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By C. W. Covington, H. C. Cook, J. F. Libsch

Sputtered aluminum thin films were prepared in each of two conventional bell-jar vacuum systems. One system utilized an inner "getter sputtering" enclosure; the second system was a standard diode sputterirlg arrangement. Consistent and repeatable film properties were obtained in both systems provided sufficient cleanup and presputter time was allowed. The various problems associated with aluminum sputtering are discussed, with pavticular attention to the vzinimization of film contamination by outgassing and oxidation. The growth and structure of the aluminum thin films were studied with the aid of electron wzicroscopy and related to deposition rate, substrate temperature, and film thickness. The resistivity of the films was correlated to film structure and surface roughness. Resistiuities as low as 3.5 microhm-cm (2.3 x bulk resistiuity) were measured for relatively thick films (20,000). THIS investigation was undertaken to explore the problems and film characteristics associated with the sputtering of aluminum. Earlier work reported on aluminum sputtering has stressed the contamination of both the cathode and film as well as abnormally low deposition rates.' Data on sputtering yields,3 however, indicate that aluminum sputtering could be practical. Recently, it was shown by Theuerer and Hauser3 that aluminum sputtering was feasible in a conventional oil-diffusion pumped vacuum system provided an inner "getter sputtering" enclosure was employed to minimize gaseous contamination. This technique employs the getter action of aluminum to produce extremely low reactive gas partial pressures in the deposition zone. Aluminum films have already found use in solid-state electronic devices such as transistors and integrated microcircuits. To the present time, most aluminum films have been prepared by evaporation due to the ease with which this metal can be evaporated. Controlled sputtering of aluminum offers a number of advantages over evaporation, however, such as 1) manufacturing compatibility with other metals which must be sputtered, 2) better control of process variables resulting in more repeatable and uniform films, 3) generally better adhesion resulting from higher-energy metal atoms, 4) built-in material supply for continuous operation, and 5) the ability to deposit alloys. The data presented in this paper are the result of two separate studies. One study utilized a small "getter sputtering" enclosure (System A) and was concerned with the structure and properties of thin aluminum films up to about 1600A thick. In this thickness range, study of the film structure was possible with transmission electron microscopy. The second study was conducted with a conventional diode sputtering apparatus (System B) and covered $ much wider range of film thickness up to about 34,000A. Emphasis was placed on developing techniques which would extend aluminum sputtering to an existing in-line continuous deposition process.4 I) EQUIPMENT AND PROCEDURE System A. Fig. 1 shows a schematic of the "getter sputtering" inner chamber used and Fig. 2 is a photograph of this chamber mounted on an 18-in. access ring of a standard liquid-nitrogen trapped bell-jar vacuum system. This chamber was designed after a similar system used by Theuerer and auser.3 The configuration allowed the glow to emanate in all directions from the cathode. Argon (99.99') was allowed to enter only at the top of the chamber such that most of the reactive gases entering with the argon were reacted with the aluminum vapor and deposited on the chilled walls of the chamber before reaching the deposition zone. Provision was also made as shown, Fig. 1, for heating and cooling the substrate from about 20" to 400°C. Two substrate materials were used: Corning 7059 glass (12 by 12 by 0.048 in.) and carbon films about

Jan 1, 1967

By Geoffrey Purcell

Improvements which have been made in commericial flotation systems during the past fifty years have resulted more from trial and error methods in the mill than from research in the laboratory. Research has often provided explanations of why mill changes have improved the metallurgical process. Hopefully, in the next fifty years, changes in mill flowsheets will come about, primarily, as a result of research work. However, since minerals, in their infinite variety, cannot be reduced to a standard state, research on commercial ores will have only a local utility, and research on pure minerals will have little commercial application. What will emerge from research on pure systems are mechanisms of adsorption, and this in turn may throw some light on the very much more complex adsorption processes taking place in the pulps of commercial ores. Quartz, without a doubt, has been the subject of more research effort than any other mineral, but we are still a long way from completely understanding its behavior in flo¬tation. Hematite and calcite have received considerably less attention. Ores containing a mixture of all three minerals, however, are commercially important, and the iron deposits in Alabama have been extensively studied by the United States Bureau of Mines (1). The literature reveals no reports of research on synthetic mixtures of all three.

Jan 1, 1967

By W. I. Duvall, D. E. Stephenson. Discussion by R. G. K. Morrison

R.G.K. Morrison (Chairman, Dept. of Mining Engineering and Applied Geophysics, McGill University, Montreal, Que. Canada) - The authors have introduced a subject, the intensive study of which has awaited scientific developments. These are now such as to justify a thorough review of our thinking on the causes and control of rockbursts. The formulae developed in the paper, the comparison between rockbursts and earthquakes in figure 1 and the energy data relating to explosives serve as an effective foundation. In the paper this writer is quoted as suggesting that energy of the order of 10 x 10 11 ft. lb. may have been released in some of the heaviest rockbursts in the Kolar Gold Field. He now hastens to add that such an estimate has no scientific validity. It arises only from a casual comparison of surface and underground effects of the medium heavy bursts, referred to in the paper and estimated by Jones at 3.0 x 1010 ft.lbs., with those of obviously greater magnitude. In any case, we have the estimate by Jones above, that by a team of seismologists 1 on the Witwatersrand of 10 x 1010 ft.lbs., that by Coates of 3.8 x 10" ft.lbs., also referred to in the paper, that by Blan-chard2 for the catastrophic rockburst at Springhill, N.S., of only 7.4 X 107 ft. lbs., and finally the range covered by Cook, referred to in the paper. It is probable also that data for the heavy rockburst at Merkers3 in the WERRA potash area of Germany are available as it was recorded on seismographs from Moscow to Spain. It is the writer's impression that some standardization is present in the estimates above for 10 x 10 10, 3.8 x 1010 and 7.4 x 107 ft.lbs., respectively. The latter, for Springhill, represents a relatively low order of magnitude. It is obvious that any energy estimate must be related to the local geometry of openings at the time of the event. It is also obvious that any explanation of the causes of rockburst must be capable of providing a wide range of energy. However, we must remember that the energy release is an effect indicating magnitude. The cause lies with the mechanism initiating the primary failure, generating the seismic activity, to which much of the damage is probably due.

Jan 1, 1967

By Sidney Katell

This report, covering the period January 1966 through December 1966, is a continuation of a series that began with the publication of Information Circular 7516 in October 1944. It is the eighth in a series of reports prepared in cooperation with the American Association of Cost Engineers. The abstracted articles are concerned with all phases of cost engineering in the field of chemical and petroleum plants and related subjects. They are from the following sources: 1. American Association of Cost Engineers Bulletin. 2. Bureau of Mines Information Circulars. 3. Bureau of Mines Reports of Investigations. 4. Chemical Engineering.

Jan 1, 1967

By L. T. Grose

The Bureau of Mines conducted a comprehensive study of the Kanab, Kolob, Kaiparowits, and Harmony coalfields of southwestern Utah to obtain additional information and to determine the potentials of these coalfields as sources of energy for steam-electric power-generating plants. Field examinations were made to ascertain the geologic structure and the stratigraphy of the coalfields, the accessibility of the coal-bearing strata, and the general nature of the coal-bearing strata and the terrain. Many mines, both active and abandoned, were examined, and key personnel in the coal industry in the area were consulted. Available analyses of southwestern Utah coals were compiled, and tentative conclusions regarding the rank and quality of the coals were drawn. Coals have been classified by rank according to the standards established by the American Society for Testing and Materials in 1964. The Parr formula for moist, mineral-matter-free British thermal units has been used to calculate the rank of each sample, except as otherwise noted. Water resources related to the areas of the coal reserves also were investigated. Existing literature and maps pertaining to the geology of the areas were reviewed. Production potentials of the coalfields and economic conditions affecting the possible utilization of the coal reserves as sources of energy for steam-powered electricity-generating plants were investigated and analyzed. The data obtained and the conclusions reached as a result of this study are included in this document. The total reserves of subbituminous A and high-volatile bituminous C coals in the fields of southwestern Utah are estimated to be at least 8 billion short tons at depths generally less than 2,000 feet. It appears likely that this estimate will be increased as additional data are made available through exploration and other investigations. Sufficient coal is available in four southwestern Utah counties to supply three or four large steam-electric plants. If the States involved grant water rights to companies planning to build steam-electric plants, the cost of producing power with coal might be attractive and might justify the construction of one or more of these plants.

Jan 1, 1967

By A. G. Sharkey

THE PURPOSE of this investigation was to develop methods for analyzing coal derivatives and products from the Fischer-Tropsch synthesis. As part of this investigation it was necessary to study the mass spectral characteristics of many classes of compounds. The mass spectra of alcohols, the trimethylsilyl ether derivatives of alcohols, acetal-type compounds, ketones, esters, and naphthenes were correlated with structure, and analytical methods were formulated. A method was devised to determine the ratio of branched to normal hydrocarbons up to CIS in the Fischer-Tropsch product. Low-ionizing-voltage mass spectrometry was combined with type-analyses to analyze tar acids and neutral oils from coal. The necessary sensitivity correlations at low-ionizing voltage were developed, particularly for phenolic compounds. Special analytical techniques were developed for the mass spectral analyses of specific compounds and compound types including (1) oxides of nitrogen, (2) hydrogen sulfide, (3) isomers of butenes and pentenes, and (4) hydrogen deuteride. An investigation was made of the effects of various hydrocarbons and oxygenated compounds on tungsten filaments in the mass spectrometer. The operating characteristics of rhenium filaments under similar conditions were studied. Several improved sample handling techniques were developed, including an automatic manometer and a self-filling micropipet. Studies were made of anomalous and negative peaks in the mass spectra of certain gases.

Jan 1, 1967

By J. G. Walters

This bulletin presents, in collected and tabluated form, Bureau of Mines and American Gas Association (EM-AGA) carbonization data pertaining to the chemical analysis of tars and the characterization of tars and light oils obtained from U.S. coals.

Jan 1, 1967

The Bureau of Mines studied available information on the nature and occurrence of potential sources of aluminum in the United States, its Pacific island possessions, and Puerto Rico to obtain data for use in evaluating the production capability and costs of extracting the aluminum from such materials. The quantity, type, and grade of the materials range from 4 billion tons of bauxite, bauxitic clay, and kaolin averaging 33 to 42 percent Al2O3 to nearly 600 billion tons of anorthosite containing only 27 percent Al2O3. Principal deposits of bauxite, bauxitic clay, and kaolin occur in Arkansas, Georgia, Hawaii, and Oregon. Major anorthosite deposits are located in New York, Wyoming, California, Idaho, and Montana. About 11 billion tons of material in deposits of various types of clay, the kyanite group of minerals, laterites, and shales averaging 27 to 30 percent Al2O3 comprise additional resource's from which aluminum some day may be extracted. Material meeting specifications of the study was found in only 22 States and the Pacific island possessions. Utilization of these large low-grade sources of aluminum awaits development of processes that are economically competitive with the Bayer process for extracting alumina from baxuite, which is at present the only commercial ore of aluminum. Changes in economic and political conditions also may play important roles in the eventual development of the potential sources of aluminum.

Jan 1, 1967

This report briefly describes the broad program of research and technologic work conducted by the Bureau of Mines on coal and related subjects during 1966. In addition to n description of investigations on mining, preparation, and utilization of coal, an account is given of the Bureau's work in mine health and safety, coal resources, mine explosives, and environmental conditions relating to coal mining and utilization. Details of most of the projects are reported in publications cited throughout this report. Centers and laboratories conducting the coal research and related investigations appear in appendix A; organizations, institutions , and companies contributing to the Bureau's coal research and technologic program are listed in appendix B.

Jan 1, 1967

By Kung-Lee Wang

This report describes the linkage of all mining sectors with all other manufacturing, services, and final demand sectors of the U.S. economy. Besides being a basic data source, it provides a framework for aggregate economic impact analysis with respect to the mining industries. The framework is an open-static input-output model specifying 48 mining industries as classified in the Standard Industrial Classification Manual for all mining activities and 76 nonmining industries which collectively exhaust, all economic activities. The 124-sector model used in this report is an expansion of the preliminary 82-industry aggregation estimates made by the Department of Commerce. In the expanded model, 48 ruining industries are substituted for the original 6. The methodology used to ascertain the industry-by-industry procurement cost estimates and product ion flows necessary to the construction and expansion of the basic 82-sector model included personal interviews, case studies of specific mining activity analysis, and published and unpublished data from the Bureau of Mines and the Census of Mineral Industries, The end products of this study are two tables arranged to show the direct purchases necessary for each industry to support the level of economic activity and the total purchases generated in each industry throughout the economy by each $1 of aggregate economic demand in 1958. The tables may he used for economic impact studies and market analysis by firms engaged in or closely associated with the mining industries. Some illustrations of their usages are presented.

Jan 1, 1967

By R. A. Guereca

Preliminary to an experimental study of selected physical properties of helium and related gases) the Bureau of Mines Helium Research Center conducted a data-gathering literature survey. This report combines the results of the 1961-63 literature search into a usable format. The data accumulated on the physical properties are presented in tables and graphs. The data in the tables were chosen for exact representation and comparison of specific values. An attempt was made to select the most reliable and consistent value available for a given property without extensively analyzing each source reference. The methods of evaluation are discussed later. The graphs show trends and anomalies which may be obscure in tabular form. (Reprints of the graphs) with the scale grid enlarged 2 1/2 times) are available upon request through the Research Director) Helium Research Center.) The literature search was conducted using Chemical Abstracts as the primary reference source with additional information drawn from Applied Science and Technology Index) Chemical Reviews) Physics Review) Science Abstracts (Physics») and other abstracting services. Part of the data included in this report have been tabulated previously by others (£-1).5 In a few areas) the sources of information are scarce and obscure (for example) refractive index and dielectric constant). The search was extensive; however) some sources

Jan 1, 1967

By Scott W. Hazen

COMPREHENSIVE summary is presented of results of several years of research at the Bureau of Mines Mining Research Center at Denver on adapting and applying techniques of statistical analysis in mine and mineral-deposit sampling and in computing grade and tonnage of ore for a mineral deposit. In addition to elementary statistical theory the material presented in the bulletin includes: (1) Certain special statistical techniques that have been found useful in mining applications; (2) problems, implications, and limitations that may be encountered in applying these techniques in mine sampling and evaluation; and (3) numerous examples to demonstrate application of the theory and techniques.

Jan 1, 1967

By J. Parker

As a practicing mining engineer, I face many rock mechanics' problems daily and would like to mention one or two examples to illustrate the current gap between laboratory investigations and actual field problems. I would like to endorse Dr. Obert's suggestion that more field measurements and observations should be undertaken. There is an ever-increasing body of data beginning with Hast's results in Sweden,l then measurements at Elliot Lake, Canada, and so on, including our own measurements at White Pine, which clearly indicate that the horizontal stresses underground. are often at least as large as the vertical stresses. Visual observation of the deformation of roof and pillars (including failure due to horizontal compres- sion) also demonstrates that the horizontal stresses are often most important: Yet almost every laboratory investigation begins with the assumption that the only stresses acting are vertical. Roof spans in layered formations. for example, are calculated on the assumption that the rock behaves as a gravity loaded beam. This is all too often unrealistic.

Jan 1, 1967

By J. R. McWilliams

Several of the current concepts of brittle fracture involve consideration of the existence of defects or flaws. Griffith 1 observed that the tensile strength of brittle materials was several orders of magnitude less than might be expected from the calculated strength of the molecular bonds. He was able to show that the stress concentration at the tip of an elliptical crack is sufficient to raise the local stress level many fold. He therefore proposed that real materials do contain such stress risers in the form of minute cracks and that this accounts for the rather large difference between theoretical and actual strengths of brittle materials. The degree of stress magnification depends to a great extent upon the orientation of the crack with respect to the general stress system, and to the general geometry of the crack.

Jan 1, 1967

By W. C. McClain

In the design of underground excavations, rock mechanics considerations are nearly always based on an elastic behavior of rock. Most rocks do exhibit a certain amount of elasticity, and the application of principles and concepts of elasticity to rock mechanics problems has been largely responsible for progress in the field over the past 10 or 15 years. No doubt the theory of elasticity will remain the most useful analytical tool available for both the design of underground openings and the interpretation of phenomenological data.

Jan 1, 1967

Researchers, medical organizations, statisticians, and others often use data on the nature and rate of occurrence of occupational diseases in directing their efforts and plans. Very often this information is developed from the reports of the States which describe the nature of work¬men's compensation claims and awards and the frequency with which they are made. To be meaningful, the statis¬tical information must be viewed in the context of the State laws involved. There is considerable variation among the laws of the different States. The Bureau of Mines has responsibilities for protecting the health of persons employed in the mineral industries and for the development of useful mineral products. To assist the Bureau in the accomplishment of its objectives, this compilation has been undertaken. For the benefit of the mineral industries, and any others who may have a similar interest, this volume is made available. An earlier compilation of the Bureau of Mines on this subject was published in 1952.4 However, during the intervening years, sufficient changes have been made in State laws to warrant completely recompiling the information. This publication includes the laws of the States, the District of Columbia, Puerto Rico, and the Virgin Is¬lands through 1964. Only those portions of the workmen's compensation laws which apply to or as ' related to occupational diseases are presented, and in each case enacted additions to and deletions from the basic law have been incorporated into the text of the law, thus snak¬ing it unnecessary to search out the various amendments made each year.

Jan 1, 1967

By John J. Mulligan

The Bureau of Mines investigated the tin deposits of the Cape Mountain area during July and August 1962 to test the effectiveness of detrital-cover sampling in permafrost areas as a relatively cheap and simple means of guiding mine development and exploration. Results indicate that systematic detrita1-cover sampling can be used effectively to delineate obscure deposits with sufficient accuracy to permit sampling with a minimum of trenching or drilling. Extensions of known outcroppings were traced in sufficient detail to guide lode sampling and several previously unknown tin-bearing lodes were found and sampled. Lode sampling was limited to the minimum needed to establish the reliability of detrital-cover sampling results. The results of previous lode and placer investigations are summarized and detrital-cover sampling methods and results are described in detail.

Jan 1, 1966

By Norman G. Foster

The mass spectra of four tertiary butyl substituted thiophenes are reported. A comparison and contrast with earlier structure correlations made by API-RP48 mass spectroscopists is presented. The fragmentation routes of these types of molecules are discussed and explained in terms of existing theories in mass spectrometry. Low ionization voltage data are presented to support the mechanistic picture developed. Structures are inferred about some of the ions, and these are correlated with existing theories. Metastable peaks in the spectra are used to support the fragmentation paths. The presence of doubly charged ions in the spectra is noted and the possible implications toward mechanisms discussed. The general picture of simple, small fragments leaving the ion moiety upon further fragmentation is developed in detail. Some suggestions are presented for further work utilizing isotopically labeled molecules to establish firmly the general picture of fragmentations of the alkylthiophenes.

Jan 1, 1966

By Charles G. Zink

Anthracite is widely known as a domestic or space heating fuel. The prevailing market ratio of domestic to industrial consumption was about 80 to 20 up until 1950. Since then it has been shifting until now the ratio index is about 50/50, exclusive of overseas export. Despite a declining domestic space heating market, the demand for industrial anthracite remains good. However, as a result of stringent air pollution regulations, there is a renewed interest in this low sulphur coal which cannot smoke under any conditions. Anthracite serves other important industries such as power generating, metallurgical, cement, ceramic, chemical, water sewage and industrial wastes filtration. Anthracite is an excellent natural source of carbon and may be utilized in many processes.

Jan 1, 1966

By R. O. Vernon

The Florida Peninsula has existed as a part of a much broader plateau, since at least the Early Cretaceous. This plateau, the Floridan Plateau, now consists of the present peninsula and a broad submerged shelf of equivalent size extending the length of the state and out into the Gulf of Mexico. Florida Peninsula was separated from the mainland United States by a negative area called the Suwannee Straits. To the south of this feature existed an environment similar to today?s Bahamo Banks where very pure calcium and magnesium carbonates with associated evaporites were deposited. Thus the Eocene and Oligocene contain little or no quartz sand or clay minerals except in the Panhandle west of the Suwannee Straits where some clastics were contributed by rivers from the north.

Jan 1, 1966