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Gold recovered on the strikes at the Central Norseman mill, Norseman, Western Australia, has an approximate assay fineness of 850. Bullion recovered from the cyanide plant at the mine is of much lower value, and occasionally its assay fineness has been as low as 250. This indicates either that the fine gold particles in the ore consist of an alloy richer in silver than the coarse particles or else that a silver mineral, as well as the gold, is dissolved by the cyanide solutions.It had been observed at the mine that the amount of silver in the bullion appeared to increase when galena appeared to be more abundant in the stoped ore. Interest was, therefore, attached to the possible occurrence of a silver mineral associated with galena and, at the same time, soluble in cyanide.Four specimens of ore from different horizons in the mine were collected by the mine staff for examination as to whether any marked difference in the fineness of gold was apparent on a polished surface and for determination of the silver minerals. As the Norseman ore-body is a quartz reef containing a very small percentage of sulphide, the specimens were selected either because they cont;:lined free gold or because they were, relatively rich in sulphides. They were obtained from the following localities at the Phoenix shaft.1. Level 16, section 28.2. Level 16, section 31.3. Level 8, section 31.4. Level 14, section 38.Specimens Nos. 1 and 2 were thus obtained from different positions at the same mining horizon, while specimens Nos 2 and 3 were obtained from different levels in the same vertical section of the mine.All the specimens consist of quartz characterized by thin, discontinuous seams of sericite and the presence of a little ankerite. Gold and sulphides tend to be localized along these seams, but particles of gold and sulphides are also scattered throughout areas of white quartz. This scattered distribution of the sulphides in relatively wide areas of quartz has involved the preparation of two or more polished sections from each specimen.The outcome of the microscopical examination of these specimens has been to determine that there is no appreciable variation in the colour of the polished particles of gold and, therefore, no marked difference in the amount of silver alloyed with the coarse and fine particles. The presence of small quantities of the tellurides sylvanite, hessite and altaite has been revealed, and found to vary in abundance with the abundance of galena.

Jan 1, 1944

By P D. Katsabanis

According to Persson(1) steady state detonation along a cylindrical charge can be regarded as a self propagating process in which the axial compressive effect of the shock front discontinuity changes the state of the explosive so that exothermic reaction sets in with the requisite velocity.

Jan 1, 1990

By Ke Yang

Drilled shafts are widely adopted as the foundation for sound walls. However, there has been a lack of uniformity in design and analysis methods and design criteria, in terms of factor of safety against ultimate capacity failure as well as the allowable deflection. In order to establish a uniform design methodology for the drilled shafts supporting sound walls in cohesive and cohesionless soils, respectively, a database of full-scale lateral load tests on fully instrumented drilled shafts was collected. Based on the compiled database, existing design methods and design criteria of laterally loaded drilled shafts were evaluated. Broms method and COM624P (or LPILE) are suggested as the design methods for drilled shafts supporting sound walls in both cohesive and cohesionless soils. Additionally, the corresponding design criteria, including factor of safety and permissible deflection, for both design methods are recommended. Two full-scale lateral load tests on fully instrumented drilled shafts were subsequently conducted in Colorado to further verify the design recommendation. A comprehensive geotechnical investigation program was also carried out at the two new lateral load test sites that included pressuremeter test, SPT, as well as laboratory triaxial consolidated undrained tests and direct shear tests on the soil samples taken from the lateral load test sites. The test results obtained at these two load test sites were employed to validate the recommended geotechnical design and geotechnical testing methods for the drilled shafts supporting sound walls.

Jan 1, 2007

By Alejandro Gutiérrez, David Ahues, Paola Merino, Felipe González

A Discrete Elements Method (DEM) study of load movement within a SAG mill 12,192 × 7620 (40′ × 25′) in normal operating conditions is performed. The purpose is to determine how the geometry of the lifters affects the kinetics of the load inside the mill. Specifically, the changes produced by the incorporation of inclined lifters and spiral or helicoidal pulp lifters to the kinetics are evaluated. Four study cases are identified: first, the base case corresponds to a conventional geometry; the second case corresponds to inclined lifters incorporation; third case corresponds to a mill with helicoidal discharge; and the fourth case corresponds to a mill with inclined lifters and helicoidal pulp lifters. To save computational resources, the water that enters the mill has been modeled by varying the coefficient of restitution. The results of a series of experiments are presented to determine how this coefficient varies when having impacts on surfaces with different liquid levels. A comparative analysis is made of the following variables: mean transport speed and material flow, for normal operating conditions. Taking as reference the mill with straight lifters and radial pulp lifters (case 1), the case with the inclined lifters and radial pulp lifters increases the material discharge flow less to 76 mm of size by 5.1%, and this value increases even more when the helicoidal pulp lifters are incorporated reaching a 58.6%. The most significant change is seen in the flow through the grates and the pulp lifters discharge, which can increase substantially improving the operation.

By Victor Romero, Steve Redmond

All Rights Reserved. Printed in the United States of America. Information contained in this work has been obtained by SME, Inc. from sources believed to be reliable. However, neither SME nor its authors guarantee the accuracy or completeness of any information published herein, and neither SME nor its authors shall be responsible for any errors, omissions, or damages arising out of use of this information. This work is published with the understanding that SME and its authors are supplying information but are not attempting to render engineering or other professional services. No part of this publication may be reproduced, stored in a retrieval system, or transmitted in any form or by any means, electronic, mechanical, photocopying, recording, or otherwise, without the prior written permission of the publisher. Any statement or views presented here are those of individual authors and are not necessarily those of the SME. The mention of trade names for commercial products does not imply the approval or endorsement of SME.

Dec 1, 2011

By Stratton-Crawley R., G. E. Agar

"A study has been done of the scale-up of laboratory bench-scale flotation to continuous plant circuit performance. It was found that the impellor speed and the air flow rate influenced the results and in this case extreme values of these operating variables were required in order to reproduce the plant rougher results in the laboratory. Despite the experimental uncertainty introduced by these extreme values, it was demonstrated that the plant performance could be predicted and experimentally reproduced with bench-scale tests.IntroductionThe mineral processing industry relies heavily on batch flotation testwork to design flowsheets, evaluate reagent s and compare various types of ore. The batch tests are generally regarded as being directly comparable within themselves, but quite often they relate poorly or not at all to continuous circuits. Obviously this dilemma generates considerable uncertainty with wide-ranging ramifications. One of the manifestations of this unfortunate situation is the commonly expressed opinion that ""it may work that way in the laboratory, but it will never work that way in the plant"".In a previous publication, a method was described whereby the results of batch bench-scale tests could be used to simulate a locked cycle flotation test series. The work to be described here is a continuation of that investigation with an extension to the simulation of an actual plant circuit. It would have been preferable to progress from laboratory batch data to a continuous pilot plant and then finally to a full-scale plant operation. However, because that possibility did not present itself, an attempt will be made to show that the performance of an existing plant circuit can be successfully simulated from batch data. The success of the procedure can be judged by the agreement among the plant results, a locked cycle test and the predicted results based on batch tests."

Jan 1, 1982

By C J. Kruger, E le Roux

Anglo American Platinum has adopted a strategy of Best Practice Principles (BPP) for sampling, mass measurement, analysis and metal accounting for more than a decade now. When new plants are designed, the most suitable sampling equipment and sampling protocols are implemented and material flows and plant layouts are designed around sampling strategies. A few years ago, a crushing plant for a high-grade matte stream was commissioned.The design called for the high-grade material to be crushed to 95 per cent passing 2 mm and the design allowed for a single cutter primary Vezin sampler, increments taken from a gravity flowing stream at regular intervals, whilst filling a tanker for the pneumatic offload at our base metal refinery. This was a single point of sampling and analysis that would measure the wanted output from our smelting complex and the input to our refineries. In addition, the design incorporated the functionality to collect increments in an ‘interleaved’ fashion from the Vezin sampler for internal precision checks.The metal accounting strategy for Anglo Platinum is the ongoing measurement of all inputs, outputs and stock levels for all our operations for platinum group metal (PGM) and base metal (BM) content. Included are yearly stocktakes, usually done on 1 February every year, across the smelters and refineries (at least the base metal refinery). A trend was developing in the accounting period immediately following the introduction of the new crushing and sampling facility, whereby the absolute difference between the physical stock and theoretical stock (PGMs predominantly) increased for the two respective sites on an ongoing basis. The smelter (sender) showed an increase in physical stock compared to the theoretical stock and the base metal refinery (receiver) showed that their theoretical stock increased against their physical stock. Because of this anomaly, an additional stocktake was held in September for the period in question and it was confirmed through the physical stock measurement results, that the PGM accounting problem was indeed pointing towards the evaluation of the high-grade matte stream.This paper showcases parts of the process that took place to explain the poor accountabilities for the respective sites. Previous results from the sampler ratification process (of the interleaved sampling design) were analysed again, a physical inspection was carried out on the sampling system again and the sampler performance was monitored (quality control parameters) for the period.From these investigations, it was found that airflows present inside the Vezin introduced the sampling bias and a change in sampling protocol was introduced as well as physical changes to the sampling equipment were made to eliminate the airflow and thus the bias conditions significantly. The accounting period which followed, after a phased upgrading process, showed that the accounting between our smelter and base metal refinery had been restored to within statistical limits (difference between physical and theoretical stock below five per cent relative to theoretical stock).CITATION:Kruger, C J and le Roux, E, 2017. Pitfalls in Vezin sampling for finely crushed materials, in Proceedings Eighth World Conference on Sampling and Blending , pp 151–158 (The Australasian Institute of Mining and Metallurgy: Melbourne).

May 9, 2017

By D. G. Klaren

Self-cleaning fluidized bed heat exchangers are conquering the world for reason that they are able to solve any severe fouling problem in indirect heat transfer due to the circulation of cleaning particles through the tubes of vertical shell and tube exchangers. In most cases, these particles consist of chopped metal wire. Moreover, self-cleaning fluidized bed heat exchangers perform with excellent heat transfer at very low liquid velocities, which makes completely new designs of shell and tube configurations possible. Further, self-cleaning fluidized bed heat exchangers show a strong shear thinning effect in non-Newtonian liquids. All the above characteristics make the self-cleaning fluidized bed heat exchanger an ideal tool for the indirect heating of laterite nickel slurry in High-Pressure-Acid-Leach (HPAL) plants. Preliminary tests and evaluations of these heat exchangers have shown that the performance and price of these heat exchangers used for the production of nickel and cobalt from a laterite slurry, cannot be matched by existing conventional heat exchange systems. This article explains the principle, design, lay-out and enormous advantages of the self-cleaning fluidized bed heat exchange technology in a plant suitable for an annual production of approx. 45,000 ton nickel and 4,500 ton cobalt from laterite slurry through high pressure'acid leaching.

Jan 1, 2002

By K. H. J. Clarke

"ALTHOUGH nickel was not identified as a separate element until a Swedish scientist, Axel Frederick Cronstedt, did so in 17 51, its utilization dates from pre-historic times. From its humble beginnings nickel has grown in importance until, today, in our clocks, television sets, automobiles, and air-planes, in our bridges, tableware, farm implements, and the equipment which processes our food, it is constantly at our service.For convenience in assembly, data and information relative to The Marketing of Nickel will be outlined in five phases: (A) Sources, (B) Distribution, (C) Utilization, (D) Market Development, and (E) Conclusions."

Jan 1, 1960

By Jay Nopola, Christopher Johnson, Matthew Minnick, Erik Hemstad, Erik Walega

Mining data collection, storage, and interpretation methods have progressively changed over time. Data collection, for the most part, has transitioned from handwritten notes and logs based on manual gauge readings to real-time data streaming through instrumentation capable of directly communicating with site-based data historians or cloud storage. Data collection and storage have had to adjust commensurately with the volume of data, leading to more complex database architecture. Geoscience interpretation methods have also changed; however, the first goals of modeling and understandings from first principles remain the same and are typically deeply rooted in historical academic work. Machine learning methods are becoming more common, available, and implemented by industry and practitioners. Despite the wide accessibility of machine learning methods, the population of geoscience subject matter experts in the underlying theory of this analysis type is limited. This form of analysis, therefore, must be conducted carefully and in conjunction with subject matter experts, on both machine learning theory and the field it is being applied to. This paper aims to provide background history on data analytics and machine learning, current methods and practices, and high-level geoscience case study examples, as well as take aways regarding the mining industry, potential pitfalls specific to geosciences, and possible perspectives on the direction of artificial intelligence in the future.

Jun 25, 2023

By Hazel Lyman Nickel

Daring to try where others had failed, Herbert and Lou Henry Hoover translated from the Latin the principal (and first) textbook on the mining and metallurgical profession, De Re Metallica, 1556, which had been in use for two centuries and then had lain dormant for 350 years in a language unreadable except by a chosen few. Thus the Hoovers enriched the English tongue with a vitally important contribution to history in the fields of mining, metallurgy, and chemistry. To them it was a joint hobby, because they were actively interested in the beginnings of the mining profession in which they had both been trained. Illuminating the years of toil to perfect this translation shone their ideal of service to humanity, since, in the Preface, they refer to their task as "a labour of love", which had to find the moments for its execution in night hours, weekends, and holidays, extending over a period of about five years. And they add: "If the work serves to strengthen the traditions of one of the most important and least recognized of the world's professions, we shall be amply repaid". While a student at Stanford University, during the years of 1891-95, Herbert Hoover had become familiar with a copy of this Latin mineralogy classic, De Re Metallica, a rare book in the private library of Dr. John C. Branner, at that time head of the department of geology and mining. Another Stanford student in geology was also examining and studying the ponderous volume of twelve 'books'. She was Miss Lou Henry, of Monterey, who graduated in 1898, and the following year became Mrs. Herbert Hoover. Interwoven through the tapestry of their life experiences gleamed the silver thread of their interest in this mediaeval Latin textbook. Just nine years lacer, the Hoovers had commenced their translation, while they were in temporary residence in London after the seething years in China under the shadow of the Boxer rebellion.

Jan 1, 1949

By Dean Bray

During the past three years, a new rear-dumping dragline bucket technology has been patented, developed and tested at North Dakota coal mines. Field testing has shown that this new concept in dragline bucket technology can improve strip-mining efficiencies by reducing cycletimes and increasing dumping radius. This article details the process, participants and the results for the development of a rear-dumping dragline bucket. Participants in the process In November 1995, the board of directors of Dakota Coal authorized the execution of a field test and option agreement and a license agreement with the partnership of D.F. Schmidt, electrical/maintenance supervisor, and Bill Lengenfelder, president of Modern Industrial. The board also authorized entering into a dragline bucket field-testing agreement with the Falkirk Mining Co.

Jan 1, 1999

By Kenneth E. Hay

Researchers from the U.S. Bureau of Mines conducted a field study to assess the safety of remotely controlled mobile roof supports (MRS) in a retreat pillar mining operation, Data were collected to provide the Mine Health and Safety Administration with criteria needed to develop guidelines for MRS use and to determine if precursors could be identified that would alert miners to imminent roof falls. Two test sites at which two different support methods-MRS's and posts were used and were monitored to obtain information on entry stability. Pressure transducers and string pots were installed on all four MRS's to obtain loading and displacement information. and roof bolt load cells. sonic probes, extensometers, and survey targets were installed in the surrounding entries to obtain information on ground behavior. Results showed a larger increase in roof bolt loading and roof movement when MRS's were used, especially in the intersection area. Roof bolt loads in the entries showed decreases in load when the MRS's were set and increases up to 11,1 kN (2,500 lbf) when the MRS's were unloaded. Unloading of one MRS in a pair did not significantly increase load on the other. MRS's I and 2 usually had the higher loads, with these loads increasing as the pillars on each side were being mined. MRS 3 normally had lower loads than I and 2: however, it also experienced some very high loads when in the last position near the pushout. MRS 4 usually had the lowest loads, primarily because it was located near the solid pillar that was not being mined.

Jan 1, 1995

By Kevin Beirne

Most people involved in the mining industry are familiar with student-industry co-op work-study programs. Many colleges and universities have used them for years. Northern College’s Haileybury School of Mines student co-op program adds a new dimension of productivity to the college and the mining industry. The college is located in Hailey-bury, Ontario, Canada. An example of the program’s success is the school’s relationship with Sabin Metal’s SMC (Canada) Ltd.’s McAlpine Mill in Cobalt, Ontario. Students gain practical knowledge and experience while industry gains an eager-to-learn worker. And many of the college’s advanced research services are made available to industry to supplement their own capabilities. The McAlpine Mill was established to provide custom milling of slags and ores. It also recovers metal values from other products of the primary and secondary precious metal industries.

Jan 1, 1999

By S. McGinn

The Brunswick Mine Diesel Particulate Filter Study was one of several research projects initiated by the Diesel Emissions Evaluation Program (DEEP). The study was carried out at Noranda?s Brunswick Mine in Bathurst, New Brunswick by Noranda Technology Centre and Brunswick Mine personnel with the collaboration of Natural Resources Canada - Canada Centre for Minerals and Energy Technology (CANMET), National Institute of Occupational Safety and Health (NIOSH), Andreas Mayer of VERT, and diesel particulate filter (DPF) system suppliers. The study began in early 2000. Field evaluations continued for 20 months. The final report?authored by Sean McGinn?was submitted to DEEP in the Autumn of 2003.

Jan 1, 2004

Geochemical projects in progress or recently completed in the Bureau of Mineral Resources, Geology, and Geophysics (BMR) cover a wide range of topics and include research projects, regional studies, and prospecting programmes. However, in these notes emphasis is given to projects which are directly relevant to mineral exploration.FIELD INVESTIGATIONSStream sediment sampling, rock and soil sampling, and geobotanical surveys have been used by the BMR in a number of areas, partly in attempts to locate specific zones of mineralization, and partly to investigate the effectiveness of the various methods under different conditions of climate and topopraphy and in different geological settings.Stream sediment sampling has been most successful in the Territory of Papua and New Guinea. For example, in the South Sepik area, zones of disseminated su1phide mineralisation were found to give rise to anomalies with peak values of up to 1,000 p.p.m. copper, compared with background values of about 40 p.p.m. (Dow et al., 1968). By contrast, the results of rather limited work in the Northern Territory and in the Kimberley district of Westen Australia were inconclusive.Rock and soil sampling, on the other hand, was successfully used in a number of areas in Northern Australia, particularly at Rum Jungle and Tennant Creek.Rum Jungle area In the Rum Jungle area, where uranium and base metal mineralization is mainly associated with a Lower Proterozoic black slate sequence, samples, of c-horizon soil or weathered 'rock are generally collectedfrom the bottom of drill holes, usually 15 to 20 ft deep, bored with a power-operated auger.Surface sampling indicates that such a technique would probably have shown up all the major geochemical anomalies delineated by deep sampling, but the latter gives slightly more consistent and slightly

Jan 1, 1970

By Jack Bedder

"Editor’s note: We would like to thank those who make this annual issue possible. A special thank you goes out to the industrial minerals annual review editor, to the Industrial Minerals & Aggregates Division Technical Committee chair and vice chairs, and to the authors of the individual commodity profiles.Jim Norman, member SME, of Tetra Tech, is the industrial minerals annual review editor.Ebrahim K. Tarshizi, member SME, of Michigan Tech, is chair of the Industrial Minerals &Aggregates Division’s Technical Committee.The technical committee vice chairs include: • Hyunjung Kim, member SME, of Chonbuk National University, agricultural materials.• Xihui Yin, member SME, of Kemira, ceramics and refractory materials.• Nikhil Gupta, member SME, of Virginia Tech, chemical raw materials.• Jasson Giddens and Swadhin Saurabh, members SME, of Oil Dri Corp of America and Mill Creek Engineering, respectively, chemical raw materials.• Snehamoy Chatterjee, member SME, of the Michigan Tech.• LeDeana Roberts and Shubham Verma, members SME, of Imerys and U.S. Oil Sands, respectively, fillers and pigments.• Thomas Hilderbrand and Kaiwu Huang, members SME, of Thiele Kaolin Co. and Virginia Tech, respectively, sorbents, filters and process aids.• Rhaghav Dubey and Edgar Blanco, members SME, of Outotec and FL Smidth, respectively, specialty mineralsAntimony generally occurs along with gold, lead, copper and silver. There are more than 100 antimony minerals, although the sulfide mineral stibnite is the main one.Antimony enters the supply chain either as a result of mining (primary production) or recycling (secondary production). China has by far the largest antimony resources and is, as a result, the world’s center for antimony mine production. In 2016, it accounted for more than three quarters of the global mine supply out of a world production figure of 130 kt (143,000 st), according to the U.S. Geological Survey. The biggest, and most high-grade deposits are found in southern China, with the largest mines located in Hunan, Guangxi and Yunnan provinces. Tajikistan, Russia, Australia and Bolivia are the largest mine producers outside China. A new antimony project in Oman made progress in 2016, producing first metal in April 2016 in test facilities, and then ordered three furnaces for a 26 kt/a (28,600 stpy) antimony metal and oxide smelter that is due on stream in late 2017.Antimony ingot production is not as widespread as is antimony mine production, owing to the high levels of pollution that are associated with antimony smelting. It is for this reason that smelting has been largely confined to China and other Asian countries, where environmental legislation is less stringent.Antimony oxide production is undertaken on four continents with China being the biggest producer. There is also a considerable amount of oxide production in Europe — which relies on imported feedstock, mostly from China. Antimony also enters the supply chain through recycling. Lead containing antimony is produced in a number of countries, mainly in secondary lead smelters. Typically, a blast furnace charge containing used or discarded battery plates, type metal or bearing metal is reduced to lead bullion, which is refined in reverberatory furnaces and melting pots. In the main, the antimony recovered is consumed in metallurgical applications. China was the biggest secondary antimony producer in 2016, and accounted for 25 retardants and lead-acid batteries. Flame retardants accounted for roughly 50 percent of consumption in 2016 with batteries representing about 25 percent. Other end uses include plastics and heat stabilizers, ceramics and glass and a variety of metallurgical applications. Demand has been sluggish since the global financial crisis, mostly because key markets failed to recover strongly from the downturn, particularly in Europe."

Jan 7, 2017

By BUREAU OF MINES

Mercury has been used by mankind since prehistoric times. It has been, and is now, widely used in industry and medicine and has unique properties which make direct substitution difficult or impossible. At present its prin- cipal uses are for electrical apparatus, control instruments, electrolytic soda preparation, mildew-proofing paints, pesticides, and medical and dental preparations. Deposits of mercury are less common than those of other base and precious metals, but some of the deposits are very large and have been ample to meet the world's past demands. The price of mercury has had many sharp fluctua- tions, but in general, the limited number of producers has resulted in a more stable price structure than that of many other commodities. The United States has been one of the main producers of mercury, and from 1850 to 1961 produced 3,247,704 flasks. Yearly production since World War II has varied from 4,535 to 38,067 flasks. An estimate of domestic resources of mercury producible at various price ranges was prepared for each mercury mine by combining specific knowledge of mercury mineralization with estimates of potential, based on geologic informa- tion and past production history. The sum of the individual estimates for each price range is shown in a table. A parallel estimate of nationwide production potential was made from a study of past price and production relationships. These were analyzed by plotting yearly production figures against the previous year's price, expressed in dollars of constant purchasing power. An equation was fitted to the data by mathematical means and was used to extend the curve into areas of higher than historic prices. Potential production rates at various price levels were taken from this graph. The estimated yearly production rates were used to make an estimate of total potential based on the premise that produc- tion rates and reserves have a proportionate relationship.

Jul 1, 1964

By Percy W. Bidwell

THE statisticians had defeated Germany months before she invaded Poland. With batteries of adding machines they had proved that she was suffering from serious deficiencies in critical food- stuffs and in practically all of the raw materials necessary for the conduct of modern warfare. Their calculations showed that with respect to fats, oils, wool, cotton, hides, petroleum, iron, copper and other metals, the Reich was bound to be at a great disadvantage vis-a-vis the French and British as long as the latter could keep open the lines of sea communication. The conclusion seemed obvious-"Germany can't win." The more cautious of the commentators introduced qualifications as to the length of the war and the tightness of the British and French blockade. They also made a third qualification as to the character of the struggle- whether it was to be a war of attrition or a war of movement. But since the invasion of Norway in April, there is no longer any doubt on this score. It is a war of movement-a war in which fuel, lubricants, and metals are being consumed on a scale never before seen.

Jan 1, 1940

By R. W. Bartlett

DISILICIDE coatings, MeSi2, on refractory metals are usually grown by a solid-state diffusion reaction similar to the parabolic oxidation of metals. Two or more silicide compounds occur in each of the binary silicon-refractory metal systems. When an adequate source of silicon is available during the coating process, the lower silicide compounds are usually not formed.1 However, during service application of the coated refractory metal, continued heating causes further diffusion and growth of the lower silicides. A study of the growth kinetics of the lower silicides in the molybdenum and tungsten binary systems with silicon was previously reported.2 The present study is concerned with the growth kinetics of Ta5Si3 and Cb5Si3, formed as conjugate layers between TaSi2/Ta and CbSi2/Cb diffusion couples, respectively. Diffusion couples consisting of disilicide-coated tantalum and columbium sheet coupons were subjected to diffusion heat treatments, cross-sectioned, and scanned by an electron-microprobe analyzer to determine the relative X-ray intensity profiles. These profiles correspond closely to concentration profiles for the constituents, and were used to identify phases and locate phase boundaries. The analysis of a single specimen after a diffusion-anneal provides only one value for the Me5Si3 phase thickness, corresponding to the time and temperature of the diffusion treatment. Consequently, each isothermal curve showing the rate of accumulation or depletion of silicide phases required several samples with identical diffusion temperatures but different diffusion times. The disilicide coatings were prepared by pyrolizing commercially pure silane in a hydrogen carrier gas. The hydrogen was purified by passage through a palladium membrane. Commercially pure tantalum and columbium sheet metal coupons, 0.005 by $ by 2 in., were used. All of the coated specimens for each system were prepared together in a single group in order to minimize coating variations among individual specimens. During pyrolysis, the brightness temperature was maintained at 1200°C. With suitable flow rates at this temperature, only the disilicides of tantalum and columbium were formed in detectable amounts. Coated specimens were subjected to diffusion an-neals in a tube furnace with automatic proportional control within ±10°C. A H2-Ar mixture, deoxidized and dried over anhydrous magnesium perchlorate, was used to prevent oxidation during the diffusion anneal. Diffusion couples were cross-sectioned, polished and examined with an A.R.L. electron-microprobe X-ray analyzer. Both metal constituents in each specimen were simultaneously scanned using a 1-p beam spot size and either 1- or 2-µ steps. Analyses were performed using the Ka radiation of columbium and silicon, and the La, radiation of tantalum. For all specimens, an acceleration voltage of 30 kv was used, and integration was made against the specimen current. LiF and A DP monochrometers were used to isolate characteristic radiations. Three or more traverses were made on each specimen. The intensity scales were adjusted using the constituent metals and standard samples of the silicide compounds which had been verified by X-ray diffraction. The relative intensity profiles were used directly, in conjunction with the standard samples, to identify compounds and phase boundaries. The stoichiometries differ considerably between the silicide compounds in both systems, and the homogeneity range for these silicide compounds is narrow. These characteristics result in marked differences in relative intensities of the fluorescing elements—differences which permit ready identification of phases and phase boundaries. Projections of both electron back-scattered images and characteristic

Jan 1, 1967