfit consists of a 4-in. post-hole auger with 3/4,-in. pipe for drill stem, in 4-ft lengths, with a turning handle fitted to a top pipe T. The auxiliary tools are: a chisel-bit drill made from 3/4 or 7/8-in. tool steel welded to a 4-ft length of 3/4-in, pipe, so that the regular pipe string can be used; also a churn or "mule foot" made from 3-in. pipe, slotted on one side, belled to a 4-in. tempered cutting edge on the bottom, all welded to a 3/4-in. coupling by a yoke. Other tools required are pipe wrenches and cleanout tools made from old auto springs (Fig I). A 4 1/2 or 5-in. collar welded to a plate is often used to protect the mouth of the drill hole. In general the auger is used in the typical clay overburden and brown phosphate matrix, which is relatively soft. The churn or "mule foot1' is used in hard pan, lump phosphate or cherty ground. The drill is used for breaking flint, often found loose in the overburden. The drill with the chisel bit is used for trimming sides of the hole, sounding for lime bottom and breaking through hard lumps. Holes have been drilled to a depth of 80 ft, but the limit of efficient operation is about 50 ft. In deep holes it is necessary to unscrew the string in 20-ft lengths, to

Jan 1, 1948

By A. N. Roberts, N. W. Stump

New developments in on-stream analysis using immersed radioisotope gages including results from plant installations are described. The control of grinding and flotation using a small digital computer has been complemented by this development. A control scheme for grinding, which is based on maximum throughput at constant product size, and preliminary work in flotation control are also outlined.

Jan 1, 1975

By G. E. Keller

In connection with the work of Committee D5, Coal and Coke, of the American Society for Testing and Materials in developing new standards and improving old standards, series of tests were made to check the variance of sample preparation and analysis of American coals. Table I in the "Tentative Method of Preparing Coal Samples for Analysis - 02013-62T" is rather complicated, and the tests were designed to develop data for the simplification of this table. An allowance of 20% of the total variance of sampling and analysis for the sample preparation and analysis steps was used. Also, instead of coals being grouped into ash ranges, they were grouped as washed and raw (unwashed) coals. As a result of these tests, a simplified Table I for Tentative Standard 02013 has been proposed. A standard test for laboratories to check their variance of sample preparation and analysis has been developed. Committee D5 on Coal and Coke of the American Society for Testing and Materials has been making a study of all standards applying to coal for the purpose of improving and bringing them up to date and for breaking some of the existing standards covering a number of tests into single standards. As an illustration, sample preparation is now partly covered in ASTM Designation D492-48, Sampling Coals Classified According to Ash Content, and partly in ASTM Designation D271-58, Laboratory Sampling and Analysis of Coal and Coke. The latter contains, in addition to parts of sample preparation, methods for determining Moisture, Ash, Volatile Matter, etc. Although revision of sampling methods and sample preparation methods are now assigned separately, it is possible that they may end up as one standard. One of the first new Tentative Standards developed as the result of these studies was ASTM Designation D2013, Tentative Method of Preparing Coal Samples for Analysis. Although this method is quite an im- provement over that in the old standards and gives very specific instructions, Table I (attached) is quite complicated and rather hard to understand. In order to take advantage of reduced quantities or weights, it is necessary to know the ash content within rather narrow limits before sample preparation and no distinction is made as to whether the coal is cleaned or uncleaned. No limits of accuracy are assigned to the sample preparation and analysis. The total over-all accuracy of sampling, preparation and ash determination as given in D492-48 has been specified for commercial sampling procedure as follows: "This procedure is intended for an accuracy such that if a large number of samples were taken from a single lot of coal, the test results in 95 out of 100 cases would fall within ? 10 per cent of the average ash content of the sample." Although Appendix 11, Method for Determining the Over-All Variance of Reduction and Analysis in the Tentative Methods for Mechanical Sampling of Coal, ASTM Designation D2234-63T, does give a method for determing the over-all accuracy of preparation and analysis expressed as variance and also the F test, it does not permit the determination of the variance at the various stages of reduction or of the ash determination. It was decided in 1961 to ask a number of laboratories to run a series of tests for the purpose of determining the variance at various stages of reduction and analysis with the view of simplifying Table I of the Tentative Standard D2013-62-T. This paper is a record of this series of tests with recommendations which resulted from the tests. At the same time and preceding these tests the International Organization for Standardization under Committee TC/27 WG 7 was studying the same problem. Tomlinson1 of England and Dr. paul2 of West Germany had made studies giving quite a bit of information. Also Schwerd and coryel13 published some information which was the main basis for the Mechanical Division provision in ASTM Tentative Standard D2013-62T, Table I. In checking with the various laboratories which offered to cooperate in these tests, none was found which used mechanical division through the entire preparation procedure. It was then decided to use riffles at all stages with the thought that if riffles gave satisfactory variances, approved mechanical

Jan 1, 1965

By F. W. Bryan, D. H. Lynch

Introduction This paper is a general description of current central Florida phosphate mining, beneficiation, and product transportation. It is directed and believed to be of interest to engineers not familiar with this industry. Deposit: The phosphate deposits of central Florida are generally located in a five county area which includes Polk, Hillsborough, Hardee, Manatee, and DeSota counties. Geologically, the deposit is of marine origin and is identified as the Bone Valley formation. This formation is Pliocene to Recent in geological age and overlies a Miocene limestone formation known as the Hawthorn. The Bone Valley formation sediments are regionally characterized by equal proportions of apatite, quartz, and clay. The clay is predominantly of the mont-morillonite family. On a local scale, however, the proportions of these three major constituents vary considerably. The phosphate occurs as the apatite mineral (Ca 10F2(PO4)(6) and with the clay and sand, the minable ore is commonly referred to as matrix. This matrix is overlain by unconsolidated overburden of sand and sandy clays, ranging in depth from 10 to 45 ft. The matrix usually occurs in fairly horizontal continuous beds from 3 to 25 ft in thickness. The bedded limestone formation lies directly below the matrix and is generally well defined. The phosphate particles range from 3/4 in. to 200 mesh (Tyler) in size. The phosphate particles coarser than 14 mesh are called pebble phosphate and those less than 14 mesh are termed flotation feed which, when beneficiated, subsequently become concentrates. Through mining and beneficiation, phosphate quality is measured in BPL percent which stands for bone phosphate of lime units. In subsequent chemical manufacturing, the quality is indicated by P205 content. The deposit is economically characterized by various ratios such as tons of product per acre and cubic yards handled per ton of product. Magnesium, iron, and aluminum content are also considered in evaluating ore reserves. These elements are often critical to the chemical fertilizer processes. Presently, an ore body is considered economically minable if it meets the criteria shown in [Table 1]. These, of course, are general guidelines and specific costs and returns on investment must be considered in each case for acquiring reserves. On a new grass-root venture, a 20-30 year life is generally expected with a mineral recovery of 80%. History and Uses Phosphate mining in central Florida began around the turn of the century. However, in the early days, only pebble phosphate was produced until about 1930 when technology was available to beneficiate the -14 + 150 mesh particles. The -150 or -200 mesh material was discarded as it is today. The basic processes for beneficiation are washing, scrubbing, desliming, sizing, and flotation. These basic unit processes are essentially the same today although many improvements have been developed since the early days. Phosphate is used primarily in the production of high analysis fertilizer chemicals, typical of which are triple superphosphate, monoammonium phosphate (MAP), and diammonium phosphate (DAP). Phosphate is also used in the production of food preservatives, dyes for cloths, vitamin and mineral capsules, steel hardeners, gasoline and oil additives, toothpaste, shaving creams and soaps, bone china dishes, plastics, optical glass, photographic films, light filaments, water softeners, insecticides, soft drinks, road fill, and livestock feed supplements. Florida produces over 80% of the nation's marketable phosphate rock and one-third of the world production, according to the US Bureau of Mines. This amounted to approximately 35 million tons in 1975. Exports of Florida phosphate rock were to such countries as Canada, Japan, West Germany, Italy, and India, with Canada and Japan being the major users. Almost 95 o of all outbound cargo shipped through the port of Tampa is phosphate rock or related products. Beneficiation Following is a description of Agrico's new Fort Green beneficiation plant which is typical of the newer large capacity plants being built in the field. Agrico's Fort Green mine was completed in 1975 and is located in the southwest corner of Polk County and is directly adjacent to Manatee, Hillsborough, and Hardee Counties. With some minor differences, Fort Green is typical of a modern central Florida plant. The rated capacity is 3,000,000 plus tons of product per year and this varies according to the richness of the ore being handled. A simplified flowsheet is presented in [Figs.1 and 2]. This plant is served by three draglines of the 40-cu-yd class. The phosphate beneficiation is usually divided into three major functional steps: (1) washing and screening to produce a pebble product and flotation feed, (2) feed preparation and (3) flotation to produce concentrates. The typical plant is similarly divided into these three functional areas. Washer: Briefly, the slurried matrix is pumped from two draglines simultaneously at a combined rate of about 20,000 gpm at 2000 tph (solids) to rotary trommel screens sized to make a 7/8-in. separation. ([See Fig. 1]-) The trommel oversize is sent to hammermills where it is crushed and returned to the trommel screens, or pumped to tailings if minor impurities (Fe203, A1203, MgO) are too high. The trommel undersize is pumped to 14 mesh stationary (static) flat screens. The flat screen over¬size is subjected to three stages of 14 mesh vibrating screening and two stages of log washing in order to produce a final pebble product. The pebble product (+ 14 mesh material) is conveyed by belt conveyor to a large on-ground storage pile. Pebble product is reclaimed through a tunnel and loading system below

Jan 1, 1980

By E. E. Bauer

Technical data describing the critical points for selection of the proper hammer and of the boom and power pack for mounting on mobile gyratory crusher installations are presented. Charts describing typical rocks with breakability indexes for hammer selection are included. Comparative data of representative available hammers along with criteria for evaluating hammer selection are also presented. Factors affecting the selection of the boom and the power pack, as well as optional features for ease of operation and improved safety are described.

Jan 1, 1986

By John B. Goddard, David R. Brosnahan

Leaching of uranium in situ from sandstone deposits with ammonium carbonate solution containing dissolved oxygen occurs rapidly compared with the leaching of the bulk of the sulfur present as FeS2. However, because of their high reducing capacity and their relative abundance, the FeS2 minerals consume the bulk of the oxidant. A pressure leach apparatus was constructed that permitted measuring oxygen consumption by FeS2, best described by a first-order reaction. The experimental rate constants for various cores are roughly proportional to their FeS2 contents.

Jan 1, 1983

Although the Suggestions to Institute Authors, as revised and amplified over the years to meet changing conditions and experience, have had as their primary objective the guidance of the author who is preparing a paper for record in the TRANSACTIONS, there are in this current version many excellent suggestions for the preparation of any material for publication by the Institute In this connection it should be emphasized that in a sense, and to a degree determined by the editors, the Institute has in its journals "a place for everything," especially a place for the article of practical nature that is of immediate but not necessarily permanent interest Such articles may be referred by the Institute Technical Publications Committee to the editors or submitted directly to them , [Papers (TECHNICAL PUBLICATIONS and TECHNICAL NOTES) authorized for the TRANSACTIONS are, with the discussion, gathered together at the end of the calendar year and with a table of contents and index, bound, according to Branch classification, as volumes of the TRANSACTIONS

Jan 1, 1952

By John A. Ames

AMERICAN pioneers first discovered "commercial" salt in western New York State. Geologists gave the classically correct name of Salina to the salt bearing strata of New York. Rock salt occurs in rocks of approximately the same age and stratigraphic position as New York's Salina "group", to the south and southwest, in western Pennsylvania, eastern Ohio and northwestern West Virginia. Sodium chloride and associated salts occur in brines throughout much of the same area as the rock salt. Brines also are found in areas well beyond the margins of that under which the rock salt lies, especially to the west in Ohio and to the south in West Virginia. The occurrence of the brines in the same area as the rock salt is almost always coincidental rather than indicative of a physical association.

Jan 5, 1950

By Robert E. Delavault, Harry V. Warren

IN the worldwide search of buried orebodies and for entirely new areas of mineralization, geo-chemistry is taking on an increasingly important role. Indeed, geochemistry itself is splitting into various specialties-hydrogeochemistry, pedogeo-chemistry, and biogeochemistry. This article primarily relates to developments in these fields in British Columbia, but many of the remarks are applicable to the whole continent.

Jan 10, 1953

By Guy D. Bruno

Through the remainder of this century, world consumption of fluorine per ton of primary aluminum produced will continue to be substantially reduced. Growth of the primary industry will offset some of the unit consumption, but demand for new fluorine sources will decline sharply. Continued application of dry fume scrubbing system will be the most significant factor in reducing demand.

Jan 1, 1979

By G. T. Lineberry

Power requirements for a piece of mobile mining equipment are largely dependent on the set of conditions in which they must operate. These conditions are isolated and key parameters are identified. The effect of operating conditions on power determination is investigated. A simulation technique is developed to predict ranges of power demands for off-highway haul units as an archetype, permitting the analysis of changeable operating conditions. This program uses given data, conditions, and probabilities and ranges to solve for individual components of power, which can then be summed. By adopting such a technique, a systematic and rational determination of power is made possible. The usefulness of this basic approach in the determination of power requirements for other mobile mining equipment is emphasized.

Jan 1, 1983

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

NEW MEMBERS The following list comprises the names of those persons who became members during the period Mar. 1 to 15, 1914: Members ADAMS, JOHN H., Cons. Engr First National Bank Bldg., Birmingham, Ala. ALEXANDER, WILLIAM H., Miner 80 Maiden Lane, New York, N. Y. AUSTIN, EDGAR TAYLOR, Asst. Smelter Supt., Mond Nickel Co., Ltd., Coniston, Ont., Can. BAKER, DANIEL, JR., Asst. Treas., Standard Lime & Stone Co. 524 Equitable Bldg., Baltimore, Md. BALL, MAX WAITE, Geologist U. S. Geological Survey, Washington, D. C. BARREN, HARRY B., Supt. Blast Furnaces, Inland Steel Co., Indiana Harbor, Ind. BAUMANN, HENRY N., JR., Amalgamator 365 Lynn St., Seattle, Wash. BLACK,, THOMAS B., Min. Engr Care Vulture Mines Co., Wickenburg, Ariz. BRADT, HARLAN H 429 West 111th_ St, New York, N. Y.

Jan 4, 1914