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By P. I. Brooker

The semi-variogram, the basic tool of geostatistical estimation procedures, must itself be estimated from the available data. From a numerically simulated two-dimensional deposit, with known variability expressed through its semi-variogram, the standard arithmetic mean estimator is used to calculate experimental semi-variograms. These are determined on a series of data sets obtained from the deposit with various sampling grids that cover different areas of the deposit and have a mite range in the number of available data. The orders of discrepancies between estimated and theoretical semi-variograms are determined in this idealized situation; and this provides a basis against which to assess experimental semi-variograms made on field data.

Jan 1, 1984

By A. C. Bluemel, J. S. Harper, J. H. Jett

Can the mining industry in the United States accept the change and challenge of the "Now Generation" of an entirely new high-performance automated transportation system? Advanced transportation systems for the mining industry can be defined as those which lend themselves to automation and meet definite performance and cost objectives. The term automation shall mean that control of transportation system is accomplished by a closed loop electronic circuit which, when started on command, will continue to cycle as programmed until such time as an intelligent feed-back causes the system to shut down.

Jan 1, 1970

By Charles Will Wright

The present struggle for economic and industrial supremacy by the Communist world is against the United States, its main target, and the other Free World nations. The basis of industrial power is minerals, so the Communist nations are building up mineral production within their borders, often regardless of costs, and are acquiring quantities of mineral products from Free World countries for future use. They are contracting for additional supplies and advancing funds for the development of these quantities. A number of the less developed mineral producing countries of the Free World are being infiltrated by Communists and Communistic influence. This situation is well known, but as yet little has been done to oppose these activities or to awaken the public to their seriousness. The Communist countries are still far behind the Free World Nations in production of many essential minerals. But, shortages are being made up from Free World nations in exchange for petroleum, manganese ore, chromite and other products. Restrictions on shipments of strategic materials to Communist countries have not been maintained.

Jan 1, 1964

US 4,192,852-Precipitation of iron values as a jarosite from a sulfate solution obtained as a byproduct in the hydrometallurgical processing of zinc sulfide ore The solution is cooled, partially neutralized, and clarified. The clarified solution is heated to a temperature of 80 to 100°C in the presence of sodium, potassium, or ammonium ions to precipitate substantially all of the ferric iron as jarosite The precipitate is thickened, filtered, and washed The residual solution may be processed for zinc or other nonferrous metal values R V. Pammenter and C J Haigh, assigned to Electrolytic Zinc Co of Australasia Ltd. Mar. 11, 1980. 16 pp. (423-42) Filed: 5-8-78 (903,524). Priority- Australia, 5-9-77 (PD0030) (Drawings below.)

Jan 1, 1982

By H. G. Kok

The continuous increase in energy costs has made it necessary to consider a broader use of belt conveyors for the transportation of material from the mine pit to the processing plant. Hard rock has to be crushed before it can be moved by belt conveyors. Systems are in the planning stage for mining hard rock, such as copper and iron ore, by using high-capacity, mobile, or semi-portable crushers. The mobile crusher is located in the pit, and the crushed material is transported by energy-efficient, shiftable belt conveyors out of the pit.

Jan 1, 1983

By G. Aertsen

THE CHAIRMAN (HENRY D. HIBBARD, Plainfield, N. J).-This excellent paper fills a gap in our Transactions and is most acceptable. In the early days another way of casting tire ingots, sometimes called cheeses, because of their shape, was to use a 22-gage sheet-iron cylindrical can for each ingot of the proper size to give the weight desired. These cans were bottom cast in groups, usually of four, each can being surrounded by a heavy iron ring somewhat taller than itself the top of the can being covered by a circular cast-iron plate having a small conical riser in the center, about 2 ½ in. in diameter at the bottom and 10 in. high. The top plate was clamped down to resist the upward pressure of the fluid metal and the space between the can and the outer ring, usually about 2 in. wide, was filled with dry sand. The riser permitted the escape of some of the air displaced by the steel and also increased the pressure in the steel when the mold was filled, and so diminished somewhat the tendency for gas holes to form. But little was known of segregation and pipe in those days, though the center of an ingot was understood to be the worst part, and it was separated in part in the disk which was punched out in perforating the ingot. This disk was about 8 in. in diameter and from ¾ to 2 in. thick, the variation in thickness being to rectify the weight. When an ingot was too -heavy, a thicker disk-was made by not driving the punch in quite as far as when the ingot-weight was right. Then the bloom was turned over and the punch driven in on the other side, which finished the punching and detached the disk. The tire bloom was then" becked" and later reheated and rolled as described in the paper. The forging was done with a 10-ton double-acting steam hammer. The steel generally speaking had lower carbon, from 0.45 to 0.55 per cent., than tires today have, and the tires were smaller, the most common size of ingot weighing 1,060 lb. each. BRADLEY STOUGHTON, New York, N. Y.-This paper was specially requested by the Iron and Steel Committee, because that Committee thought so important an industry should have its history written by one who was familiar with it, and before he had forgotten, or all the rest of the world had forgotten, its early stages. Mr. Aertsen has said that it is not an exhaustive research. I think it would not be any different if it were an exhaustive research, because our library made a careful attempt to find some written light on the history of these tires, but very little was found.

Jan 4, 1917

By V. M. Karve, K. K. Majundar, K. V. Viswanathan, J. Y. Somnay

The effect of calcium, magnesium, iron (both ferrous and ferric) and aluminum ions, which are commonly encountered in a typical beryl ore, was studied in the flotation of pure beryl, soda-feldspar and quartz. The vacuumatic flotation technique was employed. With sodium oleate as collector and in the absence of any activator, beryl floated in a pH range of 3 to 7.5, whereas feldspar and quartz did not float at any pH up to 11.5. The pH range of flotation increased in the presence of the ions studied. With calcium and magnesium ions beryl floated from 3 to 11.5 pH and beyond, soda-feldspar floated beyond pH 6 and quartz floated beyond pH 8. Ferrous ion activation was found to be similar to that of calcium and magnesium. Activation by ferric and aluminium ions was found to be complex and the lower and upper critical pH for all the three minerals was around 2 and 10 respectively. These studies indicated the possibility of separation of beryl from feldspar and quartz even in the presence of calcium, magnesium and ferrous ions between pH 4 and 6. Flotation tests on a mixed feed of pure minerals in a 10 g cell revealed that beryl can be selectively floated from feldspar and quartz if ferric ion is reduced to ferrous state or if it is complexed. Beryl occurs mostly in pegmatites, and hence is associated with feldspar, quartz and micas and small amounts of other minerals such as apatite and tourmaline. The separation of beryl from these minerals is difficult because all the silicates accompanying beryl have more or less the same physical properties. Specific gravities of beryl, feldspar and quartz are 2.70, 2.56 and 2.66 respectively. Electrostatic separation has been suggested but no work has been reported. ' The adsorption of sodium tri-decylate tagged with Cl4 on beryl, feldspar and quartz reveal similarity in surface properties. Much work has been reported on the flotation of beryl from ores, either directly or indirectly as a by-product, but little is known about the fundamental aspects of beryl flotation. Kennedy and O'Meara3 laid emphasis on prior cleaning of the mineral surfaces with HF. Mica is removed first by flotation of beryl with oleic acid, around neutral pH. Runke4 introduced calcium hypochlorite conditioning in a final separation stage for activating beryl in a mixed beryl-feldspar concentrate, and after washing to remove the hypochlorite, floated beryl with petroleum sulphonate. The Snedden and Gibbs5 procedure is somewhat similar to that of Kennedy and O'Meara. Emulsified oleic acid is used as collector. Recently Fuerstenau and Bhappu6 studied the flotation of beryl, feldspar and quartz with petroleum sulfonate in the presence of activators and stressed the importance of iron in the flotation of beryl. From the studies conducted in this laboratory, it was found that feldspar and quartz as such do not float with sodium oleate, but in practice selective flotation of beryl from feldspar and quartz in an ore is found to be impossible with sodium oleate as collector. A glance at the chemical analysis of typical beryl ore indicates the presence of several ions like Ca ++, Mg++, Al + + + and Fe+++ in abundance and Ti++++ and Mn++ in traces. Hence, in an attempt to explain the behaviour of feldspar in the beryl flotation, the effect of Ca++, Mg++, Al+++ and Fe+++, which are known as gangue mineral activators7'8 has been investigated. Materials and Methods: Lumps of beryl ore (hand picked) were boiled with 10% sodium hydroxide and washed with distilled water. They were further boiled many times with 10% hydrochloric acid till no positive test for iron was obtained with ammonium thio cyanate. This was followed by thorough flushing with double distilled water. The lumps were crushed in a porcelain mortar and pestle under water. The minus 65 + 100 mesh fraction was used for testing and was always stored under distilled water. Pure feldspar and quartz were similarly prepared and the minus 65 + 100 mesh fractions collected. Inorganic ions tried as activators were ca++, Mg++ , Fe++, Fe ++ and A1 +++ . Calcium nitrate, magnesium chloride, ferrous ammonium sulfate, ferric ammonium sulfate and aluminum nitrate of G.R.E. Merck grade were used. B.D.H. technical grade sodium oleate was used as a collector. The vacuumatic flotation technique developed by Schuhmann and Prakash was used for studying the effect of pH on flotability. 7 The indications given by this work were confirmed by using 10 g miniature cell.'

Jan 1, 1965

By David Mitchell

MANY of the difficult operating problems of the preparation of coal for market, of sampling coal shipments and in the utilization of coal are caused by segregation in the coal mass. Segregation may be of two kinds: i.e., "size segregation," in which parti- cles of the same size in a mass of coal containing a range of sizes collect to-gether and "density segregation," in which particles of the same density or specific gravity in a mass of particles of varying density gather together. MECHANICS OF SEGREGATION Size segregation cannot take place with closely sized coal. As the size range increases, the tendency for size segregation increases. Similarly, cleaned coal with particles of approxi- mately the same specific gravity have very little tendency for density segrega- tion. The wider the density range of particles and the more particles of different density, the greater the chances are for density segregation. FIG. 1.-SEGREGATION IN A SIDE-FILLED The following discussion deals primarily BIN with coal of a wide size range as screenings and of wide density differ-ences as uncleaned or run-of-mine screenings. If a mass of coal containing particles of a wide size range is subject to the stream action of a moving current of water, the small particles are transported farther than the coarser. Particles of different density in a stream of moving water are subject to the laws of classification, the heavier settling out first. The familiar sluice box of the gold miner and the action of rivers and other streams in classifying material according to

Jan 1, 1937

The Mississippi river was discovered by French explorers that came southwestward, by way of the Great Lakes, from eastern Canada. Vignan, Joliet, De Champlain, and others of the French pioneers in the first half of the seventeenth century, dreamed of a short cut to China by means of the great waterways they explored. In a geographical book published in London in 1726 by Daniel Coxe an account is given of "a new and curious discovery and relation betwixt the river Meschachebe [Mississippi] and the South Sea, which separates America from China, by means of several large rivers and lakes". Louis Joliet, a fur-trader, and Jacques Marquette, a Jesuit missionary, reached the Mississippi and paddled their canoes on its broad waters on June 17, 1673.* They descended the river as far as the entry of the Arkansas tributary, and then returned overland to Canada, being deterred from going farther south by reason of Indian hostility. Several years later Robert de La Salle, a French trader, starting from Quebec, went westward to Lake Michigan and thence to the Illinois river, which he and his comrades descended in their canoes to the junction with the Mississippi, and then followed it to the sea. They reached the Gulf of Mexico on April 9, 1682. Thus the great central waterway of North America was made known. These French-Canadian voyageurs, or boatmen, traded with the Indians for furs in the Upper Mississippi valley, and when in need of bullets they noticed the outcrops of lead ore, from which, probably in the last decade of the seventeenth

Jan 1, 1932

By C. E. Beecher

The application of gas or air under pressure to obtain more oil from a sand which has been practically exhausted by ordinary production methods has been practiced to a limited extent for many years. Until recently such methods were confined to the Eastern fields, principally those of Ohio and West Virginia, where in many cases the production obtained after applying pressure for a few years was nearly equal to the total production prior to that time which had been obtained by the usual production methods. As early as 1917, J. 0. LewisL called attention to this method of increasing the recovery of oil and cited the phenomenal results obtained by H. E. Smith, I. L. Dunn and 0. C. Dunn, who pioneered the application of air or gas pressure recovery methods. With this information available it would appear that other oil-producing sections of the country have been extremely slow to realize the advantages of repressuring. However, after a few successful projects in the Mid-Continent area, the oil producers appreciated t' e value of this method for obtaining further and profitable production from their practically exhausted leases and are now making extensive use of it. In general, it has been the practice to apply pressure to the sands when production has declined to a small yield per well. The purpose of this paper is to discuss some of the advantages which may be expected from returning gas under pressure to the oil sands during the early stages of development, before the rock pressure has been dissipated and the gas exhausted, and to stimulate discussion of this subject on which comparatively little actual field data are available. The Function of Gas Gas associated with or dissolved in the oil is the source of energy causing movement of the oil to the well. When this energy is dissipated production ceases. The exception to this general statement is found in fields where hydrostatic water pressure may supply energy after the gas

Jan 1, 1929

By Fred DeVaney

THE coercimeter, as its name implies, is an instrument for measuring the coercive force? of magnetic substances. It was developed by Davis and Hartenheim in the Special Studies Section, Metallurgical Division. A detailed description of this apparatus may be found elsewhere.2 The coercive force determinations of magnetic materials are inter-esting because of the relationship established by Gottschalk,4 who showed a linear relationship between the magnetization coercive force and the specific surface of comminuted particles. The value of this relationship in determining grinding efficiency has been shown by Dean.3 The determination of the surface contained in the subsieve sizes has always been a difficult problem for investigators. They made approximate measurements of the surface of coarse materials by sizing on screens, but for the determination of the surface of the sub-sieve sizes it was necessary to make detailed grain counts or, elutriation tests, or to study dissolution rates. The technical literature contains many references to other methods for determining these surfaces, either by some special apparatus or by mathematical calculations based on distribution lines. Many of the methods are long and tedious, and the results of some, at least, are questionable. The turbidimeter gives quick results on ground cement. By using magnetite as the material to be ground, a simple determina-tion of its coercive force by the coercimeter, requiring 10 minutes or less, can be transposed directly and accurately into units of relative surface. This subject has been pursued further by the U. S. Bureau of Mines in cooperation with the Missouri School of Mines and Metallurgy, Rolla, Mo., and the following is a description of the results.

Jan 1, 1938

By R. P. Heuer, Paul M. Tyler

THE literature on refractories, although fairly extensive, is so scattered through books and periodicals as to be difficult of access to the general reader and most of the individual papers serve merely to illuminate some particular phase of the industry. Two general treatises by American authors8.16 are available, also the somewhat older works by a well-known British authority, 12,13 but these make their appeal to the technically minded ceramic engineer. Another small group of publications deals with the use of refractories, mainly in the iron and steel industry.1, 3,5,6,11,15 Raw materials utilized by the refractories industry have been covered by sundry books and articles. For the relatively nontechnical reader and economist, however, there appears to be no single review that purports to describe the industry as a whole. Furnace linings and other products that are classed as "refractories" are designed primarily to withstand high temperatures but this important property is by no means the only requirement; a suitable refractory material must likewise withstand slagging (chemical' action), abrasion (physical wear), and spalling, as well as the various other stresses and physical phenomena induced by heat, of which softening or incipient melting is only one phase. Nevertheless, subject to these highly practical considerations, the definition of a refractory material is based upon temperature resistance. Broadly speaking, any material that shows obvious signs of fusion after being heated slowly to 1500°C (2732°F) cannot be classified as a refractory material. The characteristic properties and requirements of refractory materials are conveniently summarized in Fig 1, prepared on the American Refractories Institute Fellowship at Mellon Institute, Pittsburgh, Pennsylvania. Most of the factors of service and properties of refractories given in this chart are interdependent and are greatly affected in degree by the functions of temperature and time. The factors in the chart are believed to cover the commoner questions.

Jan 1, 1949

By Richard N. Hunt

Bingham has produced 6 per cent. of this country's copper. In total production, it ranks fourth among the copper camps of North America, the order being Butte, Michigan, Bisbee, and Bingham. In its annual production, it held that same rank until 1919, when its production was exceeded by the combined production of the Globe-Miami district of Arizona. Bingham has also been a lead camp of the first order. Utah ranks third among the lead-producing states, and its production comes largely from three camps which, in the order of their productivity, are: Bingham, Tintic, Park City. Bingham's silver production is important, but it does not rank high as a silver producer. Utah owes its rank as first among the silver-producing states to Tintic, a camp 40 miles due south of Bingham. The United States Mineral Resources reports a total production from Bingham for the period 1865-1920 having a gross value of $528,043,432. History of the Bingham District Bingham is on the eastern flank of the Oquirrh range 30 miles southwest of Salt Lake City, from which it can be reached in an hour by auto, or by the Denver & Rio Grande or the Bingham & Garfield railroads. The automobile route is a paved road across the floor of Great Salt Lake Valley, through farming country. The Bingham & Garfield railway leaves the level of Great Salt Lake at the northern end of the Oquirrh range, and in 20 miles it climbs 2100 ft., and deposits the traveler upon a shelf cut in the side of Bingham Canyon below most of the mines, which are farther up Bingham Canyon and its tributary Carr Fork. Below lies the town, a narrow ribbon running for a couple of miles along the bottom of a canyon 2000 ft. deep—an almost impossible site for a community numbering, in prosperous times, 5000 to 7000 inhabitants drawn from all quarters of the globe. Up the canyon and down, and beneath the steep slopes nearby, and beneath the town itself, are the mining operations of over half a century. During the past two decades one mine, the Utah Copper, has become so gigantic an operation as to dominate all other activity in the camp. It has become the greatest copper mine on the continent in production,

Jan 1, 1924

By L. R. van Wert

CAREFUL research into the nature of the metallic state has yet to discover, with any certainty, its essential quality. We do riot yet know, for sure, what it is that makes the metallic elements different from, if not actually unique among, all created things. We do know, of course, that metals have certain more or less characteristic properties-they are hard, strong, and tough, and good conductors of heat and electricity, and these so-called metallic properties provide a definition of a sort. How- ever, it is the structure rather than the behavior of the metals which gives the really fundamental information necessary to the understanding of metallicity. But this information is not easily obtained. Nature has a way of keeping secrets. But happily we do possess some knowledge of how a metal is built up, and it is this matter, rather than the presentation of a formal definition, that will be discussed here.

Jan 1, 1937

By Thomas Leonard Watson

Sulphide ore-bodies of more or less lenticular shape occurring in metamorphic crystalline schists, gneisses, and slates, and conforming closely in strike and usually in dip to the inclosing rock, have been recognized and described along the Atlantic seaboard from Quebec to Alabama. The ore-bodies do not entirely conform, in all cases, to the structure of the inclosing schists, but they sometimes cut across the foliation in dip, though conforming more closely with the direction of strike. In composition the principal sulphide mineral is usually py-rite or pyrrhotite, or both, accompanied by copper, frequently gold, and almost always some sphalerite and galenite. Other metallic ores are, so far as these sulphide bodies have been investigated, less common; silver is not uncommon, and in some of the pyrrhotite masses nickel is present in quantity sufficient to be commercially valuable. Cobalt frequently accompanies the nickel, usually in smaller amount, and the two vary much in relative proportion. Quartz and calcite are probably the most common of the non-metallic minerals. A number of silicate minerals are frequent representatives in one place or another ; garnet, am phi-bole, biotite, pyroxene, zoisite and others. The sulphide bodies of Virginia, comprising both pyrite and pyrrhotite, are among the most extensive along the Atlantic seaboard. Among the pyrite bodies may be mentioned the well-known and extensively worked mines of Louisa and Prince William counties, located on the main pyrite belt (A, Fig. 1) of the middle and northern, eastern Piedmont region in Virginia, and among the pyrrhotite bodics is the famous " Great Gossan Lead" (13, Fig. 1) of the Floyd-Carroll-Grayson coun-

Jan 1, 1908

By A. R. Anderson

UNTIL recently all discussions directed at justify-ing the use of mechanical-loading equipment and conveyors have referred chiefly to tons per man and cost per ton. But there is another consideration that ? will speed the adoption of mechanical loading in mines even though tons per man on present day stand-ards were not increased nor the cost per ton decreased. With restricted immigration, improved facilities for education in our mining communities, and increased opportunities for recreation, the type of man who can or will throw 20 tons of coal per day over the side of a mine car is disappearing. Whether we will it or not provision must be made to replace muscular effort by mechanical means. Fortunately, indications are that the process will be accompanied by increased output per man and lower production cost, and though the outlook may now be a bit clouded in spots, all should profit by the change. The operator should enjoy a more stable business with more assured profit, the miners should get a better livelihood with less arduous effort and under safer and pleasanter working conditions, and the consumer should gain the assurance of a supply of coal always available at reasonable prices. That sounds like the millennium in the coal business perhaps. Of course, it is not, but there is just enough of that millennium stuff in it to encourage those of us who are working with today's problems of applying loading and conveying equipment to underground opera-tions. If we discern clearly that there can be no back-sliding, and that all will share in whatever advantages accrue, we will carry on more vigorously, and may right-fully expect to have the necessary cooperation of all the elements within the industry. As nature does not seem to have followed a definite plan in the formation of coal deposits it is not likely that any one standard method or type of equipment can be evolved for mining the coal. The method of mining that maybe most advantageously employed with load-ing machines and conveyors depends on the character of the strata overlying the coal as much as anything else.

Jan 4, 1927

By James E. Harding

The usual method of sampling mineral deposits is to drill holes and assay the sludge or core. Though the results thus obtained may not represent the true average value of the deposit, it is on these results that estimates of practically all large orebodies are made. In a large number of cases, the results of exploitation fall far short of the estimated value of the orebody. The standard method of making these estimates is to find the cubic contents of triangular prisms, in the apexes of which the drill holes are placed, by. multiplying the surface area by the average depth of the ore in the three drill holes and then multiplying the cubic contents by the specific gravity of the ore or rock to find the tonnage. The assay value is found by dividing the sum of the products of the depth of ore in each hole and the corresponding assay value by the sum of the depths of the ore in the three holes. As the latter part of this method is subject to many mathematical errors, it should not be depended on. Some engineers, therefore, use a discount factor, but as this factor is either arbitrarily selected or is obtained by obscure methods, the results are no better than guesswork. The standard method is correct when the drill holes are so laid out that the triangular prisms are equilateral in cross-section. But as ore deposits cannot always be drilled into at regular intervals and because of the human factor, if many holes are drilled, triangular prisms of all degrees of angularity are produced. In such cases it is necessary to assume that the influence of the different holes is not the same in all directions, which assumption of course is absurd. The area of the triangular prism is usually found by scaling; an ore-body of sufficient size to justify churn drilling is too large to be handled conveniently on maps having a scale larger than from 1000 to 1 to 1,500 to 1 and maps of such scales cannot be accurately measured. A variable is thus introduced in the first operation. In addition, the scaling is frequently done from blueprints, which sometimes shrink as much as 4 per cent. between printing, washing, and drying. The error due to scaling may be eliminated by surveying the location of each hole and

Jan 1, 1922

By Carl A Zapffe, George A. Moore

In a previous publication from this laboratory1 the conclusion was drawn that the embrittling effect of occluded hydrogen on iron and steel must result from the precipitation of the gas within small openings through the crystal structure. A review of the literature then published indicated the real existence of crystal substructures of the mosaic type and gave presumptive evidence that the "rift openings" associated with hydrogen occlusion are the same as the L'disjunctions" of the mosaic theory. Inasmuch as no clear conception of the actual nature of the crystal fragments and openings inherent in these theories has been established, it was considered desirable to obtain direct micrographic evidence of their true configuration. In this direction the standard methods of metallographic attack have proved useless. Recourse was had, therefore, to the direct examination of the surfaces upon which failure by cleavage had resulted from the presence of hydrogen. It was expected that such a surface, unaffected by chemical attack and undis-torted by polishing, would reveal the fine openings penetrated by the gas and thus indicate the real nature of the substructures. Materials Studied In commercial steels, defects caused by hydrogen take various external forms according to such factors as structure and purity, and to the extent to which hydrogen either occludes or produces chemical changes. The present work relates only to the well-known transcrystalline hydrogen embrittlement—-"pickling brittleness "—in which elemental hydrogen occluded within the grain develops cleavage characteristics. For example, hydrogen embrittlement resulting from hydrogen reaction products is excluded from detailed study. It was also desirable, as far as possible, to have the study uncomplicated by other elements which themselves cause brittleness. Three types of iron were used. These included ingot iron, decarburized free-machining steel, and a specially prepared, aluminum-killed, electrolytic iron. This choice allowed a comprehensive selection of unavoidable minor impurities and inclusions, which could subsequently be shown to have no specific effects on the structures within the grains. Carbon, and any other impurities free to react with hydrogen, were first removed by a preliminary annealing treatment in hydrogen. Subsequent treatment in vacuo extracted much of this hydrogen and its gaseous reaction products. The resultant ductile iron was then embrittled either by a second anneal in hydrogen, followed by rapid cooling, or by cathodic electrolysis. Group 1: Prepared from Armco Ingot Iron As shown in Table 1, the principal impurity in this iron was oxygen, which survived the purifying treatment to a large extent. Two series were prepared. The first (Nos. SIO-24) was purified only one day in hydrogen and dehydrogenized one day in nitrogen. Containing both hydrogen and its

Jan 1, 1943

By Carl A. Zapffe, George A. Moore

In a previous publication from this laboratory1 the conclusion was drawn that the embrittling effect of occluded hydrogen on iron and steel must result from the precipitation of the gas within small openings through the crystal structure. A review of the literature then published indicated the real existence of crystal substructures of the mosaic type and gave presumptive evidence that the "rift openings" associated with hydrogen occlusion are the same as the L'disjunctions" of the mosaic theory. Inasmuch as no clear conception of the actual nature of the crystal fragments and openings inherent in these theories has been established, it was considered desirable to obtain direct micrographic evidence of their true configuration. In this direction the standard methods of metallographic attack have proved useless. Recourse was had, therefore, to the direct examination of the surfaces upon which failure by cleavage had resulted from the presence of hydrogen. It was expected that such a surface, unaffected by chemical attack and undis-torted by polishing, would reveal the fine openings penetrated by the gas and thus indicate the real nature of the substructures. Materials Studied In commercial steels, defects caused by hydrogen take various external forms according to such factors as structure and purity, and to the extent to which hydrogen either occludes or produces chemical changes. The present work relates only to the well-known transcrystalline hydrogen embrittlement—-"pickling brittleness "—in which elemental hydrogen occluded within the grain develops cleavage characteristics. For example, hydrogen embrittlement resulting from hydrogen reaction products is excluded from detailed study. It was also desirable, as far as possible, to have the study uncomplicated by other elements which themselves cause brittleness. Three types of iron were used. These included ingot iron, decarburized free-machining steel, and a specially prepared, aluminum-killed, electrolytic iron. This choice allowed a comprehensive selection of unavoidable minor impurities and inclusions, which could subsequently be shown to have no specific effects on the structures within the grains. Carbon, and any other impurities free to react with hydrogen, were first removed by a preliminary annealing treatment in hydrogen. Subsequent treatment in vacuo extracted much of this hydrogen and its gaseous reaction products. The resultant ductile iron was then embrittled either by a second anneal in hydrogen, followed by rapid cooling, or by cathodic electrolysis. Group 1: Prepared from Armco Ingot Iron As shown in Table 1, the principal impurity in this iron was oxygen, which survived the purifying treatment to a large extent. Two series were prepared. The first (Nos. SIO-24) was purified only one day in hydrogen and dehydrogenized one day in nitrogen. Containing both hydrogen and its

Jan 1, 1943

By P. G. Shewman, T. L. Wilson

Using published surface-diffusion (D,) data and published sintering equations, it is shouln that surface difusion should dominate the neck-growth stage of intering for all materials in which D, has been measured (six metals and A1as). Also, grain boundary diffusion can be expected to contribute appreciably to shrinkage and possibly to neck growth below some critical temperature of the order of 70 pct 01- the absolute melting temperatuve. In view of the widespread conclusion in previous sintering work that volume diffusion dowzinates neck gvowth, experiments were conducted using spherical copper powders to test this conclusion. Scaling studies on neck growth at 950°and 1020°C clearly demonstrated that suyface diffusion dorninates. Kinetic studies on shrinkage gave more equivocal results that indicated an increasing role of' grain boundary transport at lower temperatures. Five diarszeters from 100 to 300 u were used in the scaling sludy and a temperature range of -650' 10 950 C was covered in the shrinkage studies. All experiments were conducted in dvy hydrogen. In 1949, Kuczynski published his now classic paper on the determination of the transport mechanism in sintering from the time laws of neck growth. In the interim, these laws have been applied to many systems and slightly modified by several authors. Essentially all these authors concluded that, for crystal- line materials, the dominant transport mechanism in neck growth is volume diffusion. This stems from the observation that the neck radius increases about as t"5 and that the activation energy approximates that for lattice diffusion. A related but independent series of studies stems from Mullins' rigorous analysis of the growth of the groove formed where a grain boundary meets a free surface." xperimental work stemming from this analysis has shown that for each crystalline material studied (Au, Ag, Cu, Ni, Fe, Pt, Al2O3) surface diffusion was clearly the dominant transport mechanism for groove widths up to the order 10 to 20 p. The ratio of the quantity of material being carried by lattice diffusion to that carried by surface diffusion increases linearly with the groove width, so surface diffusion is dominant for all widths under 10 to 20 u. The analysis of the relative contributions of surface and volume diffusion to grain boundary grooving, and to neck growth in sintering, shows that they are quite similar. Thus, using the available surface-diffusion data and the approximate equations of Kuczynski, or the more rigorous recent equations of Nichols and Mullins, 3 it can be shown that the small necks between particles must grow almost entirely by surface diffusion. The purpose of this study was to re-examine the basis for the conclusion that the neck-growth stage of sintering proceeds by volume diffusion. Using spherical copper powders, of several different diameters, precise experimental measurements were made of both neck growth and shrinkage. Application of Herring's scaling laws to the neck-growth data clearly indicated that neck growth occurred by surface transport, even though the neck radius increased as or Using the recent analysis of Mullins and Nichols as well as published data on surface diffusion, it is shown that the observed time law, as well as actual rate of neck growth, can be satisfactorily explained by a surface-diffusion mechanism.

Jan 1, 1967