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By William M. Hinton

This report describes the approach, procedures, and results of a program to develop training materials for roof bolter operators. The objective of the program was to design and produce a training sequence which would prepare roof bolter trainees for job performance. Data was collected and analyzed using the general procedures of Instructional Systems Development (ISD). Input data came from a previous roof bolter training analysis program. This data was expanded and structured through a series of ISD steps: objectives hierarchies, media selection, syllabus, lesson specifications, and train¬ing materials development. The resulting program consisted of an ordered sequence of 15 lessons. The media mix for the 15 lessons included lectures, slide-tape lessons, and hands-on instruction using operational roof bolters. Contents of all lessons were reviewed and approved by the Bureau. The key recommendations were to (1) validate the materials and measure relative effectiveness of media formats; (2) survey mines for training resources and conditions - match materials to user capabilities, rather than selection state of the art technology/media; (3) develop job performance aids (JPAs) rather than simulators; (4) create a style/media/JPA development guide for use in future projects of this kind.

Jan 1, 1982

By Mark P. Meyer

A mineral investigation of the Chugach National Forest, Alaska was conducted jointly by the U.S. Geological Survey and the U.S. Bureau of Mines from 1979 to 1983 as part of the RARE II program. The U. S. Geological Survey remapped the geology and distribution of mineral resources. The Bureau investigated mines, prospects, and mineral occurrences. Previously unreported mineralization in three areas, Long Bay, Wells Bay, and Miners River were discovered in the western portion of the SOUND study area. Copper, lead, zinc, gold, silver, nickel, cobalt, fluorite, and arsenic were found in north-northeast to north-northwest trending shear zones, veins, felsic dikes, and granitic intrusives in Tertiary Orca Group metasedimentary rocks.

Jan 1, 2011

By J. R. Thoenen

For several years the Bureau of mines has been investigating the characteristics of ground vibrations produced by quarry blasts. Considerable basic information has been obtained in the course of this study, and the results have been made known to the public through various publications listed in the accompanying bibliography. The studies have been confined to obtaining fundamental knowledge of the characteristics of the vibrations themselves, because it was evident at once that he problem was extremely complicated. It was felt that any attempt to predict the effect of a ground vibration on an' type of artificial structure would be useless until the complexities of building vibrations are better understood. As opportunity offered, teats wore made in various types of structures and the effects of vibrations from many different sources were measured. In one set of tests (5)4/, it was demonstrated that the behavior of a building as quite different if it was shaken by vibrations originating outside tae foundation walls than if the source of the vibrations was within the building; vibrations coming from the round outside seemed to shake the building as a single loosely-coupled structure, whereas mechanically induced vibrations within the house seemed to set floors and walls in motion as independent units, each of which communicated its own natural motion to the adjoining member, causing a very complicated movement that was impossible to interpret.

Jan 1, 1938

By J. R. Thoenen

For several years the Bureau of mines has been investigating the characteristics of ground vibrations produced by quarry blasts. Considerable basic information has been obtained in the course of this study, and the results have been made known to the public through various publications listed in the accompanying bibliography The studies have been confined to obtaining fundamental knowledge of the characteristics of the vibrations themselves, because it was evident at once that he problem was extremely complicated. It was felt that any attempt to predict the effect of a ground vibration on any type of artificial structure would be useless until the complexities of building vibrations are better understood. As opportunity offered, teats wore made in various types of structures and the effects of vibrations from many different sources were measured. In one set of tests (5)4/, it was demonstrated that the behavior of a building as quite different if it was shaken by vibrations originating outside tae foundation walls than if the source of the vibrations was within the building; vibrations coming from the ground outside seemed to shake the building as a single, loosely-coupled structure, whereas mechanically induced vibrations within the house seemed to set floors and walls in motion as independent units, each of which communicated its own natural motion to the adjoining member, causing a very complicated movement that was impossible to interpret.

Jan 1, 1938

By B A. Tapp

The minerals industry in Australia is currently regarded as the country's economic saviour; the bastion of economic security. As Fitzgerald (1974) stated, 'Australia's natural endowments in minerals are the envy of most countries of the world'. As a result the proposed new mineral developments are on a scale that hitherto in the sixties would have been completely un-envisaged. It is reported that Australia is poised on the verge of a 16 billion dollar mining-based investment boom: a boom that will see Australia dominate the energy export field, the mineral processing field, and create the 'coal dollar'. This growth scenario has many inherent dangers, and it is the authors' contention that these should be carefully considered before further development proceeds. Two of the major problems related to the mineral industry growth scenario are the predictability of the future metal market, and the energy cost of mining. The latter problem is the one discussed here. The mining-mineral processing industries in Australia currently use about 36 per cent of Australia's primary energy budget. This large energy input is dominated by two major industries, iron and steel and the rapidly developing a1uminium industry. These two combined use over 20 per cent of the total Australian energy budget. In an industry which is export oriented about 96 per cent as expressed in ex-mine value terms û much of the energy input is exported along with the product. The authors therefore urge that serious consideration by the mineral industry be given to the relatively high energy intensiveness of process operations, especially in respect of the aluminium industry.

Jan 1, 1980

By Lenin Salazar Dulanto

La baja de precios en algunos minerales ha obiligado que las empresas mejoren su proceso productivo a través del uso de equipos de última tecnología en los procesos de mecánica, hidráulica, electricidad y electrónica, así como en la eficiencia en el corte y taladrado, extracción y transporte. Sin embargo, tanto el desatado y sostenimiento manual desarrollaron un estréss y desgaste de energía en el trabajador. En este sentido, el presente trabajo señala una nueva forma de realizar tales operaciones en el ciclo de minado de la empresa Milpo a fin de garantizar la seguridad física de los trabajadores y equipos.

Jul 31, 2003

By W. D. Monaghan

Flame cutting and welding is one of the major causes of fires and explosions in underground U.S. coal mines. On May 20, 2006, a flame cutting operation at the Darby Mine No. 1 led to an explosion that resulted in five fatalities. On January 22, 2003, another explosion caused by flame cutting at the McElroy Mine resulted in three fatalities and three serious injuries. On June 22, 1999, a flame cutting and welding operation at the Loveridge Mine caused a fire that resulted in sealing of the mine for an extended period. Finally, on March 19, 1992, an explosion at the Blacksville No. 1 Mine that was caused by welding resulted in four fatalities. The National Institute for Occupational Safety and Health (NIOSH) conducted a study on fires and explosions in underground U.S. coal mines that were caused by flame cutting and welding operations to determine the root causes of these types of fires and explosions. The methodology included interviewing mining personnel who perform flame cutting or welding operations in underground U.S. coal mines and visiting mines to observe these operations, and MSHA reports of investigations and accidents statistics were analyzed. The results were used to identify and compare differences between flame cutting and welding practices and techniques in small and large mines, Eastern and Western mines, low seam and high seam mines, room and pillar and longwall mines, and between experienced miners and new miners. As a result of this study, best practices and interventions were developed to reduce the number of fires and explosions caused by flame cutting and welding. This paper provides a summary of this work. Disclaimer: The finding and conclusion in this report are those of the authors and do not necessarily represent the views of the National Institute for Occupation Safety and Health.

Jan 1, 2009

By J. S. Miller

This report presents a complete coverage of results from Bureau of Mines preliminary research and the field application of explosive fracturing techniques to prepare oil shale for in situ recovery of shale oil. Small-scale surface tests were conducted to determine the feasibility of using a nitroglycerin-base explosive for creating rock fractures. Prior to underground testing, surface and near-surface tests with liquid explosives showed that explosions in sheetlike layers simulating underground fractures would propagate effectively. Successful surface experiments were conducted using layers of explosive placed between glass plates and explosive-saturated sand confined in small-diameter metal tubes. The tests in glass-plate reservoirs and metal tubes demonstrated that nitroglycerin would detonate and the explosion would propagate in cracks as thin as 1/32 inch and through distances up to 12 feet. In a shallow field test, nitroglycerin was detonated in a vertical crack in limestone and produced extensive fracturing. Explosive fracturing tests were performed in oil shale formations on seven sites near Rock Springs, Wyo. The procedures included (1) displacing and detonating nitroglycerin in natural or hydraulically induced fracture systems; (2) detonating nitroglycerin in wellbore shots; (3) displacing and detonating nitroglycerin in induced fractures followed by wellbore shots using pelletized TNT; and (4) detonating wellbore charges using pelletized TNT. The research on oil shale formations demonstrated that nitroglycerin displaced in a natural or hydraulically induced fracture would detonate, and the explosion would propagate through the explosive-filled fracture. Shooting a pattern of wells in oil shale at 100-foot depth with wellbore charges of pelletized TNT developed a satisfactory interwell fragmented zone. Tests performed on other sites at depths to 385 feet caused fragmentation of rock around the wellbore and provided interwell communication. Fourteen methods used to evaluate the extent and degree of fragmentation in the explosive fractured oil shale are discussed.

Jan 1, 1974

Editor’s note: As usual, the June issue features an industrial minerals review. And some thanks are in order. Thank you to the industrial minerals annual-review editor, to the technical committees chair and vice chairs and to the authors of the individual commodity profiles. Jim Norman of GeoTrans Inc. is the industrial minerals annual-review editor. William Langer, U.S. Geological Survey, is the chair of the SME industrial minerals technical committees and the vice chair of the technical committee for construction materials. Other technical committee vice chairs include: •Lucy McCartan, U.S. Geological Survey, agricultural minerals. •Steve Herron, Oglebay Norton Performance Minerals, ceramics and refractory materials. •Srinivas Veeramasuneni, U.S. Gypsum, chemical raw materials. •Ismail Yildirim, Imerys, fillers and pigments. •Charles Landis, BPM Minerals, sorbents, filters and process aids. •Ray Harris, Wyoming Geological Survey, specialty minerals. Their help makes possible this June industrial minerals issue. On behalf of the readers, the editors thank them

Jan 1, 2004

By Jason Morrison

The Norwegian Lake Tap Method was successfully used to tap into the side of Lake Dorothy 36.5 m (120') below the lake surface. The lake tap allows water to flowinto an access tunnel from the lake lowering the water elevation below its natural out-fall. When the lake reaches a predetermined elevation below the outfall, a 1.5 m (60?) valve in the tunnel will be shut and discharge from Lake Dorothy will stop temporarily allowing construction of a dam located 2.9 km (1.8 miles) downstream at Bart Lake. The lake tap and tunnel were one phase of the $64 million Lake Dorothy Hydroelectric Project, owned and operated by Alaska Electric Light & Power Company (AEL&P), a private utility located in Juneau, AK. The Lake Dorothy portal site and tunnel are located approximately 25.7 km (16 miles) southeast of Juneau, AK, in the remote Tongass National Forest at an elevation of 701 m (2,300') above sea level in the mountains above the Taku Inlet. Thirty degree snow covered mountainsides and limited access by helicopter were just two of the many factors which challenged this unique project. The lake tap and tunnel development consisted of 250 m (820') of horizontal tun-nel, averaging 3.6 m x 3.6 m (12' × 12'), excavated using conventional drill and blast methods in highly competent Granodiorite and Tonalite rock, placement of one 3.9 m (13') long concrete plug, or bulkhead, located at the tunnel midpoint, and one 3 m (10') diameter lake tap into the side of Lake Dorothy. This paper will provide an analysis of the logistical and engineering challenges involved in the development of one of only a handful of lake taps in North America. AEL&P and contractor J. S. Redpath Corporation worked together to complete this critical project phase safely and on schedule, in a location accessible only by helicopter and plagued by constantly changing, harsh weather conditions. A strict schedule had to be maintained to ensure the timely operation of the downstream dam and power plant.

The ultimate goal of a mineral processing plant is to recover as much of the target mineral(s) as possible from the ore being treated to achieve the best economics. Selection of the mineral processing techniques is the most important step in achieving this goal. However, due to the complexity of the ore, the recoveries of valuable minerals may be not satisfactory even when the mineral processing technique(s) are well chosen. In other words, minerals of interest can be lost to the tailings for mineralogical reasons. For example, gold is mainly extracted from the ore by gravity, flotation, cyanidation, or a combination of these processes, and high recovery (>90%) can be achieved when gold occurs as coarse grains. However, when a refractory ore is being processed, gold extraction will be challenged by mineralogical factors, which often cause gold losses to various tailings. Mineralogical factors affecting gold recovery mainly include grain size, shape, surface coatings and rimmings, presence of cyanicides, oxygen consumers and preg-robbers, presence of slow-dissolving gold minerals and the refractory nature of submicroscopic gold. Among these factors, locking in sulphide, silicate and other minerals as fine-grained gold inclusions and/or as invisible submicroscopic gold is by far the most common factor leading to poor gold recovery encountered in gold ore processing. Processing of PGE ores faces the same challenges as gold. Small grain size and locking of PGM in sulphide and non-sulphide minerals often cause PGM losses. When silver ore contains significant amounts of pyrargyrite, proustite and stephanite, silver recovery by cyanidation can be very low because of the slow dissolving kinetics of these minerals. In the processing of base metal ores, high content of pyrite, intergrowth of chalcopyrite with sphalerite and presence of clay miner-als may cause problems in recovering Cu-, Pb- and Zn- bearing minerals. Process mineralogy helps address all issues and problems related to mineral processing with predicting and trouble-shooting being two major objectives. It provides useful information on process selection, flowsheet development, recovery improvement and reagent consumption optimization. The information acquired from a process mineralogical study can be used as a guide for a metallurgical testwork program for process design or optimization.

Jan 1, 2014

The properties of interfacial water at hydrophilic surfaces are of great importance in many technological areas including flotation, solid-liquid separation, dispersion and emulsions, flocculation, adsorption, corrosion, and soil contamination. This paper examines the use of FTIR/internal reflection spectroscopy (FTIR/IRS) to study the spectral characteristics of interfacial water at silica surfaces. FTIR spectra were characterized by consideration of the OH stretching region (3000-3800 cm-1) associated with the vibrational spectra of interfacial water. The broad peak in this region was deconvoluted in order to isolate overlapping spectral features that describe the nature of hydrogen bonding in interfacial water. Three distinct bands were found; -3600 cm-1 (free OH), -3400 cm-1 (incomplete tetrahedral coordination), and -3240 cm-1 (complete tetrahedral coordination) and the variation of their intensities with pH was found to be significant. This spectral information helps to explain orientation and bond ordering of interfacial water molecules at hydrophilic surfaces.

Jan 1, 1998

By Felipe De Lucio Pezet

"El presente trabajo desarrolla la teoría de los pernos sobre la roca como método de sostenimiento y control de los mismos dentro de la mina subterránena. La aplicación de este método desplaza a las técnicas convencionales como el enmaderado y la manpostería, las cuales fueron usadas principalmente en el siglo XIX. Asimismo, el método de empernar la roca introdujo un nuevo conocimiento ya que se basa en la resistencia a la tracción y en el principio de refuerzo de la roca in situ. De otro lado, los pernos de roca originales fueron perfeccionados y variaron sus elementos para usos específicos, así como se implantaron los pernos cementados con mortero de cementoPortland y con resinas orgánicas sintéticas."

Nov 20, 1967

By M Suzuki

Although several models for the surface tension of molten oxide slag have been proposed, suitably accurate predictions of this property are not yet possible. The surface tension, or surface excess free energy, of molten oxides is largely determined by the ionic coordination induced by surface relaxation. However, the associated mechanism of surface structural relaxation for molten oxide mixtures such as slag is complex and not yet fully understood. To allow a better evaluation of surface relaxation characteristics, the present work analysed the ionic coordination associated with the surface-relaxed states of several oxide mixtures. This work especially focused on calcium aluminate slags because these materials exhibit complex relationships between composition and surface tension. The effects of incorporating low concentrations of SiO2 as a surface active component on the surface ionic coordination were also examined. X-ray absorption techniques were used to assess oxygen and cationic elements in glassy samples after surface relaxation treatments, and molecular dynamics simulations based on a polarisable ion model of molten slag with vacuum/melt interfaces were also performed. The X-ray absorption techniques provided data related to electron yields (which are primarily associated with surface features) and fluorescence yields (which evaluate the bulk material). Thus, the ionic coordination characteristics of both regions were investigated. The results of molecular dynamics calculations allowed statistical analysis of the distributions of Al- or Sicentred polymorphs as well as the bond angles between cations and oxygen anions in the vacuumexposed and bulk regions in the equilibrated melt. The results indicated that bridging oxygen ions were preferentially distributed in the relaxed surface region rather than non-bridging oxygens. These bridging oxygen ions represented vertex connections between AlO4 or SiO4 tetrahedra. In the case of the calcium aluminate slags, the addition of one Ca2+ ion as charge compensation for two Al3+ ions was found to be necessary to form two AlO4 tetrahedra. This specific feature of surface ionic coordination could be responsible for the complex trends observed in surface tension data. The incorporation of low concentrations of SiO2 reduced the proportion of tetrahedrally-coordinated Al ions such that higher coordination states become dominant in the bulk of the material, whereas AlO4 tetrahedra were preferentially distributed in the surface region. SiO4 tetrahedra were the preferred Si-centred polymorph and were likely connected to one another to form bridging oxygen ions at the surface. On the basis of these results, a model to predict slag surface tension was proposed, and the energy of the formation of the ionic clusters resulting from surface relaxation was taken into account.

Aug 21, 2024

By Kurt M. Larson

Future haulage cost projections led Foster Yeoman Limited into developing a fully mobile crushing and conveying system at its Torr Works quarry in Somerset, England. The purpose-built system has an effective throughput of 2,500 tonnes/hour and features an Orenstein and Koppel (O & K) manufactured walking frame, a Fuller-Traylor type 54 X 74 TC gyratory crusher, and unique mobile conveyor modules designed and manufactured by Foster Yeoman. Used in a single-bench operation in this 6 million-tonne per annum limestone aggregate quarry, the system is fed at the production face by 2 Caterpillar 992C loading shovels. The entire system is moved on a daily basis following production face locations.

Jan 1, 1986

By R. G. Gürtunca, J. A. Breslin

This paper briefly describes the progress in mine safety in the United States, with emphasis on recent events that have followed since the explosion at the Sago Mine in January 2006. Legislation following the mine accidents last year and areas of work carried out by the National Institute for Occupational Safety and Health (NIOSH) related to the accidents are discussed. American coal production in 2006 was 1,150 million short tons. Most of this coal is consumed domestically, with annual exports of coal about 50 million tons. One third of annual production is produced at surface mines and the rest from underground. This coal is produced by about 82,000 miners working at 1,400 coal mines. Major improvements in coal mine safety have been made in the US since the Federal Mine Safety and Health Act of 1977. The fatal injury rate in underground coal mines between 1977 and 2004 was reduced by 47.8% to 0.036. The annual number of fatalities dropped from 112 to 14 during that period. Likewise, the non-fatal days-lost injury rate was reduced by 42.6% from 10.87 to 6.24. The improvements in mine safety during this period can be seen in the graph of underground coal mine explosion fatalities and injuries from 1980 to present, which is shown in Figure 1. Between 1984 and 1993 (9 year period) there were 5 explosions and one major mine fire, for a total of 55 fatalities. Over the seven year period from 1993 to 1999 there were no fatalities from coal mine fires and explosions. However, in the six years since 2000 there have been 5 explosions and one fire, which have caused 37 fatalities. [ ]

By Chris Mark

Successful longwall mining requires a stable tailgate entry. Gate entry performance is influenced by a number of geotechnical and design factors, including: - Pillar size and pillar loading; - Roof quality; - Floor quality; - Entry width; and, - Artificial support (primary and secondary). This paper describes a comprehensive, practical, design methodology, based on statistical analysis of a nationwide data base of longwall ground control experience. Geotechnical surveys were conducted at 44 U.S. longwall mines, and underground observations of site geology, entry conditions, and support design were recorded at each mine. The observations were combined with discussions with mine personnel to identify 69 longwall gate entry designs as satisfactory, unsatisfactory, or borderline. Only conventional longwall designs, in which the pillars are expected to carry the full abutment loads, were included in the data base. Designs which employed yield pillars only were excluded. The case histories were characterized using five descriptive parameters. Pillar design was described by the Analysis of Longwall Pillar Stability Factor (ALPS SF). A major new contribution is the Coal Mine Roof Rating (CMRR), a rock mass classification system that quantifies the structural competence of bolted mine roof. Other quantitative measures were developed for primary support, secondary support, and entry width. Multivariate statistical analyses indicated that in 84% of the case histories the tailgate performance could be correctly predicted using just ALPS and the CMRR. Most of the misclassified cases fell within a very narrow borderline region. The analyses also confirmed that primary support and gate entry width are essential elements in successful gate entry design. The relative importance of the floor and of secondary support could not be determined from the data. Based on these results, a simple equation was developed to guide the design of longwall pillars and gate entries: ALPS SF,, = 1.76 - 0.014 CMRR Where: ALPS SF, = ALPS SF suggested for design. Guidelines for entry width and primary support density, as related to the CMRR, are also provided.

Jan 1, 1993

By C. A. Komar

The Bureau of Mines conducted oil-displacement tests in the laboratory with three water-in-oil and five oil-in-water emulsions that were created with ultrasonic energy at a frequency of 20 kHz and an acoustic intensity of approximately 100 watts per cm2. Emulsions of either crude oil or kerosine, brine, and 112 to 2 percent emulsifier were formed during 30 seconds of acoustic irradiation. Results indicate that ultrasonic energy induces greater and more uniform dispersion of one liquid in another in the presence of small amounts of chemi¬cal emulsifiers. When the emulsions were injected as a buffer slug before waterflooding, recovery of the oil-in-place was 8 to 22 percent greater than with conventional waterflooding in the test specimens, regardless of the con¬tinuous phase (oil or brine). The emulsions do not appear to be applicable to the Appalachian area; however, because the oilfields are too "tight," the clays in the formation remove the emulsifier from the displacing fluid, and not enough additional oil is produced, compared with recovery using conventional waterflooding, to warrant the increased operating costs.

Jan 1, 1969

By H. Margolin, E. Ence

Two versions of the Ti-Mn binary diagram have been published recently.' , -0th diagrams show two compounds in the region between 40 and 70 wt pct Mn, but disagree as to the reaction in which these compounds are involved. The investigation of the manganese-rich portion of the Ti-Mn binary diagram was undertaken at New York University as part of an investigation of ternary systems with titanium and manganese in order to determine which of the proposed diagrams is correct. A number of alloys between 31 and 70 pct Mn were prepared in a manner similar to that described by Cadoff and Nielsen; except that low currents (110 amp in argon atmosphere) and long melting times (up to 20 min) were used to prepare the alloys. Compositions were determined from weight-loss data, assuming all loss as due to manganese. Heat treatments were carried out with relatively large pieces, since there was a tendency for manganese to be lost during heat treatment. When X-ray diffraction data was to be obtained, the central parts of heat-treated specimens were used to make filings or powders which were not heat treated. Specimens were heat treated from the as-cast state. Heat-treatment times were as follows: 1150°C, 1 day; ll00°C, 2 days; 1000°C, 5 days; and 900°C, 15 days. It should be noted that equilibrium was not attained at 900°, 1000°, and in one case, at 1150°C. Metallographic specimens were electrolytically polished and strain etched by a technique described elsewhere.' At least four, and possibly six, phases were found in the region investigated. On the basis of information available at this time, a completely self-consistent diagram cannot be constructed, and therefore data are presented only for those phases which have been identified by both X-ray and microstruc-ture. Of the compounds detected, the one highest in manganese is the Laves phase, TiMn,, which is hexagonal with a MgZn, type of structure.V he diffraction data for TiMn2 from a 70 pct Mn alloy annealed at 1150°C are shown in Table I. The c/a ratio and parameters of TiMn2 agree well with those of Wall-baum hnd Rostoker et al. The values obtained here are c/a = 1.641, a = 4.825A. Another compound is the y-phase which is estimated to contain about 60 pct Mn. The y-phase has a structure which is identical to that of TiMn, with c/a = 1.639, a = 4.906Å. The fact that y has a Laves-type lattice would suggest that TiMn, has a range of solubility which extends from the composition of TiMn2 (69.6 Mn) to that of y (60 pct Mn). However, this could not account for microstructures which, in the 60 to 70 pct Mn region, show several phases in both the as-cast state and after annealing at 1150°C. Fig. 1 shows a two-phase structure of a 60 pct Mn alloy annealed at 1150°C. The phases present are y (white) and e (dark). If y were TiMn, then, according to Rostoker et al.,' the second phase of Fig. 1 should be P-Ti. The diffraction data for the 60 pct Mn alloy of Fig. 1 are shown in Table I. The starred d-values are from the e-phase and these lines do not correspond to those of &Ti. Comparison of as-cast and 1150°C microstructures of the 60 pct Mn alloy indicates that e precipitated from y. Since y has a

Jan 1, 1955

By G. Krauss, J. M. Thompson, H. Y. Kumagai

Boron-doped p-type and arsenic-doped n-type source materials were used to deposit thin silicon films on amorphous fused quartz substrates by cathodic sputtering in argon atmospheres. All as-sputtered films were found to have high electrical resistivities of about 104 ohm-cm, despite controlled variation of the substrate temperature from 50O to 400°C. The high resistivity of the n-type films persisted even after postdeposition heat treatments as high as 1000°C, while p-type films showed a sharp decrease in re-sistivity to values on the order of 1 ohm-cm or lower after heat treatments above 650°C. X-ray and electron diffraction, together with transmission electron microscopy of the p-type films, revealed that the improved electrical properties resulted from two distinct processes. A primary crystallization or recovery within the pains, which were approximately 200Å diam in the as-sputtered films, accompanied the initial sharp drop in resistivity at 650°C. Following this process, a secondary recrystallization or discontinuous grain growth was nucleated in films heated at 1000°C. The resulting significantly increased size of certain grains and the corresponding decrease in grain boundary area accompanied an additional decrease in resistivity after heat treatment at 1000°C. The properties of thin silicon films are of interest because of their possible application in device technology. Although evaporated silicon films on amorphous substrates1-3 and both sputtered and evaporated germanium films4-' have been studied in some detail, sputtered silicon films have not been widely investigated. It has been observed that evaporated silicon films deposited at substrate temperatures below approximately 600°C are amorphous.1,3,9,10 At substrate temperatures higher than this, the films are polycrys-talline, sometimes exhibiting a fiber texture with the fiber axis normal to the substrate surface.' Similar results have been obtained with germanium films, although in this case the substrate temperature for the amorphous to crystalline transformation is reported to be as low as 150OC.5 The mechanism of film deposition by cathodic sputtering differs markedly from that of thermal evaporation. It might be expected, therefore, that the properties of sputtered and evaporated silicon films would also differ. The purpose of our study was to determine the effects of deposition conditions and heat treatments on the electrical resistivity, structure, and composition of thin silicon films sputtered on fused quartz substrates. EXPERIMENTAL DETAILS Apparatus. A schematic diagram of the sputtering apparatus is shown in Fig. 1. The vacuum chamber was enclosed by an 18-in.-diam by 12-in.-high Pyrex bell jar mounted on a stainless-steel base plate. Access holes in the base plate were used to supply argon gas to the chamber, to allow for various electrical feedthroughs, and to provide mechanical motion to the shutter between the source material and substrate. The chamber was evacuated by a pumping system consisting of a 720 liter per sec oil diffusion pump backed by a 13 cu ft per min mechanical pump. Ultimate pressures of less than 1 x 10-6 torr could be achieved. The substrates were securely mounted on the stainless-steel substrate holder by quartz tabs held in place by stainless-steel screws. Temperatures of the substrate holder were measured by a thermocouple inserted within the holder. A quartz lamp was used to heat the holder and temperatures as high as 420°C could be maintained. Deposition Conditions and Procedure. The substrates used were polished fused quartz slides 116 by 1-12 by 3 in. and were outgassed at 200°C for 1 hr at a pressure less than 1 x 10-5 torr before film deposition. This was followed by a presputtering period of 2 hr during which the movable stainless-steel shutter was so positioned that deposition on the substrate was prevented. At a sputtering voltage of 5000 v dc and an argon pressure of 0.03 torr, the cathode cur-

Jan 1, 1967