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By Qingguo Xue, Jingsong Wang, Guang Wang, Yuanyuan Zhang

Due to complicated structure and composition of high-phosphorus iron ore, pure substances were used to simulate the chemical composition of high-phosphorus iron ore to study the reaction of fluorapatite at different temperatures and effect of additives. The gasification process of P during carbothermic reduction process was investigated using a quadrupole mass spectrometer gas analysis. It is found fluorapatite was reduced to phosphorus which diffused into iron and gas phase. From the gas analysis, it was observed that PO and P gas species were vaporized around 800 °C. As the reduction temperature increased, the diffusion of phosphorus into iron was enhanced. The presence of Ca(OH)2 as additives not only promoted the reduction of iron oxide, but also decreased the degree of fluorapatite reaction to inhibit P into iron.

Mar 1, 2018

By Gordon M. Matheson, David K. Miller

Possible impacts to the water quality and production capacity of ground water supply wells by blasting is a common cause of complaints for blasting contractors, mining companies, and local regulatory authorities. The major complaints of changes in well water quality include; turbidity, discolored water (red, brown, black, yellow and milky water), and nitrate and/or coliform contamination. The major complaints for changes in well water production capacity include: loss of quantity production, air in water and/or water lines, damage to pump, and damage to well screen or borehole.

Jan 1, 1997

By A. Warczokand

The cleaning of copper smelting slag requires magnetite and cuprous oxide reduction. The slag reduction with coke, injected coal powder or bunker oil is strongly endothermic and requires heat generation by fuel combustion or the use of electric energy. The reduction of fayalitic slag with calcium carbide is slightly exothermic and the formed calcium silicate modifies the slag. Thus, the additional energy is required only for covering furnace heat losses. Results of crucible scale tests showed the rate of slag reduction approximately five times higher in comparison of the slag reduction with coke under the same conditions. It seems that the effect of exothermic reaction and slag modification with CaO at the reaction interface results in very high rate of slag reduction. Industrial scale tests carried out in the Anglo-American Chagres Smelter demonstrated the possibilities of effective reduction and cleaning of the slags from a flash smelter and Peirce-Smith converters in a Teniente Slag Cleaning Furnace. The slag reduction was carried out without any reductant or stirring gas injection, simply by calcium carbide charging through a furnace mouth, and was very fast.

Jan 1, 2007

By AIME AIME

NEW YORKERS look forward to the third week of February as the time of the year when they can count on seeing their friends-from far and near gathered in the city for the four-day annual session of the Institute.., Indeed, the metropolitan district is so large that in engineer who lives in New, Jersey and has his office on the lower end of Manhattan island may easily pass a whole year without seeing an acquaintance who lives in Westchester and has an office near Forty-second Street. If the Institute served no other function than to provide a place where friendship may be renewed, ideas exchanged, and new acquaintances made it would still be worth while. But when about 30 technical sessions at which about 160 papers are read and discussed are compressed into four days the annual meeting is also entitled to high rank as an intensive course of post-graduate instruction in the newest development in mining and metallurgical technology. Last, but not least, it is the occasion of a good time for one and all, even if they do get more than a little behind on sleep before the end of the fourth day. Nine o'clock is the time set on Monday morning for the beginning of registration, but a half-hour before that a number have always 'put in an appearance, and this is fortunate, because by 10 o'clock four sessions had begun, those on mining methods, geophysics, a round table on the valuation of coal, and the session of the Local Section delegates. Three committees of the A. S. T. M. were also in simultaneous session, so the meeting may be fairly said to have started "in high."

Jan 1, 1931

By E. Buehler, R. H. Willens

A Hew melting technique has hem adapted to the rapid quenching of- alloys from the liquid state. The inelting method has no limitations on the alloys investigated for there is no reaction with crucible materials and the most refractory materials are easily melted. The vate of heating is so rapid that alloys which have a high vapor pressure constituent can be melted with a minimal loss in material. Several new superconductovs have been discoveved by vapid quenching of lolten alloys. THE rapid quenching of alloys from the liquid state has led to the discovery of many new metastable phases. The methods initially used were limited to alloys which did not react with crucible materials.1,2 There was also the unmentioned limitation in tem- perature. Alloys with melting points much greater than 2000°C could not be melted in the rapid-quench apparatus. Recently, there have been successful attempts to rapidly quench reactive alloys by Moss et at. and Matthias Moss et al. injected powdered material (325 mesh) into a high-temperature plasma and the high-velocity molten droplets impinged on a cooled copper plate. The technique innovated by Matthias was to melt the alloy in an arc furnace and splatter it against a copper plate by means of a high-velocity gas jet aimed at the melt. I) FAST COOLING APPARATUS The creation of a metastable phase in a given alloy system by rapid cooling from the melt is contingent on the quenching rate. Some alloys require very slow rates while other alloys require the ultimate in quenching rate. At the present time, the vertical-gun technique of Duwez and willens' has demonstrated, in practice, the highest quenching rates and thus the best

Jan 1, 1967

By Xiaoxu Sun, Jianchao Yao, Jiancheng He, Shijie Lu, Hongxi Zhou

"The ball mill performance relies on impact grinding, but it has disadvantage of the lower efficiency when the ore is finer; while tower mill relies on friction shear affection with high energy efficiency, which is considered to be one of the most potential fine grinding equipment all over the world. Generated by the agitator device, the internal media movement is complex because of comprehensive interaction of screw mechanism, cylinder structure and adjacent media, which is the key factor of grinding process. But the kinematics parameter ,such as speed, acceleration, stress and so on, of media motion cannot be obtained through traditional laboratory test method, which restricts deeply research on finer grinding mechanism seriously. In order to solve this problem, characteristics of media motion in tower mill is studied via the discrete element method. Coefficient of restitution, coefficient of static friction and coefficient of rolling friction are the key parameters affecting the media movement, which were calibrated by stacking angle test firstly. A 3kW tower mill is established as the model for simulation. At last one appropriate simulation strategy is selected to increase simulation accuracy. The characteristic of media motion is obtained based on the computer simulation analysis: macroscopically, the media in tower mill is a dynamic equilibrium state generally accompanied by spiral up and down movement all the time. And it has been found that the maximum lifting height is proportional to the rotation speed of agitator shaft. The velocity of media at the edge of screw stirrer is biggest, while the velocity of media near the cylinder wall is smaller, so the grinding performance between the two ring areas is the best. The rotational speed of agitator shaft and media filling ratio are the two most important operating parameters in tower mill. The impact curve of two main operating parameters on the grinding intensity and energy efficiency are obtained. All these can provide theoretical basis and technical support for operating parameters setting of industrial tower mill."

Jan 1, 2018

By V A. Maltsev, V I. Panin

The question of prediction and prevention of dynamic events û rock bursts (RB), tectonic rock burst (TRB) and mining-induced earthquakes (MIE), induced by large-scale mining, are discussed. The mine itself and the host geological environment are taken as a natural-technical system (NTS) whose evolution is characterised by alteration of the adaptation-bifurcation (catastrophes) periods. So, to predict TRB-MIE means to predict the limiting NTS states that are determined from the NTS geological monitoring data, and to prevent the said events means to control the processes of rock deformation and failure within the critical zone. The study considers particular examples of how TRB-MIE-events are predicted and prevented in apatite mines, Kola peninsula, Russia.

Jan 1, 2000

By Llewellyn A. Rubin

Under Bureau of Mines Contract H0122007, Telcom, Inc., with the assistance of Fenix & Scisson, Inc., conducted a 17-month research and development project aimed at provid¬ing a field-test model of a guidance system for use with the Bureau of Mines Probe Drill. The Probe Drill is a part of the Bureau's Mine Rescue System developed under Contract H0101262. Volume I of this report is subdivided into seven sections. Volume II consists of a number of supporting appendices. In addition, there were delivered under the Contract, a number of other documents which are referenced in the text. Section 1 deals with essential contract information, Program Background, and a general system description. Section 2 covers the project chronology in brief. Section 3 is a digest of design considerations and implementation related to the requirements of the Contract. Section 4 is a description of the System, including illustrations of the hardware, and software. Section 5 is devoted to Operation and Maintenance. Para. 5.1 describes step-by-step field assembly and disassembly of the downhole unit. Para. 5.2 covers Operation. Para. 5.3 covers various aspects of maintenance from the lowest field echelon possible. Higher level maintenance must be accomplished in the laboratory, for the present field-test model. Para. 5.4 covers system calibration. Para. 5.5 covers detailed step-by-step operational sequences. Section 6 covers the results of the field testing, post-test evaluation, and recommendations. Essentially, we conclude that the present hardware (field-test model) has proven every aspect of system performance, but failed to provide reliable assurance of an operationally ready system. Telcom, therefore, recommends a three-phase continuing effort devised to provide the operationally-ready model of the system.

Jan 1, 1973

By Lever R. R

The paper discusses assay methods generally used when prospecting for gold, and also the applicability of various chemical methods, it describes a new paper chromatographic technique.for making fairly rapid semi-quantitative assays for very fine gold. Testing of the method in field work shows that this simple method could have applications in geologic work, in prospecting and in certain routine mine sampling work. It is not yet a method that can be used to detect anomalies in traces of gold dispersed around an orebody, as is general practice in geochemical prospecting.INTRODUCTIONAccording to the English economist Harrod (1958), "the acute shortage of gold in the world-because currency value has not been adjusted in line with the fall in the goods value of the various currencies-has been a familiar fact for some time now". Harrod calculates that a rise in the price of gold to double its present value is necessary to rectify this condition, and that, if this rise were to take place, increase in production and reduction in private hoarding might well bring annual accretion to world stocks from the presentaverage of about $464 million to a figure close to the $2,000 million that would probably eiiminate these shortages.Any increase in the price of gold is bound to lead to a great increase in prospecting at working mines, in abandoned areas and possibly in untouched country. Prospecting, techniques for base metal orebodies have improved greatly in the last thirty years; but methods available to detect gold occurring without accessory metals have not received the same attention. With this in mind a paper chromatographic method of assaying for gold has been developed by Lever (1958). In the field this semi-quantitative method has proved...

Jan 1, 1959

By L. A. Weakly

The Viburnum ore trend is the largest, single known ore body of lead in the world. Four well-known mining companies operate in the trend, which is approximately 64 km (40 miles) long and up to 610 m (2,000 ft) wide, located some 121 km (75 miles) southwest of St. Louis, MO. Total production from the mines for 1979 was 33 kt/d (36,000 tons) of ore or 472 kt/a (520,350 tons) of lead and coproduct metal. The district is the number one producer of lead, providing 90% of the United States' output with its coproducts, zinc ranking second, and copper and silver both ranking sixth in total US output. Mining is done in a stratiform deposit approximately 305 m (1,000 ft) in depth with the host rock principally dolomite. Ore is mined in large open stopes by the method commonly referred to as room-and-pillar mining. Mining methods and equipment are fairly similar, with the mines classified as trackless, all mining equipment operates on rubber tires. This paper will present a description of the different methods and equipment used to move ore from the active heading underground to the ore shaft for hoisting to the surface. Basically, three methods are incorporated: front-end loader and truck haulage combination; front-end loader and truck, with main line track haulage combination; and front-end loader and truck, with conveyor haulage combination. The logistics of each system, such as method of use, equipment specifications, ore handling rate, and those cost figures that could be made public, will be included.

Jan 1, 1983

By Wenqiang Bao, Qijie Zhai, Ting Wang, Shaobo Zheng, Huigai Li

The type of inclusions with different sizes in as-cast low carbon steel strip which is deoxidized by Si–Mn has been characterized by scanning electron microscope (SEM) and transmission electron microscopy (TEM). SEM observation and analysis suggested that the type of inclusions larger than 1 μm is manganese silicate. TEM analysis was carried out to investigate the composition and structure of nano-inclusions. Inclusions with diameter about 100 nm are manganese silicate, MnS–Si(Mn)Ox complex particles and isolated cubic Al2O3. Furthermore, HREM observations have revealed that there were two kinds of ultrafine particles in size range of 5–10 nm. One is spherical monoclinic Cu2S; the other is silicon-iron oxide particles with morphology of long strip. In addition, some thermodynamic calculations were performed to explain the corresponding relation between the type of inclusions and their size.

Mar 1, 2017

By S. H. Lorain

Shortly after the Strategic Minerals Act of 1939 we passed by Congress, the Bureau of Mines was authorized to begin a program of investigation of domestic sources of strategic minerals. Since World War I, the Philipsburg district had been virtually the only one in the United States that was producing manganese on a commercial scale. Consequently, the district was among the first to he investigated. During the summer of 1939, the Geological Survey mapped the geology and ore deposits of the district. In late July 1939 the writer examined the district for the Bureau of Mines. On the basis of this examination and of the work performed by the Geological Survey, the Bureau of Mines diamond-drilled at several properties in the district during the summer of 1940. This report reviews the mining history and geology of the district, and presents the factual data obtained by diamond drilling.

Jan 1, 1950

IT is customary to make an alloy of copper in the same way, not to increase its quantity as with gold or silver, but to corrupt it for the art of casting and to destroy a certain natural viscosity in it. For this result it is accompanied by tin and also, sometimes, brass. But its proper and true alloy is fine tin, except, however, when you wish to make hammered works. For these, copper must be pure and without any trace [of impurity], otherwise it cannot be hammered thin, gilded in the fire, drawn into a wire, or made into vessels for use as is customary; but in casting, tin is almost essential. When you come to this association, just as it changes nature and appearance according to the proportion of tin which you give it, so it changes name and is no longer called copper but bronze, or, for a greater distinction of the quantity of tin for every hundred or more of copper, it is called by skilled workmen metal of more or less fineness as it contains more or less tin. This is recognized by the whiteness and brittleness: changing from red, which is the color of copper, it becomes white; from soft and flexible it becomes hard and brittle as glass. This admixture removes it so far from its original nature that one who does not know that it is a compound material believes it to be one of the number of metals engendered by Nature. Now, so that you may understand well, I tell you that various kinds of this are made, all according to the proportions of the quantities and according to the kind of work. For one kind of bronze is desired by those who make statues; this is not desired by those who make artillery or by those who make bells, mortars, basins, and similar cast objects. Now in order to alloy it into the species of bronze, eight, nine, ten, up to twelve pounds of tin are put with every hundred pounds of copper. Those who want it to make bells put twenty-three, twenty-four, twenty-five, and twenty-six, depending on the tone, on whether they are large or small in form, and on whether they wish to make the tone deep or sharp and clear. From twelve upwards is used for all other works that need it, either for hardness or to give them fluidity in casting by surpassing the degree of

Jan 1, 1942

By Steve Colbum

LTl’s MapStar LPS (laser positioning system) utilize both tripod mounted and hand held reflectorless distance meters. These are eye safe, easy-to-use, and specifically designed to endure the harsh environment characteristic to the mining, quarry and explosives industries. Survey data collected by the systems is digitally stored in a ruggedized data collector and then processed with a specialized, interactive software program, which can be run on any standard PC. Win Prof, the Windows-based analytical software package is used to reduce the data for generating bench face profiles, surfaces, volumes, estimating true burdens and mining ratio calculations. In addition, the software has many other built-in routines to calculate powder factors, toe shear, to map structural contacts and to predict the flyrock potential based on the Burden to Energy ratios. An extensive, built-in library of explosive’s data facilitates these calculations. It will also conform automatically to user-specified minimum and/or maximum burden in relation to the explosive energy, hole diameter and bench geometry - for both vertical and inclined holes. Numerical data can be represented in 2D or 3D to emphasize the hole-burden-face relationships.In this workshop, the MapStar LPS instruments and Win Prof analytical software will be thoroughly demonstrated. Demonstrations include equipment configuration, typical field setups and several effective survey procedures, including processing of some sample data.

Jan 1, 2000

By J. P. Murphy, T. E. Leontis

DURING the last few years, the trend in the aircraft and automotive industries has been toward higher and higher operating engine temperatures. This has created considerable interest in the effect of temperature on the properties of alloys. In the magnesium field, it has been recognized for many years that the addition of cerium imparts high strength and good resistance to creep at elevated temperatures. Beck,1 in his treatise on-magnesium, has summarized the work of German investigators. This includes the unpublished data of Menking, showing the increase in strength and hardness of extruded alloys containing 2 to 20 per cent Ce at temperatures from 200 to 300°C. (68° to 572°F.) and the results of Vosskühler, who demonstrated the improved resistance to creep of alloys containing 6 per cent Ce plus 2 per cent Mn and 0.5 per cent Ce plus 2 per cent Mn at 150°C. (302°F.). Wellinger and Keil2 have also reported the creep properties of a forged magnesium-cerium-manganese alloy at 200° and 250°C. (392° and 482°F.). Haughton and Prytherch have determined the tensile properties of various forged magnesium alloys containing cerium, cerium plus manganese, cerium plus calcium, cerium plus nickel, cerium plus nickel plus manganese, and cerium plus cobalt plus manganese at temperatures up to 290°C. (554°F.). Magnesium-cerium alloys have been used in some commercial applications. It is reported that an alloy containing 3 per cent Ce plus 0.5 per cent Mn plus 0.5 per cent Ca is being used on a forged impeller in Great Britain. Two forged parts made from an alloy with a nominal composition of 5 per cent Ce and 2 percent Mn have been found on the German .BMW-801D aircraft engine. These two forgings consist of a supercharger impeller and a rear cam-follower guide. In this country, several types of pistons have been made experimentally in both .the cast and the forged conditions from an alloy containing 6 per cent Ce plus 2 per, cent Mn and in the cast condition from an alloy of magnesium plus 10 per cent Ce. The cast pistons have been tested in various types of internal-combustion engines, with promising results. This paper presents the results of an extensive investigation on the properties of various cerium-containing magnesium alloys in both the cast and the forged conditions. Data are presented to show the beneficial effects of increasing amounts of cerium on the mechanical properties of magnesium at elevated temperatures. The effects of heat-treatment on the properties of these alloys and the attendant changes in the microstructure are discussed. The

Jan 1, 1946

By L. Andrews

Mineralogy, traditionally associated with concentrator studies, is being increasingly applied to problems in pyrometallurgy. Such investigations commonly make use of a number of techniques, and the results are combined for a meaningful interpretation, which can lead to a successful solution for the problem. Mineralogical techniques are described for various pyrometallurgical operations. Examples are given of studies and investigations involving mineralogy in chemical-looping combustion, feed monitoring to platinum-smelting furnaces, and losses to slag in base metal and platinum smelting.

Jan 1, 2011

By N. E. Grosvenor

Several methods have been proposed for determining the tensile strength of rock. These have been tried out over the past several years, but the results have been erratic and of doubtful value. The tensile strength of rock is its weakest property, and this property apparently enters into all failure phenomena, whether underground or on the slope of an open pit. Therefore, it is essential that detailed quantitative information is known about the tensile strength of rock if the design engineer is going to select the proper pit slope, pit orientation, or orientation of underground workings so as to give the most economical and safest mining condition. This quantitative information may be used to orient the pit in such a manner as to allow steep slopes along two sides. This information possibly may be used to orient the direction of either underground workings or open pits so as to decrease powder consumption and to increase blasting efficiency. Hence it is of prime importance that a method of determining accurately the tensile strength of rocks be developed. The U. S. Bureau of Mines states' that no standard methods have been proposed by the ASTM for testing the tensile strength of rock. The method described in the Bureau publication is said by them to be unsatisfactory. A similar test that has been used in our laboratory in place of the USBM test is shown in Figs. 1 and 2. h this test the core is placed in a set of grips that has been designed for one particular size core. The grips are designed to distribute the stress around the core if they are tightened correctly. A universal joint or a flexible cable may be used in conjunction with the apparatus to prevent bending or twisting of the specimen. The main difficulty encountered with the system shown is the failure of the specimen within the grips. The possible cause of the failure within the grips may be due to a stress concentration set up by the uneven tightening of the grips. This method can be used only for tests on cores, and even then has been found to be totally unsatisfactory because of the failure within the grips. The U. S. Bureau of Reclamation has been using a test similar to the sketch shown in Fig. 3. Sulfur is cast around each end of the specimen to form a bearing surface and then a ring grip is used to apply a tensile stress. The grips are in contact with the sulfur cast and do not touch the specimen. This method is unsatisfactory, apparently because a large number of the specimens appear to break within the sulfur cast. Professor Wuerker of the University of Illinois uses the test shown in Fig. 4.' Professor Wuerker states2 that this method has given definite and reproducible results with the weakest as well as with the strongest rocks. The test is a supplement in all cases where cores cannot be obtained. The principle and equipment are the same as for the test for tensile strength of hydraulic-cement mortar. Soft

Jan 1, 1961

By William W. Edgerton, Calvin Locke

INTRODUCTION King County, Washington operates a regions wastewater treatment system that provides treatment to 18 cities and 16 sewer districts in the greater Seattle metropolitan area. The system serves 1.4 million people and currently includes two regional treatment plants. In 1999, a long-range planning study identified the need for a third regional treatment plant, now known as Brightwater. Prior to this project, the county has almost exclusively used the traditional design-bid-build delivery process for its capital projects. However, with the adoption of the RWSP, the county began to study the potential application of innovative project delivery methods. This paper looks at the project delivery methods used for the Brightwater project, based on the specific needs of this large, complex, and multi-faceted project. THE KING COUNTY WASTEWATER TREATMENT SYSTEM In 1958, voters approved the formation of a regional agency called the Municipality of Metropolitan Seattle, or Metro, to build and operate a regional wastewater collection and treatment system. Prior to the formation of Metro, there were no regional wastewater treatment facilities and pollution of Lake Washington and Puget Sound from untreated sewage was a concern for many residents. In 1994, King County merged with Metro. The county’s 1,087 square kilometer (420 square miles) wastewater service area covers most of urban King County and extends into portions of two neighboring counties. The system includes two regional treatment plants, a local plant, 61 pump and regulator stations, and 571 kilometers (355 miles) of conveyance pipeline which convey wastewater from local districts to the treatment plants. As with other areas, the greater Seattle/King County region has seen rapid population growth. The RWSP estimates that the current system would soon reach capacity, and called for the construction of a new third regional treatment plant, called Brightwater, to be operational by 2010.

Jan 1, 2005

A case study for the application of a novel geostatistical technique for resource estimation of a narrow steeply dipping, gold-silver mineralized quartz vein deposit is presented. The technique is novel in two respects. First, mineral grades are kriged directly rather via the accumulation method more often applied to vein deposits and, second, a modified 2D ordinary kriging algorithm is used that allows the calculation of a single grade and variance for irregular shaped blocks of varying sizes. The objective of this investigation was to evaluate the suitability of this novel geostatistical technique for resource estimation of the Poura mine deposit and, if appropriate, to lay a firm foundation for future geostatistical work at the mine. The reserve estimation concentrated on the remnant ore blocks and pillars in both underground and surface workings. The data, which was collected in 2D coordinates with grade and vein thickness values, was first analyzed statistically and used to compute experimental semi-variograms. Appropriate semi- variogram models were fitted and various aspects of the estimation technique were evaluated using cross-validation error analysis, with acceptable results. A block kriging computer program called Krige2D was developed to implement the modified 2D kriging algorithm and calculations. Production data were not available to evaluate the computed block resources, but they were compared with a previous resource data determined using an arithmetic approach. The geostatistical technique estimated slightly higher grades but lower overall tonnages as compared to the earlier arithmetic estimates.

Feb 1, 2004

By H. E. Stauss, J. Hino

INTEREST in silicon has arisen again in the past decade as a result of improvements in crystal rectifiers.' Although the preparation of silicon was first reported by Berzelius in 1880, the early product was of relatively low purity, and only the need for rectifiers in World War II led to the production of a 99.9+ pct pure powder. This material in crystalline form was consolidated into massive silicon for use, and the method developed was to melt it with selected added constituents as "doping" agents. Melting techniques, therefore, are of great importance. There are two basic problems in producing silicon ingots free of doping additions; one is the prevention of spitting and the other is prevention of cracking of the ingot during freezing. The most satisfactory arrangement yet developed for producing massive silicon is to melt and freeze in a cylindrical quartz crucible surrounded by a concentric heating element and concentric radiation shields or insulation. For example, use can be made of a tubular heater with a high frequency generator as the source of power and reflecting shields of alundum cylinders. The spitting of silicon is related to gas evolution, and the gas comes from two primary causes—adsorbed gas and the reaction products of silicon and the crucible. Gas is also released from bubbles contained in the quartz crucible walls. Improved removal of adsorbed gas can be achieved by means of controlled melting and freezing. The seriousness of the problem in vacuo is reduced with an electrically operated mechanical movement of the high frequency power coil. The upper portion of the powder charge is melted first and the high frequency coil lowered until the powder is completely molten. During cooling the high frequency coil is raised slowly. These means also reduce the final nonviolent extrusion of large beads of metal through the ingot top during freezing. Better control of spitting and bead extrusion is obtained when melting is done under helium at. atmospheric pressure instead of in vacuo. The problem of reaction between silicon charge and crucible in practice is confined to the reaction between silicon and quartz. This2 apparently is: Si + SiO2 + 2SiO The part that this reaction plays in spitting has not been isolated for separate study. SiO is a volatile vapor at the melting point; of silicon and is released freely during melting in vacuo, but hardly at all in helium at atmospheric pressure. The cracking of ingots is a major difficulty in melting silicon, and its prevention requires special melting techniques or the addition of "toughening" agents such as aluminum or beryllium.' The cracking of the ingots has been explained as being the result of the expansion that occurs upon freezing; although direct observation of freezing ingots reveals visible cracks on the surface only after a red heat has been reached, suggesting that cracking is the result of differential contraction of silicon and quartz. Silicon wets quartz, and the ingot adheres tightly to the crucible. Therefore as ingot and crucible cool, the two either have to pull apart, or at least one must crack. Surprisingly, in spite of the relative thinness of the quartz and the thickness of the ingot, the ingot and the crucible both crack. Microscopic and X-ray4 studies fail to show any plastic flow other than twinning in the ingots. Slow cooling fails to prevent cracking. Another possible solution to cracking is to weaken the crucible. Use of thin-walled crucibles finally led to success with fused quartz crucibles with a wall thickness of 0.25 to 0.50 mm. With such thin-walled fused quartz crucibles consistently uniform success is secured in producing sound ingots 30 mm in diam from the purest available grade of silicon (99.9+) without the use of any type of addition. Melts are made in the size range of 50 to 100 g. Omission of a deliberately added doping agent is not sufficient to insure pure ingots. The reaction of silicon with crucibles and the resultant solution of impurities in the silicon is well-established." In this laboratory, the presence of Al, Be, and Zr has been found spectroscopically in ingots melted in contact with alumina, beryllia, and zircon. The best crucible materials reported in the literature are MgO and SiO2. Use of MgO in this laboratory has resulted in a heavy deposit of magnesium on the furnace walls, showing that a reduction of the magnesia occurred and the resulting magnesium removed from the melt by volatilization. In the case of quartz, the silica is reduced and SiO liberated to deposit on the equipment walls. There probably is real danger that oxygen is dissolved in the ingot when either magnesia or silica is used as the crucible material. Preliminary analyses by Dean Walter in his vacuum unit in this laboratory6 indicate the presence of oxygen in undoped silicon melted in quartz.

Jan 1, 1953