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By G. K. Manning, E. R. Stein, E. E. Underwood

Columbium, carbon. and nickel additions were made to iron-base alloys with 20 pct CY. The effects on microstructure, precipitation-hardening characteristics, and High-temperature properties were investigated by means of metallographic, hot-hardness, and magnetic measurements. An austenitic alloy consistilzg of Fe-20Cr-14Ni-0.8C-2.5Cb had higher hot-lzaciness at 1700°F than the other alloys investigated. Its favorable standing is attributed to an enhanced interaction of Cb and Cr4C particles dispersed within a stable austenitic matrix. FOR the past 20 years, cobalt- and nickel-base alloys have been used for the more stringent high-temperature applications because of their excellent creep resistance. Although their performance is quite satisfactory, other base materials must be considered for large tonnage, low-cost applications such as for the automotive gas turbine. Iron-base alloys are also used extensively, but at somewhat lower temperatures, primarily because of the instability of particles or because precipitation occurs at relatively low temperatures. Since unusual stability has been reported for Fe-Cb and Cb-C compounds.1-3 it was hoped that effective amounts of these compounds could be taken into solution at temperatures just below the melting range, then precipitated upon reheating. Actually, strengthening was found to occur by both precipitation hardening in some alloys and by phase transformations in others. Among the alloys investigated, that with the best high-temperature properties owes its strengthening to a combination of carbide particle interaction and a relatively stable austenitic matrix. EXPERIMENTAL PROCEDURES Small preliminary melts of about 100 g were made in a vertical Glotube furnace, using alundum crucibles and an argon atmosphere. Alloys weighing 35 lb were melted in a basic-lined induction furnace, also under argon. The compositions of the alloys are given in Table I. The nickel-free alloys were usually ferritic, while those containing nickel were generally austenitic. Depending upon the particular heat treatments, or the combination of alloying elements, two-phase alloys of ferrite and austenite could be obtained. In the following text, however, the nickel-free or nickel-bearing alloys are referred to simply as either ferritic or austenitic alloys respectively. The small ingots were swaged at 2000°F, in steps, to rods of approximately 3/16-in. diam. The large ingots were forged at 2100°F to 1-in. sq bars. No difficulties were encountered in swaging or forging any of the alloys to as much as 90 pct reduction in area. For heat treating at temperatures above 2000°F, specimens were sealed in quartz tubes under a partial pressure of helium. No special precautions were found to be necessary at lower temperatures. Intermetallic compounds in the preliminary alloys were identified by means of X-ray diffraction measurements. Correlation of these results with micro-structural characteristics (such as color, shape, size, and location) of the compounds aided in their identification. Magnetic susceptibilities were also obtained at room temperature with a Magne Gage instrument after the various heat treatments. To

Jan 1, 1962

By Robert F. Stewart

The oxidation of structural materials at high temperatures in gas-cooled systems can be greatly retarded by the addition of small amounts of hydrogen to the inert coolant. In experimental equipment for gasifying coal with heat transferred by helium, the oxidation of graphite and metals (molybdenum, tungsten, and certain stainless steels) by trace impurities in the coolant helium was virtually eliminated by adding 0.1 to 1.0 percent hydrogen. The reaction of hydrogen with praphite does not preclude its use to retard oxidation; at 2,400° F. only 0.2 pound of graphite per square foot per year is lost for each percent of hydrogen in the helium. The addition of hydrogen appeared to prevent the mass transfer of carbon often associated with oxidation of graphite, without causing noticeable embrittlement of stainless steels and molybdenum or other damaging effects. This method has been tested in precision gas-recycle systems and applied successfully for more than a year in a pilot-scale unit operating at 250 pounds per square inch gage and 2,400° F. It is now used routinely and can be applied to many gas-cooled systems operating at high temperatures.

Jan 1, 1962

By C. M. Wayman, J. F. Breedis

The crystallography of the martensitic transformation in the Fe-30 Ni alloy was reinvestigated. The scatter in the habit Plane as determined from measurements on the mid-rib plane was smaller than reported previously, and the orientation relationship was determined from a martensite plate having known direction cosines. From agreement with crystallographic theory and from observations of the morphnlogy of the martensite plates, it is suggested that the mid-rib plane represents the starting region of the transformation. THE crystallography of the martensitic transformation in the iron-nickel system has been the subject of many investigations.&apos;-7 However, for iron alloys containing approximately 30 wt pct Ni, a wide scatter in the reported habit planes exists. In only one instance has a Laue determination of the orientation relationship been made, but the habit plane of the martensite plate studied was not determined experimentally. Because the most successful thermodynamic and kinetic analyses8 of the martensite transformation have been based on Fe-30 Ni alloys, it was considered desirable to reinvestigate the crystallographic features of the transformation in this alloy. Lieberman9 suggested that the most significant information for use in a theoretical treatment involves the determination of all the crystallographic observables from a single plate of the product phase. This was first done in essence by Greninger and Troiano10 for Fe-22 wt pct Ni-0.8 wt pct C, and is the method followed in this investigation. Some theoretical approaches11-13 in describing the martensitic transformation consider the overall transformation distortion to be comprised of a Bain distortion, or lattice deformation (PI, which produces the structure change, and a lattice invariant deformation (G), such as twinning, which together leave the interface or habit plane un-distorted. The incorporation of a rigid body rotation (R) results in a transformation distortion (E) such that the interface plane is left both undistorted and unrotated. In matrix notation, E = RPG where the lattice invariant deformation has "taken place" in the austenite. Bowles and Mackenzie14-16 in formulating a theoretical approach proposed an adjustable scaler quantity, denoted as 6, which represents a uniform dilation in the interface plane. This dilation acts to adjust the lattice spacings of the parent and product structures at the plane of contact. Using the dilation parameter as a variable, these authors were able to account for a continuous variation of habit planes in steels along a curve in the stereogram between {225}A and {259}A. she invariant line strain14 of the transformation is 6 RP, and the corresponding transformation distortion is E/6.) With the dilation parameter known, the invariant line is computed as the triple coincidence of the habit plane, the shear plane of the lattice invariant deformation, and the initial Bain cone.14 The contraction axis for the Bain distortion can be taken9&apos;17 as [010]A, and the correct permutation of the habit plane indices used. Kelly and Nutting 18 have established the shear plane (of twinning) in the tetragonal martensite of Fe-22 Ni-0.8C to be {112)M by means of transmission electron microscopy. The reasonable shear system is then {112}M which is equivalent to {011}A <01l>A. The as-

Jan 1, 1962

By K. J. Gill, P. Chiotti

Thermal, metallographic, and vapor pressure data were obtained to establish the phase diagram for the thorium-zinc system. Four compounds corresponding to the stoichiometric formulas Th2Zn, ThZn2, ThZn4, and Th2Zn17 were observed. The melting points of these compounds under constrained vapor conditions were found to be 1055°, 1105°, 1095°, and 1015°C respectively. Four eutectics exist in this system with the following eutectic temperatures and thorium contents in wt pct: 1040°C, 89 Th; 945°C, 79 Th; 1045°C, 55 Th; and 995°C, 35 Th. The standard free energy, enthalpy, and entropy of formation for the compounds were determined from zinc vapor pressure data. ALTHOUGH the thorium-zinc system has been of technical importance in the commercial production of thorium and more recently of interest to some proposed pyrometallurgical separations processes for reactor fuels or blanket materials no detailed investigation of this system has been made in the past. Some previous work has been reviewed by Hanssen.1 The existence of four compounds, Th2Zn17, ThZn4, ThZn2, and Th2Zn has been established and their crystal structures have been studied by X-ray diffraction techniques.2-4 Smirnov et al.,5 determined the solubility of thorium in zinc and investigated the two-phase region between Th2Zn17 and zinc. They calculated some of the thermodynamic properties for these alloys from emf measurements on the cells Th/ThCl4(fused)/Cl2, C and Th2Zn17(s)+ Zn (l)/ThCl4(fused)/Cl2, C. The possibility of reaction between the anode materials and fused thorium tetrachloride to produce a lower valent thorium salt would have to be resolved in order to evaluate the results obtained. The purpose of the present investigation is to establish the phase diagram for the thorium-zinc system and to determine the standard free energy, enthalpy, and entropy of formation for the compounds formed. MATERIALS AND EXPERIMENTAL PROCEDURES The metals employed in the preparation of alloys were Bunker Hill slab zinc, 99.99 pct pure and Ames Lalboratory thorium. The major impurities in the thorium in parts per million were oxygen—1250, carbon—350, iron—100, nitrogen-75, and silicon—70. The metals in the form of several small massive pieces, total weight about 30 g, were cleaned with acid, washed with water and acetone, and dried just prior to their use for alloy preparation. Tantalum containers were found to be suitable for all the alloys studied and were used throughout this investigation. The metals were sealed inside of small 1-in.-diam tantalum crucibles by welding on preformed tantalum covers. A small thermocouple well made from 1/8-in.-diam tantalum tubing was welded in the bottom of each crucible. These crucibles were enclosed in

Jan 1, 1962

By Willard L. Hunter

The research described in this Bureau of Minus report was conducted to improve the chromium-iron ratio of offgrade chromite. Two methods were used: (1) Iron was selectively reduced from chromite by carbothermic reduction in an electric-arc furnace, and (2) a mixture of carbon, chromite, and sometimes fluorspar was chlorinated to remove a substantial part of the iron. Chromite concentrate from the Mouat deposit in Montana and from northern California was used in the test work. Chromium-bearing slag and chromite that had been beneficiated by a roast-leach process were each smelted to produce high-carbon ferrochromium. Iron was selectively reduced in a laboratory-scale., electric-arc furnace. Carbon additions to the smelting charges varied from 40 to 100 percent of the stoichiometric requirement, and slag basicities were varied from 0.4 to 1.0 chromium-iron ratios of more than 4:1 were obtained with 89 percent recovery of chromium in a chromium-bearing slag.

Jan 1, 1962

By D. S. Robertson

More than 700,000 feet of diamond drilling was completed in the Blind River area between 1953 and 1958. Much of this drilling was at depths which are still not usual in North America. However, as the tendency is to deeper holes, factual data from the Blind River operation may well provide information of value in future programs. Rates of drilling decreased with in-creasing depth, but uncommonly good rates (an average of over 50 feet per day over more than 4,000 feet of hole) were achieved with proper engineering and care. Costs varied as contractors and geologists became familiar with the area Hole deviation in the Blind River area was locally severe and control of the hole trace became a major problem. Careful surveying was necessary and found to be highly re-liable. It was found that control of the hole trace above 1,500 feet was much more difficult than at depths below 1,500 feet. This is explained by the mechanics of the drilling operation. Various methods of controlling hole deviation were attempted and,

Jan 1, 1962

By E. D. Calvert

The objective of this research was to examine variations in melting and forging practice for four titanium-base alloys and to determine their effect on the resultant product. Of particular interest was the evaluation of the skull-casting technique. The data should serve as a guide to producers and consumers of titanium products. Physical properties of four titanium-base alloys in ingot form and in sheet form were evaluated and correlated, where possible, with variations in the melting and casting procedure. Consumable-electrode melting was used throughout, but arc current and furnace backfill pressure were varied, and ingots were formed both by melting directly into a water-cooled copper mold and by skull melting followed by pouring into a graphite mold. Alloying metal additions for the alloys tested were (1) 8 percent manganese, (2) 6 percent aluminum and 4 percent vanadium, (3) 6 percent molybdenum and 2 percent aluminum, and (4) 16 percent vanadium and 2.8 percent aluminum.

Jan 1, 1962

By Leonard Obert

Between 1927 and 1957, sodium borate minerals were mined by underground methods in the Kramer District, Kern County, Calif. In 1957, surface mining methods were initiated, and during the next two or more decades it is probable that most of the production from the district will be obtained from open pits. However, part of this borate deposit is sufficiently deep that surface mining may not be economical and, hence, at some future date underground methods may again be employed. This report was prepared to document the underground mining methods employed in the district before 1957. The general geology of the district and the detailed geology of each of four mine sites are presented, together with a mineral and mechanical description of the ore and enveloping rock. The report also describes the stoping, extraction, pillar support, methods of artificial support, and other factors that affect the structural characteristics of these mines.

Jan 1, 1962

By G. H. Gronhovd

This report describes the design and initial operation of a slagging gasification pilot plant installed by the Bureau of Mines at the Lignite Research Laboratory, Grand Forks, N. Dak., in 1958-59. The tests covered in this report were conducted over a period of about 2 years, beginning in April 1959. The pilot plant was designed for eventual operation at pressures ranging from 400 to 600 p.s.i.g. (pounds per square inch gage); however, for the preliminary test reported here, the gasifier was fitted with a low-pressure slagging section and operated at atmospheric pressure and at 80 p.s.i.g. The reason for using a low-pressure slagging section for initial operation was to facilitate modifications in design during the development of a reliable slagging procedure.

Jan 1, 1962

By A. H. C. A. Zimmerman

WE have just heard what must be regarded as a thoughtful, constructive and somewhat painful analysis of the financial function of our industry. While thinking about this, it is interesting to reflect on the conditions which have stunted the growth of the financial side of our affairs. Mining must be regarded as a wealthy business. •while immeasurable grub takes and development budgets have been lost, there can be little argument that a productive ore-body nearly always produces the type of wealth that breeds some extravagance. I recognize that this statement can be attacked from many sides, but an historical comparison with a commercial enterprise involving similar investment will demonstrate what I mean. However, these old times are be-ginning to disappear for a variety of reasons. High amongst these are: ( l) Increased costs of exploration. (2) Remoteness of many new finds. (3) Fixed or declining metal prices (particularly when expressed in constant dollars). ( 4) Constant demands for higher wages.

Jan 1, 1962

The study of gas emitted from face coal samples at the coal face is part of an investigation of instantaneous outbursts of coal and gas. Normally, seam gas essentially comprises methane of which the origin in the metamorphism of coal is undoubted. The origin of other gases sometimes occurring in high proportion in seam gas, particularly carbon dioxide, is more controversial. A simple meter for rapidly assessing gas in coal was developed. Tests with the meter enabled comparisons of seam gas in face coal at some outbursting and nonoutbursting mines, and under various working conditions. The varying results of widespread testing suggest certain trends, including some prospect of recognising outbursting potential at the coal face.INTRODUCTIONThe aim of this work is identification of differences in gas condition between coals subject to instantaneous outbursts and coals which have not outburst, and between faces of coals which will and which will not subsequently outburst. Any comparative test should be conducted right at the coal face on coal about to be worked and the results of testing should be available after a short period. Moreover, the method and the comparison of results should require no special skill, and be well within the capacity of junior mine officials. Any consistent relation between gas condition and subsequent mining conditions - outbursting or not might be valuable in prediction of outbursts.INSTANTANEOUS OUTBURSTSInstantaneous outbursts (Hargraves, 1958) , are largely unpredictable and unaccountable ejections of coal (up to 5,000 tons) and gas (up to 5,000,000 cu.ft.) from a standing coal face. Usually the gas is essentially methane (CH4 ) but may be essentially carbon dioxide (C02 ), or an intermediatemixture...

Jan 1, 1962

By P. H. Riordon

ONE OF the major sources of the world's supply of asbestos lies in a belt of ultrabasic rocks stretching through the Eastern Townships of Quebec where chrysotile asbestos has been mined continuously since 1878. The productive portion of the belt extends from the town of Asbestos in Shipton town-ship northeastward some 60 miles to the eastern edge of Broughton town-ship. (See map). Twelve mines, currently treating an aggregate of over 60,000 tons of rock daily, produce more than one million tons of asbestos :annually. An equal number of mines are now dormant, having for the most part exhausted their reserves. It is evident from the past and present activity, in this belt that it can look forward to at least half a century or more of large scale production. The host rock to the asbestos de-posits is essentially a peridotite which originally contained I 0 to 15 per •cent pyroxene. The peridotite, associated with dunite, pyroxenite

Jan 1, 1962

By Kenneth M. Earl

This report describes the results of a field study conducted by the Bureau of Mines during 1956 and 1957 on manganese-and iron-bearing mineral deposits in the southern district of Aroostook County, Maine. The work was undertaken to determine the extent of deposits largely concealed under glacial drift and to obtain subsurface samples for manganese mineral identification and research in ore dressing and extractive metallurgy. The investigation was confined to the Westford Hill-Daggett Hill area in Hodgdon Township and to the Stewart prospects and vicinity in Linneus Township. Over 50 magnetic anomalies were mapped by magnetometric surveys in the Westford Hill-Daggett Hill area, Hodgdon Township. The largest anomaly, as outlined by the 1,000-gamma contour, indicates a deposit 3,200 feet long with a maximum width of 350 feet. The smallest anomaly measures about 10 feet wide by 25 feet long.

Jan 1, 1962

By J. B. Malcolm

The discovery of tungsten-bearing quartz outcroppings in Vance County, N. C., by the Hamme brothers in 1942, made international news in the mining industry and was, in fact, one of the major ore discoveries made in the U.S. during the last 25 years. Operations began at the Hamme mine in 1942, but after 16 years of successful operation, the mine was closed down in 1958 under adverse market conditions. By that time, it had produced nearly 20 million lbs of metallic tungsten. Because of the square-set timber mining method then in use, mine operating expenses were high, actually representing 78% of the total operating expenses at the property. In timber work alone, 160 men were employed. Approximately 500,000 bd ft of timber were placed monthly at a direct supply cost of $1.00 per ton of ore mined. Late in 1959, following a slightly improved position in the tungsten market, company management decided that, by changing the mining method, the operation could be economically feasible. The major premise in this decision was that a reduction of from 25 to 30% of the mining costs could be achieved by the conversion of the mining method from square-sets to horizontal cut and fill. Reopening of the mine began in February 1960, Full production has now been reached and overall mine productivity has been doubled.

Jan 1, 1962

By J. F. Enrietto

It is shown that one cannot approximate the broad internal friction Peaks observed in the Fe-Mn-N system as the sum of a number of subsidiary Peaks and still vetain the concept of a single relaxation time. Furthermore, the approximation of manganese affectirg only nearest neighbor interstitial sites is shown to be incompatible with the experimental results. The results of this experiment show that the influence of manganese in the ferrite lattice extends over 3 to 4 atomic distances. NUMEROUS experiments have shown that the presence of relatively small amounts of substitutional alloying elements can profoundly affect the profile of the damping spectrum in the vicinity of the Snoek peak in bee metals.1-7 Dijkstra and Sladekl observed this phenomenon in Fe-Mn-N alloys where it appeared as a broadening and shifting of the Snoek peak to higher temperatures. The authors interpreted this as being the result of a superposition of two damping maxima—the normal Snoek peak, located at its usual position and having a normal half-width, and an interaction peak having a normal half-width, but occurring at a somewhat higher temperature. They prclposed that the interaction peak was caused by nitrogen atoms jumping from Fe-Mn sites to Fe-Fe sites, the Fe-Mn interstitial sites having one manganese and one iron atom as nearest neighbors, and the Fe-Fe sites having two iron atoms as nearest neighbors. They further suggested that the Fe-Mn sites had a lower energy than the normal Fe-Fe sites because of the presence of the adjacent manganese atoms. From the relative heights of the two postulated damping peaks, the dif-

Jan 1, 1962

By M. M. Wong

Beryllium possesses attractive properties for use in the nuclear and space fields. Since fused-salt electrorefining can be employed to produce this metal in high-purity form from low-grade or scrap metals, the Bureau of Mines investigated electrorefining of beryllium in electrolytes composed of a LiC1-KC1 eutectic mixture plus varying amounts of BeC12. Results showed a 99- percent or better reduction of oxygen and magnesium and a substantial reduction of other minor metallic impurities. Extremely pure beryllium metal was produced. Operating variables, including BeCl2 concentration in the bath (3.5 to 16.5 mole-percent), temperature of operation (450° to 550° C.), and cathode current density (45 to 770 a,/sq, ft.), were studied; their effects on the deposition of metal, working condition of the bath, and purity of the refined metal are discussed. The safety precautions used in handling beryllium in the laboratory are also described.

Jan 1, 1962

By Fred C. Bond

Any improvement in the accuracy of commercial comminution calculations under the Third Theory must be accomplished either by increased precision in energy input measurements, or by a better evaluation of the total new crack length produced, as indicated by the feed and product size distributions. Since at the present time feed and product sizes are approximated solely by the microns 80% passes, the most promising opportunity for increased accuracy lies in consideration of their plotted size distribution characteristics. This paper shows how more accuracy can be obtained over an increased range of feed and product sizes from size distribution studies.

Jan 1, 1962

By A. C. Elliott, A. J. Lafreniere

THE Hamilton Works of The Steel Company of Canada is a fully integrated steel plant with an annual capacity of three million tons. Located on the south shore of -Hamilton bay, it is in the centre of Hamilton's industrial belt. The heavy concentration of industrial activities found in this area, accompanied metallurgical well-known sources of pollution which are normal to urban areas is creating a pollution problem which concerns both industry and the general public. The Steel Company of Canada has recognized this problem and, accordingly, has adopted the policy of integrating suitable pollution control devices into its new installations. Much effort is also being expended to control the emissions of air contaminants from the existing equipment. At the Hamilton Works, there are two main sources of metallurgical dust emissions to the atmosphere -the Open Hearth furnaces and the Sinter Plant. Of these two, the Open Hearth furnaces are, undoubtedly, the largest single source of

Jan 1, 1962

By Eugene L. Grumer

High-expansion foam was applied to the flames of six fuels burning in a 1-foot-diameter tray. The flames of three hydrocarbon fuels were more readily extinguished than the flames of methanol, acetone, or unsymmetrical dimethyl hydrazine. The result is rationalized on the basis that heat transfer from flame to fuel surface is primarily radiative with the hydrocarbons and more largely convective with the nonhydrocarbons. INTRODUCTION Equipment for producing high-expansion foams has been developed by the Bureau of Mines to control coal mine fires.5 Recently such equipment has been redesigned for portability and has now been produced commercially for other fire-fighting applications. In May 1961, a 50-by 50-foot gasoline fire was extinguished within 2 minutes by a trailer-mounted foam unit that produced 12,000 cu.ft./min. of high-expansion (1,000:1) foam.6

Jan 1, 1962

By F. E. Brantley

Blister copper was successfully deoxidized with any of a variety of reducing gases; lancing techniques or a vertical-column furnace were used to contact the copper and gases. Of the gases tested, butane, when used to lance molten copper at about 1,200° C, reaction temperature, was slightly more effective than propane, natural gas, carbon monoxide, or reformed gas for deoxidizing copper from about 1.0 to less than 0.1 percent oxygen content, Laboratory-scale tests revealed that the vertical furnace, composed of a heated column packed with silicon carbide chips or hollow carbon cylinders, was significantly faster and more efficient than the lancing technique for deoxidizing molten copper with any of the gases tested. Comparison of the gaseous-reduction method with the conventional poling method suggests that the gaseous method has important technical and economic advantages for deoxidizing blister copper to any readily controlled amount of residual oxygen content.

Jan 1, 1962