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By Manuel Valerio Ortega

This Mexican amalgamation-process, invented in 1557, at Pachuca, by Bartolome de Medina, has been widely discussed in America and Europe, but thus far there is no universal agreement as to all the chemical reactions involved. Having been, after many trials, the first to succeed in effecting the amalgamation of silver-ores by the same mechanical means, but doing without one of the chemical substances which had been considered indispensable in the practice of 300 Sears, I am led to offer these notes as a contribution to the discovery of an exact theory concerning the patio process. My treatment for silver- and gold-ores being protected by letters-patent in this country, the United States, France, Peru, Bolivia and Chile, I may speak freely concerning its materials and manipulation. I. Patio-Amalgamation. The ore extracted from the mine is sorted by pepenadores, who break the large pieces with hammers, rejecting those which contain no ore, set aside the very rich to be smelted, and deliver the rest to be crushed and pulverized for direct amalgamation in the patio. The broken lumps, of about fist-size, are first ground in Chilean mills, and then reduced, in arrastras or tahonas, to fine slime. After the lama or slime has acquired a suitable consistency by the evaporation, through the sun's heat, of a part of the water which it contained, it is spread upon the patio or amalgamating-floor, where it is mixed with 5 or 6 per cent. of common salt. The next day a certain amount (depending upon

Jan 1, 1902

By Robert F. Conley

Attrition milling, once employed exclusively for the dispersion of pigments, has in recent years found a host of new applications in the area of mineral processing and mineral-pigment production. Broadly categorized, attrition milling is divided into two classes, as defined by the machinery's function, vibratory milling and rotational milling. Each mill type has been defined as a variation on ball milling and the terms, "vibratory ball mill" and stirred ball mill" appear in the literature. The primary design differences between attrition and ball mills are: (1) a stationary canister (or shell) (2) smaller grinding media (3) grinder energy is motor limited rather than gravity limited (4) strong media/feed size dependance.

Jan 1, 1983

By James E. Harding

AT just about the geographical center of the peninsula of Lower California is the El Arco gold mine. It is small and spotty, and three separate attempts to operate it in the past have failed. The only reason the present operation is possible is because of the higher price of gold and because the previous operators had spent about $300,000 developing the property with shafts, four levels, machinery, and a complete mill, all of which was acquired at a bargain price. All the known ore in the mine, to say nothing of the cost of recovering it, is

Jan 1, 1937

By Chas. F. Jackson

The work of the mining division is divided between seven sections, each in charge of a supervising engineer, as follows: 1. Metal-mining methods section, the supervising engineer of which is also supervising engineer of the Southwest Experiment Station at Tucson, Ariz. 2. Metal-mining research section. 3. Nonmetal minim section. 4. Coal-mining section. 5. Mine-ventilation section. 6. Mineral-industries survey section. 7. Electrical section. The names of the sections indicate broadly the fields covered by each, and in the following pages the objectives and type of work of each section will be summarized briefly and the active problems listed. The work done during the calendar year 1936 will also be summarized.

Jan 1, 1937

By Karl Christopherson, Vanessa de Viterbo

Trim blasting is an integral part of the mining processes at the Morenci Mine, a Freeport-McMoRan Copper & Gold Inc. property. Trim blasting near high-walls or Finals blasting requires a tighter distribution of energy but a reduction in total energy factor near the wall. Recent Finals blasting in Morenci Mine was allowing the shovel to dig to the final design limit, but causing high-wall instability due to excessive energy or production of energy (blast design and timing). Slope instability events reduced production in two of the three operating pits in Morenci over 2009. In order to avoid high-wall instability from Finals blasting, a new method was required. The new method utilizes air-decks, unconventional row timing, and blast design based on the geology predicted. Many different geologic structures and rock types exist in Morenci, and different strategies were needed for the many predicted geologies. Drill penetration rate and core mapping were the primary tools for determining the blast design. Patterns were designed within a consistent geology; with weaker rock types receiving a lighter load than the stronger rock types. Penetration rate returned by the drill would be the determining factor on the actual rock hardness. Maintaining the pattern geometry on Finals designs should not be an issue as long as the lb/hole is adjusted to reduce powder factor close to the high-wall. One requirement of Finals blasting should be that the powder factor matches the geology as closely as possible. A softer, fractured zone should use approximately one-half to two-thirds the explosive charge of a competent, sound geological zone. This has been incorporated into the final Trim blast design. It is impossible to protect every high-wall from close-in blasting, especially those with crossing prominent joint sets inclined toward wedge failure, but this new design has provided protection on walls where the mine was encountering problems.

Jan 1, 2011

By Beatriz Dogliani, Elisabeth Williams, Maria Berenice Sandobal, Carina Bertino

The environmental management of steel mill slag should be understood as a management philosophy, observing technical, economic and environmental criteria associated with their generation, storage and final destination. The slag can be considered as a synthetic mineral resource and become a very useful co-product in different areas. The Argentinean steel industry prioritizes the efficient environmental management of its waste, thus contributing to its own survival taking into account the sustainable development. In the world, the slag produced by the steel industry has been used as steel aggregate for road bases, railway ballast and filling material among others. Any factor that influences the economy of the country affects all branches of society, mainly public agencies, whose financial resources are increasingly scarce to deal with all public works. It is necessary to join efforts of private and public initiative in the adoption of alternative materials that replace the use of finite natural resources. This presentation aims to show the work done by private companies together with public bodies and universities to obtain a regulatory document for the management of slag as steel aggregates for three different uses, namely: road use, railway use and general use.

Nov 5, 2019

By D. Perednis

Fuel cells with thin samaria-doped ceria (SDC) electrolyte films deposited onto an anode support using spray pyrolysis were fabricated. The SDC films were deposited onto porous NiO-YSZ substrates at deposition temperatures between 400°C and 450°C. The influence of process parameters such as deposition temperature, flow rate, type of salt and salt concentration on the quality of the film was studied. A smooth dense film was successfully deposited using the precursor cerium ammonium nitrate and samarium nitrate dissolved in butyl carbitol (33.3 vol.%), 2-methoxy-l-propanol (33.3 vol.%), and ethanol (33.3 vol.%) solvent mixture. A deposition rate of 125 nm/h was achieved.

Jan 1, 2005

By J. L. van Niekerk, J. Gunaselvam

This study investigates the use of appropriate seating systems for the control of whole-body vibration exposure in vehicles used in the SA mining industry. Six suspension seats were tested with six test subjects to determine the most suitable seat for an articulated dump truck based on the EM1 requirement in ISO 7096 (2000) standards. Transmissibility functions were measured in the laboratory using the newly commissioned Dynamic Seat Testing Facility with two excitation levels of 1m/s2 and 2 m/s2 r.m.s. in the 0.5 - 30 Hz frequency range. SEAT values were calculated for two input spectrums, the EM1 input spectrum specified as in ISO 7096:2000 and measured road vibration data measured on a typical articulated dump truck. The averaged SEAT value calculations indicated that not one of the seats will qualify as an ISO 7096 (2000) suspension seat but that it is possible to select a seat that will significantly reduce the vibration the driver will be exposed to.

Jan 1, 2003

By A. F. Agnew

Discussion by A.E Agnew Strachan's paper summarizes a wealth of data on water-storage dam "incidents" published by USCOLD and ASCE in 1988, together with a review of tailings-dam incidents published by USCOLD in 1994. The data is summarized by text and 11 histograms. The histograms present a useful compilation of these data, although the patterns within the histogram blocks did not survive the Mining Engineering printing process - so their usefulness is impaired. Unfortunately, the text discussion is too cursory and does not highlight the significant relationships among the various causes of the incidents. Four paragraphs of text and Fig. 1 were devoted to water-storage dams, but the discussion is too sketchy, and Fig. 1 is unclear. Important statistics that could be uncovered are: •the total number of dam incidents tabulated were 500+, •earth embankments constituted 73% of those in operation and •incidents related to earth embankments were 75%, of which dam failures accounted for 24%, major repairs accounted for 42% and accidents accounted for 34%. Strachan concluded that "the majority of the dam failures are associated with overtopping (p. 49), and that the majority of incidents are associated with spillway and other facility structures" - although this is difficult to discern from Fig. 1. Confusion regarding Strachan's use of the terms "dam failures" and "incidents" is compounded by his use of "failures" and "accidents" in one paragraph of his Introduction section followed by his use of "incidents" in the next paragraph. Getting to the meat of Strachan's important paper, the tailings-dam incident survey (USCOLD, 1994), the connection between Figs 2 through 11 seems obscure. First, in the four paragraphs of introductory material, one learns that "incidents consisted of failures, accidents, seepage and other incidents of performance that did not meet design criteria" (p. 50). One does learn the helpful caveat that "structures not related to mill tailings were not included in the review" - so that the Buffalo Creek (West Virginia in 1972) and Aberfan (Wales in 1966) coal-mine failures, together with the ongoing metal-mine remediation work at Summitville (Colorado) do not muddy the waters of his paper. The all-too-brief discussion of the data shown in Figs. 3 through 11 (185 dams in USCOLD plus 26 dams in UNEP) reveals the following: •Figure 3: 57% of the incidents (failures and accidents) occurred with dams less than 20-m (66-ft) in height. •Figure 4: 63% of the incidents were due to failures alone (subset of Fig. 3). •Figure 5: Active dams had 82% of the accidents and 93% of the failures. •Figure 6: Types of dams (upstream, water-retention, downstream, centerline and "unknown") separated according to incidents. •Figure 7: Breaks out the incidents in Fig. 6 by failures, accidents and ground water. •Figure 8: Breaks out incidents by type (overtopping, slope stability, earthquake, foundation, seepage, structural, erosion, mine subsidence and "unknown"). •Figure 9: Separates Fig. 8 data into active and inactive dams. •Figure 10: Separates Fig. 9 data into failures and accidents. •Figure 11: Same as Fig. 8, but broken out by tailings-dam type (Fig. 6). Figures 6 and 7 show that most of the failures are associated with upstream or "unknown" types. Figure 9 shows that the leading causes of incidents for active dams

Jan 1, 2003

By J. O. Marsden, M. M. Botz

"Heap leaching is responsible for approximately 21 percent — 3.9 million metric tonnes — of copper production and 9 percent — 270 metric tonnes or 8.7 million ounces — of gold production worldwide. Given metal price assumptions of $2.25/lb for copper and $1,250/oz for gold, these portions of global production generate revenues of $19 billion and $11 billion, respectively. For heap leaching operations, small changes in metal extraction efficiency drive substantial changes in operating cash flow margins and affect project viability. Variances in actual metal production from budgetary forecast estimates can mean the difference between success (value creation) and failure (value destruction) for a heap leach project. Despite the importance of heap leaching for copper, gold and silver production worldwide, there are no clear standards or guidelines for developing heap leach metal production forecasts. There is considerable variation among copper and gold producers that apply heap leaching technology as to how such modeling and forecasting is applied at the operational level. There are a variety of different modeling approaches that can be utilized for this purpose. However, these vary in cost, complexity, time to implement, accuracy and credibility. This paper explores the options available for heap leach modeling, discusses the advantages and disadvantages of each approach, and provides guidelines/recommendations for an effective approach to modeling metal production at existing or planned heap leach operations. The paper also provides expected ranges of variation between actual and modeled production.Introduction and backgroundHeap leaching is fundamentally different from other methods used in the processing and extraction of gold, silver, and copper and other base metals. Considered globally, the technique represents a relatively modest portion of production compared with the primary technologies applied for copper and gold recovery. Approximately 21 percent of copper production is attributable to heap leaching techniques, as opposed to 79 percent by conventional crushing, milling, flotation, smelting and refining. For gold, about 9 percent of global production is obtained from heap leaching, compared with over 90 percent by various combinations of crushing, milling, gravity concentration, flotation and/or agitated cyanide leaching processes or, in the case of placer deposits, by direct gravity concentration and/or amalgamation. In cases where heap leaching is the primary source of metal production, the ability to accurately forecast metal production may be the difference between commercial success and failure for a project or operation. Heap leaching — of crushed or run-of-mine ore — is also commonly applied as a secondary process to treat lower-grade ores from a given deposit, such as at Chuquicamata in Chile, Cerro Verde in Peru and Bagdad in Arizona for copper extraction and at Twin Creeks and Carlin, both in Nevada, for gold. In such cases, heap leaching provides incremental revenue to supplement the primary process. Variances between actual and forecast metal production from heap leaching as a secondary process are typically tolerated and absorbed within the overall site metallurgical balance. In either case, accurate production modeling and forecasting creates significant value for heap leaching projects, is essential for managing production expectations — timing and volumes — and is likely to be a critical success factor for most heap leach projects."

Jan 1, 2017

By Sandra Penttinen

To assist blasting professionals with the creation, documentation, and appropriate methodology to standardize the data collection of the pre and post blast investigation process. Penttinen Associates will present a logical non-technical presentation focusing on: Why pre-blast surveys SAVE How to prepare for pre-blast inspections What to do in preparation of pre-blast inspections The creation of an industry standard all-inclusive pre-blast document Establishing pre-blast inspection operational standards Preserving the data.

Jan 1, 2001

By J. D. T. Steyl

Anglo American Corporation and the University of British Columbia have developed a medium-temperature oxygen pressure leaching process for the extraction of copper from chalcopyrite concentrates in an acid-sulphate system (AAC/UBC process). Leaching is performed at 150°C and surfactants are added to disperse molten elemental sulphur from the unreacted sulphide surface to prevent liquid sulphur occlusion. Copper extractions of over 95% and elemental sulphur yields of around 60% were observed over a 2-hour average residence time in a continuous pilot autoclave. Sporadic blockages occurring under continuous conditions were found to be caused by the accumulation of molten elemental sulphur mixed with unreacted sulphide mineral. A batch programme of experimentation was undertaken to establish the reason for this phenomenon. Batch experiments were conducted at low pulp densities on concentrate samples with narrow size distributions and at similar solution compositions to those experienced in the pilot autoclave. The overall rate of chalcopyrite oxidation was shown, under approximately constant solution composition, to be a strong function of the total available mineral surface area. Initial copper extraction rates followed the shrinking particle kinetic model under intrinsic surface control. Deviation from shrinking particle kinetics was however observed after a certain oxidation time. Secondary electron images identified small (typically less than 20 µm) sulphur conglomerates at the point of deviation, which 'collected' unreacted chalcopyrite mineral particles and lowered the total mineral surface area available for oxidation. These sulphur clusters are thought to be the precursor for blockages experienced in the continuous pilot autoclave. These results emphasised the importance of fine grinding (P80 5-20 µm) and suggest that shorter residence times may minimise the formation of sulphur conglomerates in a continuous autoclave operating at medium temperature.

Jan 1, 2004

By E. C. Skinner

Cardox, which consists essentially of a steel tube containing carbon dioxide compressed to the liquid state, is a trade name designating a device used principally in coal mines to break down coal. The use of Cardox to break down coal was developed in the Middle Western coal fields around 1927 or 1928. At first, a large, heavy tube was used, requiring many parts. Through experimentation and technologic improvement, the weight of the tube has been brought down from 88 lb. to 20 lb. and the new, light tube makes use of larger volumes of CO2 at lower pressures than formerly was thought possible. This blasting method is extensively used today in coal mines and probably one tenth of the bituminous coal produced in the United States is prepared with Cardox. Construction and Application As used in the coal mine, Cardox looks like a piece of steel pipe 2 to 3 in. in diameter and 3 to 5 ft. long. When it is necessary to fire a shot, the tube is wired with two leg wires that are long enough so that when the tube is pushed the desired distance into the hole the wires will protrude 5 to 6 in. It has been found that No. 18 insulated copper annunciator wire is the best material for leg wires. A two-conductor rubber-covered shot-firing cable of sufficient length is then attached to the leg wires. A 2 to 6-volt current is applied, either by means of shot-firing batteries or the standard type of shot-firing generator. Upon the application of the current, the charge in the cartridge is set off. Because the breaking action upon the coal is supplied by the relatively slow physical expansion of the carbon dioxide gas rather than by the rapid chemical formation of gases as in more familiar explosives, the result is a slow heaving action, somewhat similar to that produced by black powder, rather than a shap detonating effect. Permissible powder does its work at roughly ten times the pressures in use with Cardox. The escaped gas from a Cardox shot apparently works along the planes of weakness in the coal face, such as the coal cleats, the edges of the cut, and along the top of the seam, breaking off the coal toward the free faces and heaving the mass of coal outward. Cardox tubes are manufactured in various sizes to take care of variable conditions of seam size, undercut depth, cleatage, coal hardness, and so forth. The tubes range in diameter from 2 to 3 in. (Table I) and the normal CO2 charge is from 24 to 96 oz. For any one tube size, several sizes of shear disks are available, thus excellent control of the type of shooting desired is possible. In general, local experience and experimentation dictate the size of tube chosen for any particular job. For high coal, and deeper or wider cuts, a larger size is chosen to start with, and the opposite is true for low coal, softer coal, or small cuts. After the tube size has been experimentally selected, tests are run in the mine to determine how many shot holes are needed and where the holes should be placed. The size of the disk,

Jan 1, 1944

By E. C. Skinner

Cardox, which consists essentially of a steel tube containing carbon dioxide compressed to the liquid state, is a trade name designating a device used principally in coal mines to break down coal. The use of Cardox to break down coal was developed in the Middle Western coal fields around 1927 or 1928. At first, a large, heavy tube was used, requiring many parts. Through experimentation and technologic improvement, the weight of the tube has been brought down from 88 lb. to 20 lb. and the new, light tube makes use of larger volumes of CO2 at lower pressures than formerly was thought possible. This blasting method is extensively used today in coal mines and probably one tenth of the bituminous coal produced in the United States is prepared with Cardox. Construction and Application As used in the coal mine, Cardox looks like a piece of steel pipe 2 to 3 in. in diameter and 3 to 5 ft. long. When it is necessary to fire a shot, the tube is wired with two leg wires that are long enough so that when the tube is pushed the desired distance into the hole the wires will protrude 5 to 6 in. It has been found that No. 18 insulated copper annunciator wire is the best material for leg wires. A two-conductor rubber-covered shot-firing cable of sufficient length is then attached to the leg wires. A 2 to 6-volt current is applied, either by means of shot-firing batteries or the standard type of shot-firing generator. Upon the application of the current, the charge in the cartridge is set off. Because the breaking action upon the coal is supplied by the relatively slow physical expansion of the carbon dioxide gas rather than by the rapid chemical formation of gases as in more familiar explosives, the result is a slow heaving action, somewhat similar to that produced by black powder, rather than a shap detonating effect. Permissible powder does its work at roughly ten times the pressures in use with Cardox. The escaped gas from a Cardox shot apparently works along the planes of weakness in the coal face, such as the coal cleats, the edges of the cut, and along the top of the seam, breaking off the coal toward the free faces and heaving the mass of coal outward. Cardox tubes are manufactured in various sizes to take care of variable conditions of seam size, undercut depth, cleatage, coal hardness, and so forth. The tubes range in diameter from 2 to 3 in. (Table I) and the normal CO2 charge is from 24 to 96 oz. For any one tube size, several sizes of shear disks are available, thus excellent control of the type of shooting desired is possible. In general, local experience and experimentation dictate the size of tube chosen for any particular job. For high coal, and deeper or wider cuts, a larger size is chosen to start with, and the opposite is true for low coal, softer coal, or small cuts. After the tube size has been experimentally selected, tests are run in the mine to determine how many shot holes are needed and where the holes should be placed. The size of the disk,

Jan 1, 1944

By Joram M. Amir, Ernst Niederleithinger, Nikolaus Schneider

"Abstract: Diaphragm walls are used to provide a stable and watertight confinement for the construction of tunnels, underground railway stations, deep basements and other structures requiring deep excavations. Water seepage and soil loss through the joints have occurred on several occasions, causing extensive damage. This may have been due to uncontrolled concrete flow between the joints, unexpected geologic conditions or just poor workmanship.Different ways of quality assurance are applied on construction sites. Most of them rely on recording parameters of the construction equipment and conventional concrete quality control. In the frame of the EUREKA/ZIM project DiWaQ we have looked at several ways to perform non-destructive quality control. Some methods are to be applied after excavation before concreting (phase 1); others after the wall is completed (phase 2).For phase 1 we have used two different principles for checking the shape of the excavation, especially the joint to existing panels. A mechanical device which can be adapted to the excavating equipment was developed; field tested and validated on test and construction sites. It is described in detail in another paper in the same volume. A sonar-based device with a 10 mm resolution has shown good performance in the lab, but is still under development.For phase 2 different temperature sensors have been lowered into access holes to monitor the hydration heat developed during concrete curing. The same tubes can also be used to perform electromagnetic and ultrasonic crosshole measurements across or along joints to detect flaws. Especially the ultrasonic method has shown promising results on validation specimen at the BAM test site at Horstwalde, but limitations as well. Success substantially depended on the joint type, flaw size and distance of the sensors to the joint."

Jan 1, 2014

By M. L. Jeremic

Altered and unaltered coal from the Star-Key Mine near Edmonton, Alberta has been tested under compression and under tension. The test results showed that altered coal samples have an appreciably lower strength than unaltered coal. Altered coal samples do not give a linear load-displacement curve, peak strengths are poorly defined and yielding is observed over a range of loads, so the material can be regarded as relatively plastic. However, unaltered coal samples produce a linear loading curve with a high tangential modulus and an easily distinguished peak strength at which there is a sudden brittle failure. These findings lead to important differences in the theoretical design of ribs and pillars in underground mines in the two coal types. The substantial differences in the strength properties and behaviour of the two types of coal are governed by a higher intensity of cracks in the weathered coal. Two causes of the additional cracking can be suggested-subaerial weathering and subterranean weathering of the coal.

Jan 1, 1979

What is the best circuit to comminute primary crusher product to make beneficiation feed? Finding the best circuit to crush and grind minerals to beneficiation sizes is a complex problem that can lead to interminable discussion. Conclusions reached can be questioned. This will continue as long as the technology of comminution continues to expand, and is a mixture of many technical and economic factors in what is not a precise science. Laboratory and pilot plant procedures now exist that can help process engineers make sound decisions on which circuits are the best for crushing and grinding the specific ore being studied. It is the aim of this paper to discuss such procedures so a better under- standing of key decision parameters is avail- able, and to update comminution testing which has seen a. period of change in which new procedures have been introduced.

Jan 1, 1978

By L. Leibowitz, M. G. Chasanov, L. W. Mishler

A drop calorimeter system is described for use in measuring enthalpies to 3600°K. Data are presented for tungsten between 2800" and 3600°K. The enthalpy of tungsten in cal per mole between 2000° and 3600°K can be represented by the equation HºT- Hº298 = - 1.7622 X 103 + 5.7772T + 8.9861 where T is in degrees Kelvin. A tabulation of com -puted values is presented for heat capacity, entropy, and free energy function. A drop calorimeter has been constructed to carry out enthalpy measurements at temperatures to 3600°K. Samples are heated by induction1 and dropped into a commercial adiabatic calorimeter, modified for this purpose. The experimental temperature is limited by the melting point of container materials and compatibility of the container and its contents. Several high-temperature drop calorimeters have been described in the literature1-5 but none has been used at temperatures as high as those in the present work; our measurements of the enthalpy of tungsten range from 2800" to 3600°K. DESCRIPTION OF EQUIPMENT An overall schematic view of the equipment is shown in Fig. 1. Power for the induction coil is supplied by a 25-kw 250 kHz Ther-Monic generator coupled to an iron core RF transformer. The Sample capsule is suspended in the work coil by 10-mil diam tungsten wires which are wrapped around a horizontal 5-mil diam tungsten wire. The horizontal suspension wire is clamped between two massive copper electrodes which are fixed in an x-y motion device that allows adjustment of the position of the heated capsule from outside the vacuum chamber. The copper electrodes are connected by flexible copper straps to a 1250-joule (5 kv, 100 pfarad) condenser bank. When it is desired to release the capsule, the condensers are discharged through the horizontal suspension wire causing it to vaporize rapidly. Very reliable and precise release of the capsule is achieved in this manner. Experiments have shown that no heat correction is required for this discharge energy. As part of the temperature measuring system, two prism holders have been incorporated in the apparatus. The upper prism holder is in the main vacuum chamber itself, whereas the lower one is in a side arm attached to the drop tube below the gate valve. The upper prism is mounted on a rotary vacuum feed-through, and may be moved under a protective shield when not in use. This prevents deposition of vapors on the prism surfaces when temperature measurements are not being made. Similarly, the lower prism is mounted on a push-pull vacuum feed-through, and when not in use may be pulled into its side tube. The prism mountings are fitted with guides and stops so that they may be moved precisely into the desired position. The aim throughout is to minimize the time the prisms are exposed to vapors from the hot samples. At the high temperatures reported in this paper, only the lower prism was used. The upper prism holder in these cases was fitted with an additional radiation shield. By using a prism and viewport, the lower surface of the samples can be observed by an optical pyrometer. The measurements discussed in this paper were obtained with a Leeds and Northrup 8622-C-S series manual pyrometer which is estimated to be accurate to 0.5 pct. Pyrometer calibrations and prism and window corrections were carried out in the conventional manner6 using tungsten strip lamps calibrated by the National Physical Laboratory, Teddington, England. Prism corrections were rechecked after each use. All work to date has been done in vacuum, and no measurable change has been observed in the prism correction below -2300°K for the upper prism and below -2800°K for the lower one. The total time of exposure of the prisms is about 50 sec per run. At high temperature, the final temperature reading is corrected by using the final A value for the prism; see Ref. 6 for details of this procedure. The calorimeter is a modified Parr Instrument Co. (Moline, lll.), Series 1230 adiabatic calorimeter with automatic jacket control. Other authors5 have used a similar calorimeter with good results. The calorimeter jacket cover and calorimeter cover are attached to the drop tube which contains a radiation shield. This shield is a gold-plated copper disc which can be operated manually from outside the calorimeter. The receiver is attached below the radiation shield and is lined with tungsten. In a typical experiment, the calorimeter and its jacket water temperatures were adjusted to 0.000°K temperature difference. The sample was allowed to equilibrate in the furnace at the desired temperature for about 20 min. The initial calorimeter temperature was then recorded, the sample dropped, and appropriate shutters closed. After about 3 min, the drop tube and receiver were filled with helium to 60 torr. The final calorimeter temperature was recorded after it had remained constant over a 5-min period. The equilibration time in the calorimeter was about 25 min. Thermistor probes are used to operate a hot and cold water supply system to maintain the jacket temperature equal to the calorimeter temperature. For actual measurements of the calorimeter temperatures, a quartz thermometer was used (Hewlett Packard Dymec Thermometer, Model #2801A). This thermome-

Jan 1, 1970

By J. M. Blank, V. A. Russell

When the nucleation of silicon on a sapphire substrate is accomplished by gradually decreasing the substrate temperature while subjecting it to a constant impingement rate of hydrogen and silicon tetrachloride, the resulting deposit is characterized by widely separated islands of silicon scattered over an "open sea" of sapphire. Analysis shows that nucleation takes place mainly on sites of large adsorption energy, about 85 kcal per mole, and small surface concentration, about 108 cm-2. Crystal growth proceeds rapidly on these nuclei and results in enough depletion of Sicl4 from the ambient gas to suppress further nucleation. The technological importance of single-crystal films on dielectric substrates has prompted considerable work on the deposition of silicon on sapphire. This paper is concerned with the deposition of silicon, by the reduction of silicon tetrachloride with hydrogen, onto heated sapphire substrates. The apparatus consisted of a temperature-controlled container for the silicon tetrachloride along with gas lines and flow meters necessary to convey a hydrogen-silicon tetrachloride mixture to a reaction chamber constructed of quartz tubing. Heat for the substrate was provided by means of an inductively heated graphite susceptor. The observations pertinent to the present discussion were made with an American Optical Co. high-temperature microscope which allowed us to make motion pictures of the deposition process at a magnification of approximately 50 times. Two main categories of experiments were carried out: one on determination of critical condensation temperatures and the other on the deposition of epitaxial silicon films on the sapphire substrates. Critical condensation temperatures were determined in the traditional way by raising the substrate temperature well above that at which condensation could be expected at the impingement rates being studied and then gradually lowering the temperature until the condensation of the first silicon was observed. This was done initially with ellipsometry-type detection but it was soon discovered that the deposits were occurring as widely separated islands and groups of islands scattered over an "open sea" of sapphire. We have called these archipelago formations. They were most easily detected by optical microscopy. Data gathered from experiments of this type have been collected in Table I. Motion pictures of the formation of archipelago patterns show that the nucleation period lasts about 10 sec if the substrate temperature and impingement rate are kept constant. Essentially all of the nuclei are formed in a few seconds and all subsequent silicon deposition merely adds to the size of the established nuclei. After an archipelago formation has matured at a given substrate temperature and impingement rate, it is very difficult to stimulate any further nucleation in the open space between islands. Lowering the substrate temperature will occasionally stimulate nucleation but increasing the impingement rate hardly ever produces any more new nuclei. It should also be emphasized that the nucleation rates appear to be very small, about 104 cm-2 sec-1. They will receive special attention in the analysis section. Another series of experiments was performed employing a systematic variation of substrate temperatures and impingement rates approximating those expected to produce epitaxy. Sapphire substrates with surfaces normal to the 2233 direction were used. In contrast to the procedure that produces archipelago patterns, these films were deposited by raising the substrate temperature to a desired value at which time the silicon tetrachloride and hydrogen flow was begun. Of course, these depositions produced mainly films that were continuous. After removal from the deposition chamber, the substrate and silicon film were examined microscopically to determine the nature of the deposit and by X-ray diffraction to determine the extent to which a single-crystal film had been achieved. Results of these experiments are summarized in Table 11. Of interest for the present analysis is the fact that epitaxy appears to be confined to a fairly narrow temperature range between about 1050" and 1150°C. This also will be discussed in the analysis section. ANALYSIS In this section we shall apply nucleation theory to the data presented above with the objective of testing

Jan 1, 1967

By AIME AIME

FOUK fields of activity are now recognized by the A.I.M.E. in its award of medals for conspicuous achievement: the Saunders medal for mining, the Douglas medal for non- ferrous metallurgy the Lucai medal for petroleum, and the Rand medal for distinguished achievement in the broad field of mining administration including the organization and development of enterprises in all branches of the mineral industry. This last is known officially as the Charles F. Rand Memorial Medal, and it award is made possible through funds supplied by the Charles F. Rand Foundation. Until this year money thus available was used for other special projects, so that the forthcoming presentation of the Rand medal to Robert C. Stanley is notable as being the first time that achievement in mining administration has been thus recognized.

Jan 1, 1940