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By Y. H. Liu, R. Kiessling

The chromium, iron, and tungsten borides have been treated with ammonia at different temperatures. They are attacked, forming metal nitride and boron nitride, and the results are summarized in the tables. In the tungsten-nitrogen system a new phase has been observed, closely related to the known ß phase. THE present investigations were begun to determine whether any ternary phases exist in the transition metal-boron-nitrogen systems for the metals chromium, iron, and tungsten. Attempts to prepare such phases were made by using the borides of the metals as starting materials and ammonia as the nitriding agent. Although no new ternary phases have been found to exist, the results may be of some interest with regard to the technical use of the borides. General Procedure A steady stream of dry ammonia was passed through a silica reaction tube, the central part of which was kept at the reaction temperature while its ends were water-cooled. Weighed amounts of the borides were placed in a silica or porcelain boat and heated at different temperatures for a period of 10 to 24 hr. The boat was then rapidly removed from the reaction zone to the quenching zone, the water-cooled end of the tube, by means of a simple magnetic device. The nitrogen content of the products was determined by the increase in weight of the specimens, and the phase analysis was carried out by X-ray methods. For this analysis a Guinier-type camera, constructed at this Institute, was used with a bent, ground quartz crystal monochromator. The general reaction, which occurred in all the experiments, may be summarized as: metal boride + nitrogen -* boron nitride + metal nitride For the higher temperatures pure metal was formed instead of metal nitride. It is sometimes difficult to Discussi detect boron nitride among the reaction products by X-ray methods. Prolonged exposures of some specimens showed, however, that the strongest reflections of boron nitride were present. Additional evidence for its presence was given by the increase in weight of the specimens after nitriding. This increase was always greater than that corresponding to nitride formation only and was often in close agreement with the formula given above. Finally, a white powder, which was shown by X-ray methods to be boron nitride, was left if the reaction products after nitriding Fe,B at 448°C and FeB at 768°C were dissolved in diluted sulphuric acid. Ch rom iu m - Boron - N itrogen Five phases have been found to exist in the Cr-B system,' , and all were used as starting materials. Investigations on the Cr-N system have shown the existence of two nitrides with ideal composition Cr,N and CrN.".' * The results are summarized in Table I. All the borides are attacked and decomposed into chromium nitride and boron nitride, and the kind of nitride formed depends only on the temperature and not on the boride used as starting material. The lowest reaction temperature, however, is different for the different borides. Thus the 6 phase begins to react at about 735 "C, the r phase at about 800°, the S phase at about 900°, the 7, phase

Jan 1, 1952

By W. M. Johns

The word "Flatland" should read "Flathead" in the title of the paper by Willis M. Johns on page 184 of the June 1962 issue. The correct title is "Belt Series in Lincoln and Southwest Flathead Counties, Montana." In the same paper, reference 12 on page 191, the publication is Bulletin 12, Montana Bureau of Mines and Geology, rather than Bulletin 17.

Jan 1, 1962

By William P. Blake

In my short " Contribution to the Early History of the Industry of Phosphate of Lime in the United States,"* mention is made of the erection by Dr. Emmons and myself of a magnetic machine for the removal of iron-ore from the so-called "red sand," a granular form of apatite. At the time of writing, it was not possible to refer to my diary and notes, and the general statements were made from recollection. The subject seems to have special interest at this time, by reason of the many forms of machines now being introduced and patented for similar purposes; and, having received letters of in quiry for further details, I have availed myself of the opportunity, when recently at home for a few days, to refer to the original notes and records made by me in 1852, when living at Crown Point and Moriah, on Lake Champlain. The machine mentioned in my former communication mas pur chased of Ransom Cook, of Vermont. It arrived, and was un loaded from the boat and taken part way up to the nine, on October 18,1852. The weight was 1400 pounds and the cost $1200. It was constructed, not with permanent magnets but with electro-mag nets. It was set up and first turned by hand on October 28th, using twelve battery-cups or cells, the connections being made with wires in small cups of quicksilver. The magnets were not sufficiently strong, and the machine did not work well. More batteries were sent for, arid the machine was started with steam-power on Novem ber 6th. The ore was dried in kilns, then put through a coffee-mill crusher or grinder, and then fed upon the leather belt which carried it under the magnets. Many experimental runs were made, and some diffi culties were overcome, before December 21st, when the record states that the machine was working pretty well, using 24 cells and giving a product of from 3 to 5 tons a day of granular phosphate. The ori-

Jan 1, 1893

By Betty M. Miller

INTRODUCTION In September 1974 the Resource Appraisal Group of the Branch of Oil and Gas Resources, U. S. Geological Survey, was asked to aid the Federal Energy Administration (FEA) in its legal responsibility to generate by June 1975 an independent appraisal of the undiscovered oil and gas resources of the United States, both onshore and offshore. As a result, the Resource Appraisal Group accelerated its ongoing efforts to develop sound appraisal methods and procedures that would permit the systematic collection and evaluation of basic data from petroleum provinces throughout the Nation. The results of this independent appraisal of the Nation's conventional oil and natural gas resources were published by the U. S. Geological Survey as Circular 725, June 1975 (1). The estimates in this report of undiscovered recoverable oil and gas resources for the United States were made: (1) by carefully re- viewing a large amount of geological and geophysical information gathered on more than 100 different provinces by over 70 geologists within the Survey; (2) by applying a variety of resource appraisal techniques to each potential petroleum province; and (3) by application of subjective probability procedures to group appraisals for each petroleum province. These methods provide a range of estimates which are summarized in terms of low, high and mean values for the various provinces and groups of provinces, or regions. The basic data and procedures used are documented and are being incorporated into a dynamic, data- intensive system that can be upgraded, updated and reevaluated periodically. These data are open to public inspection. In this study, the primary emphasis was placed on conventional crude oil and natural gas in the onshore provinces and the provinces on the continental shelf out to water depths of 200 metres; estimates

Jan 1, 1977

By James R. Holden, Frederick E. Wang

Through both single-crystal and powder X-ray diffraction methods, ten A6B23-type compounds have been confirmed to exist between lanthanides (A) (plus scandium and yttrium) and manganese (B); A = Y, Nd, Sm, Gd, Tb, Dy, Ho, Er, Tm, and Lu. The formation of a compound of this type is shown to he extremely atomic size-sensitive; hence it can be classified as a "size-factorH compound. The "enveloping effect", a geometrical consideration observed in its crystal structure, is proposed as the reason for the A6B23-type compound being size-sensitive. The approximate ideal geometrical ratio of the radii R/r is 1.31 while experimentally A6B23-type compounds have a radius ratio lying within the range 1.2 to 1.4. FLORIO t al.' characterized the structure of Th6MnZ3 as fcc, space group Fm3m, with 116 atoms in the unit cell. Since then, a number of isotypic binary compounds, and recently Gd n,,' have been confirmed to exist. The fact that strontium and barium form A6Bz3-type compounds with magnesium strongly suggested the possible existence of Ba6Liz3. However, investigation3 showed the compound Ba6LiZ3 to be absent. Since both strontium and barium are group 11-a elements and are therefore "open metals",6 the nonexistence of Ba6LiZ3 can hardly be explained satisfactorily by valence-electron considerations. On the other hand, the consistent atomic-radius ratio, (R/r),* observed for the known A6Bz3-type compounds,3 strongly suggests that the formation of compounds of this type is atomic size-sensitive. Therefore, one is tempted to explain the nonexistence of Ba6LiZ3 entirely on the basis of the atomic-size difference between strontium and barium. However, this approach is not entirely without objection. Atoms are not rigid spheres and are known to vary in size within certain limits.7 Since the atomic-radius difference between strontium and barium (0.07 to 0.09A) is within these limits, it is reasonable to assume that the size difference would have a negligible effect on the formation of Ba6LiZ3. This view is further supported by the fact that the radius ratio, R/r, in other known "size-factor" compounds is observed to range widely—for example, from 1.08 to 1.45 for ABz-type compounds (C15, MgCuz type)' and from 1.37 to 1.58 for AB5-type compounds (D2d, CaZn5 type).g The present investigation was undertaken in order to find a more satisfactory explanation for the non-existence of Ba6LiZ3 and, consequently, a better understanding of the nature of the A6Bz3-type compound. The primary objectives are to confirm the previous conclusion3 that the A6B23-type compound is indeed a "size-factor" compound and subsequently to determine the atomic-radius ratio range in which the A6Bz3-type compound can exist. In order to achieve these objectives, stoichiometric A6Bz3 alloys, where manganese (B) was alloyed with various lanthanide elements (A), were selected for investigation. The atomic-radius ratios of lanthanide elements with manganese range from 1.26 for Lu/~n to 1.46 for Eu/Mn. This radius ratio range includes and exceeds the range of all previously reported A6Bz3-type compounds—1.32 for Th/Mn' through 1.38 for Sr/Li. Furthermore, the atomic-size difference between successive elements of the lanthanide series in order of atomic number) is of the order of 0.01A (europium and ytterbium are exceptions). The series of lanthanon-manganese alloy systems is ideally suited to a precise determination of the limits of allowable atomic-radius ratio for A6Bz3-type compound formation. EXPERIMENTAL PROCEDURE The lanthanide metals, in ingot form, supplied by Michigan Chemical Corp. (St. Louis, Mich.) and Nuclear Corp. of America (Burbank, Calif.), were guaranteed by the suppliers to be at least 99.9 wt pct pure (traces of silicon, calcium, and other minor constituents present on occasion, not to be more than 0.05 wt pct) as shown by spectrographic analysis. Manganese metal, in polycrystalline form, was redistilled from the commercial, chemically pure grade and was analyzed to be at least 99.95 wt pct pure. In all cases, the atom ratio between the two elements in each charge was A (rare-earth meta1):B (manganese) = 6:23 and a constant weight, 3 g, of

Jan 1, 1965

By Hendon R. Johnston

In the Tennessee Valley Authority's program of investigation and treatment of foundations for major structures, many chert, or flint, bodies have been encountered during the diamond-drilling operations. These chert bodies occur most frequently in the Knox dolomite and

Jan 1, 1948

By Hendon R. Johnston

In the Tennessee Valley Authority's program of investigation and treatment of foundations for major structures, many chert, or flint, bodies have been encountered during the diamond-drilling operations. These chert bodies occur most frequently in the Knox dolomite and

Jan 1, 1948

By C. E. Jackson, E. C. Nelson, A. L. Christenson

Much information regarding the transfornlatio~lal characteristics of a steel as it cools in a known manner from the austenitic state can be obtained from dilatometric studies. This method has received more arid more attention because of its great flexibility, accuracy, and ease of interpretation. 'The method is entirely applicable to any rate of heating and cooling although the experumental procrdures for high rates of cooling have offered some difficulties. This paper presents a description of equipment employing cooling rates up to 500 °C. per secorld and the results of dilatometric observations on six commercial steels are included. French and Klopsch1 studied the cooling transformations of a serirs OF carbon steel, using the thermal arrest method. This was followed by the systematic investigatiol1 of Esser and co-workers on the effect of carhon2 and other alloying additions. in which the transforlnation temperature\ were determined by magnetic induction measurements indicated by a string galranoineter. Emphasis was placed on determining Ar' trailsformations and the critical cooling rates for these steels. The maglietic measurements wrere used in an effort to obtain more accurate data at higher cooling rates. Measurements of thermal arrest were made also to check the validity of the magnetic indications, and good correlation was found between the two, although Esser's,Ar' temperature measurements on iron-carbon alloys were about 200°F. lower than the measurements made by Fresnch and Klopsch. A notable contril~ution by Esser was the introduction gas quenching. wever and Rose4 used a moving-coil galranometcr in the study of the .Ar and Ar" of iron-carbon alloys by the thermal arrest method and obtained somewhat lover Ar" temperatures than those observed by Esser below I per cent carbon and considerably higher ahove. They concluded that the cooling rate had little influcncc on the Ar" temperatures above 0.4 per cent carbon, although Esser had observed a decrease in the -4r" temperature with increasing cooling rate with similar steels. Digges determined the .Ar" temperature4 for a scries of high-purity iron-carbon alloys, and close agreement with his results was obtained by Greninger. The thermal arrest method. together with metallographic observation used in both these studies, represents the latest investigations of this type. Any investigation by thermal analyses is dependent on the heat of reaction and the specific heat of the

Jan 1, 1945

C. E. Dewey, Georgetown, Colo. (communication to the Secretary) : In his remarks on crushing-machinery, Mr. Douglas says (Twins., xxii., p. 322): "To insure a smaller and more uniform size of particles in the crushed material, the Dodge crusher still communicates motion to the upper extremity of tile movable jaw, which oscillates on fixed pivots projecting from its lower extremity!' The notion that, in order to obtain a fine and uniform product from a rock-breaker, the movable jaw must be pivoted at its lower extremity, seems to obtain generally among mill-men, as well as among manufacturers of machinery. My experience with machines of both types does not confirm this belief. It is true that, to obtain a uniformly fine product from a jaw-crusher, the stroke at the lower extremity of the crushing-surface must be short; but that the movement at that end must be less than at the other or receiving-end is, I think, an erroneous assumption. Figs. 1 and 2 are intended to illustrate the two types of machine. It is found in practice that the capacity and the nature of the product of either machine, as usually constructed, are governed by the opening, C D, and the length of stroke of the movable jaw at D. This being the case, machines of either type, of the same width of crushing-surface, running at the same speed, and having the same adjustment as to opening and stroke at D, should give, when fed

Jan 1, 1895

By H. C. Fiedler

SILICON-IRON strip with a cube-on-edge secondary recrystallization texture is made commercially as thin as 10 mils. With inclusions present to inhibit normal grain growth, a few grains, and these have the (110)[001] orientation, grow very large at the expense of the matrix grains. In the absence of inclusions, only normal grain growth occurs and the texture is not as strong as when it is developed by secondary recrystallization.1 Strip for use at frequencies of 400 cps and higher is made in thicknesses of 1, 2, and 4 mils by a process developed by Littmann.2 Attempts to develop a strong texture in these thin gages by the same methods as were used for the 10 mil and thicker strip were unsuccessful,2 and Littmann's solution to this problem was to cold roll the grain

Jan 1, 1963

John Birkinbine, Philadelphia, Pa.: We have in the Institute two Dudleys—Dr. Charles B. Dudley, who has so thoroughly studied the chemical composition and physical behavior of rail-steel, and Dr. P. H. Dudley, whose investigations and

Jan 1, 1900

By Harmon E. Keyes

Harmon E. Keyes (Chemical & Metallurgical Engineer, Eagar, Ariz.)-Chemical dissolution of chalcocite by acidic ferric sulfate is well known. Resulting elemental sulfur may be oxidized to sulfuric acid by heated ferric sulfate. Laboratory tests at Southwest Experiment Station, USBM, Tucson, generally confirmed stoichiometric relations of 1 part Cu dissolved to 1.750 parts ferric iron reduced, using CP chemicals, dried ore samples, and apparatus cleaned with potable water. Recirculation with open-drainage percolation to increase copper in leaching solvent was followed successfully when appropriate, both in laboratory and Pinto Valley pilot tests. Before 1924 attempts to produce ferric sulfate by aerating ferrous sulfate solution were known. Initial oxidation was satisfactory, but rate slowed below practicality as oxidation progressed and acidity increased. Also, due to hydrolysis of ferric sulfate, a ferric precipitate of hydroxide and basic sulfate resulted. Both laboratory and pilot plant tests gave similar results, regardless of whether CP ferrous sulfate or scrap iron cementation discard solution was used. Rapid oxidation of ferrous hydroxide by air alone is well known to analytical chemists. I demonstrated a process to produce acidic ferric sulfate solutions by precipitating ferrous hydroxide with milk of lime, aerat-

Jan 1, 1973

By E. J. Nielsen, P. R. Strutt

A study has been made of the progressive changes in the distribution of etch-pit structures occurring during high-temperature creep in copper + 7 wt pct Al single crystals oriented with a [113] tensile axis. The two equally stressed glide systems with the highest Schmid factor would be expected to form subboundaries of the type predicted by Kear.2 The alignments of etch-pits on sections parallel to different (111} planes consistent with these types of boundaries were not observed. However, they were consistent with planar subboundaries (on a macroscopic scale). From an analysis of Amelinckx1 it may be shown that stable cross-grid dislocation boundaries may form in the primary slip planes. These boundaries form when dislocations with a Burgers vector not in the slip plane move into the plane by combination of climb and glide. THE geometry of subboundaries formed by the interaction of dislocations of two glide systems has been analyzed by Amelinckx,1 and the particular types produced by deforming fee crystals are predicted by ear.' In this paper types of boundaries which may be formed when climb as well as glide occur are discussed as this is relevant in high-temperature creep. It is assumed in the present investigation that the etch-pits observed in Cu + 7 wt pct A1 on surfaces parallel to {111} planes delineate the sites of dislocations. Although there is no direct evidence for this previous work on a-Cu/Al single crystals by Mitchell, Chevrier, Hockey, and Mon-aghan,3 would show this assumption to be reasonable. The alignments of etch-pits which form during creep are studied on sections parallel to each {111) plane. It is then deduced that these alignments are consistent with a specific type of planar subboundary. The Cu + 7 wt pct A1 single crystals had a [113] tensile axis and Fig. 1(a) shows schematically the relation of the slip planes and slip directions (as represented by tetrahedron ABCD) with reference to the tensile axis. The two equally stressed glide systems with the maximum Schmid factor namely ß-AD and (a-BD, from the analysis of Kear,2 would be expected to form the boundaries shown in Fig. l(a) and (b), also Fig. 5(a) and (b). EXPERIMENTAL PROCEDURE The a-Cu/Al single crystals were grown and annealed in a "gettered" argon atmosphere. Chemical analysis showed the aluminum content to be uniform in each crystal and the difference between crystals was maintained to an accuracy of ± 0.25 wt pct. The initial dislocation density and mean subgrain diameter after annealing was -106 cm-2 and 250 µ, respectively. Surfaces parallel to (111) planes were produced by specially developed electrolytic machining processes. The {111} faces were next electropolished for 5 min in a solution consisting of 25 g chromium trioxide, 113 ml glacial acetic acid and 40 ml water; the applied potential was 8 v. Dislocation etch-pits were revealed using l an etchant described by 1 ml bromine, 45 ml HCl, and - 250 ml water. RESULTS In crystals strained into secondary creep at higher stresses (443 and 750 g - mm-2 at 650° C aligned rows of etch-pits parallel to slip plane traces were evident in sections parallel to the (1111, (ill), and (111) planes, see Fig. 3. As well as the longitudinal alignments in Fig. 3, well formed randomly oriented arrays indicative of an equiaxed subgrain structure are evident. At the lower stresses (100 to 230 g . mm-2) only an equiaxed structure formed during creep. The sections in Fig. 3 are from a crystal crept for 70 hr at 650°C with a CRSS of 443 g.mm-2. Two identically oriented crystals were also deformed at the same temperature and stress for 5 min and 4 hr. In the crystal crept for 5 min, the etch-pits were randomly distributed with no tendency for directional alignment, see Fig. 2(a). As shown in Fig. 2(b) aligned arrays were evident after 4 hr creep but they were not nearly so well defined as in Fig. 3. The alignments (parallel to the arrows) in Fig. 3 are consistent with the existence of boundaries in the two main slip planes a and ß. The way in which this is deduced is seen by reference to Fig. l(c), where the existence of boundaries in the a and ß planes is verified by sectioning parallel to a,ß, and d. The (111) and ß(111) planes intersect the d(111) plane along BC [101 ] and AT [011] and alignments parallel to [101] and [011] are clearly evident in Fig. 3(c) in a section parallel to the d(111) plane. Similarly the a, and ß planes in Fig. l(a) intersect each other along DC [110] and hence there will be an alignment parallel to [110 ] in sections parallel to the a-plane and the ß-plane; this is evident in Fig. 3(a) and Fig. 3(b). It is interesting to note that alignments of etch-pits consistent with the boundaries predicted by Kear2 were not observed; see Figs. l(a) and l(b). The geometry of boundaries in {111} planes as shown in Fig. l(c) is discussed later. In Fig. 4(a) the individual etch-pits are resolved and the alignments are exactly parallel to the slip trace direction [101]. However, in some areas alignments deviate away from the slip trace direction by as much as 10 to 15 deg, this is evident in Fig. 4(b), and in Fig.

Jan 1, 1969

By George S. Rice

THE A.I.M.E. Ground Movement and Subsidence Committee, pro- posed in 1920, held its first technical meeting in February 1923, under the able chairmanship of Mr. H. G. Moulton. The following list of papers and discussions, indicating the scope of the problems and relation to various conditions and method of mining, were given at that meeting by the distinguished mining engineers: J. Parke Channing, on Subsidence at Miami, Arizona; Howard N. Eavenson, on Mining an Upper Bituminous Seam after a Lower Seam Has Been Extracted; J. J. Rutledge, on Subsidence in Two Oklahoma Coal Mines; Benjamin F. Tillson, on Caving Cracks at the Franklin Mine, New Jersey; Dr. F. W. McNair, on the Dome Theory; William Kelly, on disadvantageous effects in Mining and Back-filling Working Upward a Steep-Pitching Iron-ore Bed; Eli T. Conner, on the good results of Back-Filling by Hydraulic Means in Preventing Destructive Subsidence in the Anthracite District; Thomas H. Claggett, on the merit of Systematic Pillar Drawing in Preventing Cracks in an Upper Seam; Henry H. Otto, successful results in the anthracite district in Mining Lower Seams before Upper Seams; Douglas Bunting, on Leading Factors Incident to Successful Mining of an Overlying Seam; Edwin Ludlow, on there being "less damage to buildings when there was complete removal of coal with complete packing than when room and pillar is used without extracting the pillars"; Edward O'Toole on "bumps" in eastern Kentucky mines, which he thought were the result of geologic stresses: H. A. Buehler, on Upheaval of Surface in an Illinois Case in Advance of the Face; and R. Dawson Hall, on The Mechanics of Subsidence from Mining. The author of this paper discussed various kinds of problems of ground movement and subsidence in both metal mining and coal mining; the production of great landslides by workings near an outcrop, as at Turtle Mountain, Alberta, Canada; and general

Jan 1, 1939

This is a most interesting paper and some data in it are corroborated by work I did at Watertown Arsenal some time ago with iron powder. I would like to ask Dr. Wulff to say just a little more about the compressive and tensile stresses on the surface of compacts. JOHN WULFF (author's reply).-Our work has not yet been completed; although enough data have been obtained with cylindrical compacts of iron to permit some conclusions. Briefly, in a compact 3/4 in. high and 1/2 in. in diameter pressed at 48 tons per sq. in., the residual stresses on the surface measured by X-ray diffraction techniques are as follows: The radial stresses on top center and bottom of compacts are practically zero; the longitudinal residual stresses on the side walls are near the top quarter of the compact about seven tenths that of the yield point of mild steel in tension; at the center surface of the compact they are in compression and in magnitude about 0.3 that of mild steel in tension; near the bottom, they are practically zero. F. V. LENEL.?- I was particularly interested in the work that Messrs. Wulff and Seelig reported on the influence of lubrication on the density of parts. In connection with the work of the American Society for Testing Materials on determining the green density of a compact, we ran into considerable difficulty in getting reproducible results of green density determinations. It was much easier to get a reproducible green density when the lubricant was mixed with the powder than when the lubricant was applied to the die walls; particularly when the die was not perfect-i.e., if it was somewhat rough or out of round. In this case, it was almost impossible to get reproducible green densities when the die walls were lubricated, while it was not too difficult to get reproducible

Jan 1, 1946

Frank Firmstone, Easton, Pa. (communication to the Secretary*) : It may not be amiss to point out that the top-pressure in iron blast-furnaces is largely affected by variations in the temperature of the gas. I find in my note-books, cases in which the pressure was from 9.25 to 9.5 in. of water when the material in the furnace was low (after dinner-hour), which fell to from 8 to 8.5 in., when the furnace was again full, and the gas consequently cooled. The chief cause for this effect is, that, at the higher temperature, there is a decrease in the weight of the gas in the descending-leg of the siphon formed by the down-comer and the chimneys. It does not seem probable that there is any direct relation between top-pressure and quantity of flue-dirt. Top-pressure, at any given moment, measures the " head " necessary to discharge the gas then passing, against the resistances of pipes, valves, etc., in the gas-conduits between the top of the furnace and the mouths of the chimneys, and can be increased at will by closing, more or less, the valves, or dampers, at the stoves and the boilers. The question of relation between top-pressure and flue-dirt can be settled very easily by direct experiment, working alternately with gas-valves open, and partly closed, and noting the top-pressures and the respective quantities of fluedirt collected. The quantities of fine ore blown away, as shown by Mr. Grammer's tables, are astonishing to one who has had no actual experience with Mesabi ore and hard driving. Flue-dirt, in the sense in which he uses the term, was unknown at anthracite furnaces so long as the working was normal; when it did occur, it was always an incident of scaffolding and bad work, and was no doubt caused by an increase in the velocity

Jan 1, 1904

By R. W. Jordan, J. Winter, A. J. Goldman

Kirkendall diffusion of copper and nickel atoms across the bond interfaces, as well as oxygen diffusion in the core to the interfaces, are the mechanisms which control the variation in bond strength with annealing time at 1600°to 1800°F in the cupro-nickel clad copper Mint composite. The unequal mass transfer resulting from the high diffusion rate of copper in cupro-nickel compared with that of nickel in copper caused void formation in the core. Small voids also formed in the cladding after short annealing times. These may have been nucleated by nickel oxide particles which are formed by the dissociation of the cuprous oxide in the core and the movement of oxygen to the cupro-nickel interfaces. The bond strength drops to very low values for annealing time up to 3 hr when the void density is greatest. The increase in bond strength after 16 to 72 hr at 1600°F is a result of the decrease in the void density in the cupro-nickel cladding and the growth of grains across the interface. The void density decrease is attributable to grain boundary diffusion of vacancies to the surface. The abnormally large grains in the copper preclude a similar process from taking place in the core. THE solution to many engineering materials problems that cannot be satisfied by using a single metal or alloy is often attained by combining two or more metals in such a way that each component performs a different function, while the composite meets the overall requirements. The Coinage Act of 1965 authorized a changeover from the traditional 90 Ag-10 Cu dimes and quarters to a bimetallic laminate of 75 Cu-25 Ni clad on a copper core. Economic considerations as well as physical, chemical, and mechanical properties provided a basis for the selection of this composite as a substitute for the silver-bearing alloy. An extensive survey of alloys suitable for use as coinage was prepared by Battelle Memorial Institute for the U.S. Mint.1 It was found that the cupro-nickel/cop-per/cupro-nickel composite satisfied the required color, density, mechanical properties, corrosion resistance, electrical properties, and magnetic properties to make it completely acceptable to the general public and the vending machine industry. This investigation is part of a program to determine the feasibility of reclaiming composite scrap by thermally degrading the bond strength of the cupro-nickel clad copper laminate. The composite exhibits bond degradation and subsequent bond improvement during annealing in the temperature range 1600" to 1800°F. A study of the operative diffusion processes and the resultant structural changes was made in order to explain the observed variations in bond strength with annealing time. EXPERIMENTAL PROCEDURES AND RESULTS Bond Degradation. A measurement of the forces required to peel the cupro-nickel cladding from the

Jan 1, 1969

By Lawrence K. Jetter, Robert F. Mehl

Some advances have been made recently in the theory of the kinetics of precipitation from metallic solid solution despite the complexities of the problem, but there is surprisingly little quantitative information available on rates of precipitation with which to test present theory or upon which to build new theory. Attempts to measure rates of precipitation have been beset with difficulties which originate both in the anomalies that attend the changes in the properties selectcd for measurement, as, for example, in electrical conductivity or mechanical properties, and also in the complexities in the structural changes in some systems, as in the aluminum-copper system. If the functional relationship between the quantity of precipitate and the value of the selected property is uncertain, measurements of that property are obviously of uncertain utility in determining absolute rates of precipitation. If the precipitating system passes through one or more transition stages, the interpretation of measured rates lacks definiteness; in such cases, it is necessary to measure the rate of reaction in each separate stage, if the rate measurements are to have any significance from the kinetic point of view.* These difficulties cannot be wholly avoided, for at least in some measure they are characteristic of the process of precipitation from solid solution, but they can be minimized both by the selection of a simple system and by the use of a method of measurement relatively free from anomalous behavior. The present paper reports dilatome tric measurements on the rate of precipitation of silicon from the aluminum-rich solid solution in the aluminum-silicon system—a study that approaches the desiderata of simplicity. The aluminum-silicon system offers advantages from these points of view: there are no known anomalies in the property changes accompanying precipitation; there are no known transition stages; the precipitate is an element, not a compound, and both matrix and precipitate are cubic, and while the structures are not identical (the solid solution is face-centered cubic and the precipitate is diamond cubic), the system at least approaches the ideal case of a crystal precipitating from a matrix of the same crystal type—the ideal case which Becker6 assumed in treating the precipitation process theoretically. The dilatometric method, while not free from disturbing effects, as the subsequent dis-

Jan 1, 1943

By Lawrence K. Jetter, Robert F. Mehl

Some advances have been made recently in the theory of the kinetics of precipitation from metallic solid solution despite the complexities of the problem, but there is surprisingly little quantitative information available on rates of precipitation with which to test present theory or upon which to build new theory. Attempts to measure rates of precipitation have been beset with difficulties which originate both in the anomalies that attend the changes in the properties selectcd for measurement, as, for example, in electrical conductivity or mechanical properties, and also in the complexities in the structural changes in some systems, as in the aluminum-copper system. If the functional relationship between the quantity of precipitate and the value of the selected property is uncertain, measurements of that property are obviously of uncertain utility in determining absolute rates of precipitation. If the precipitating system passes through one or more transition stages, the interpretation of measured rates lacks definiteness; in such cases, it is necessary to measure the rate of reaction in each separate stage, if the rate measurements are to have any significance from the kinetic point of view.* These difficulties cannot be wholly avoided, for at least in some measure they are characteristic of the process of precipitation from solid solution, but they can be minimized both by the selection of a simple system and by the use of a method of measurement relatively free from anomalous behavior. The present paper reports dilatome tric measurements on the rate of precipitation of silicon from the aluminum-rich solid solution in the aluminum-silicon system—a study that approaches the desiderata of simplicity. The aluminum-silicon system offers advantages from these points of view: there are no known anomalies in the property changes accompanying precipitation; there are no known transition stages; the precipitate is an element, not a compound, and both matrix and precipitate are cubic, and while the structures are not identical (the solid solution is face-centered cubic and the precipitate is diamond cubic), the system at least approaches the ideal case of a crystal precipitating from a matrix of the same crystal type—the ideal case which Becker6 assumed in treating the precipitation process theoretically. The dilatometric method, while not free from disturbing effects, as the subsequent dis-

Jan 1, 1943

By A. R. Elsea, E. E. Fletcher

Cast X-40 alloy with the lowest nitrogen content studied had a 100-hr rupture stress at 1500°F about equal to the reported value for the commercial alloy. Increases in nitrogen content progressively decreased the rupture strength, and with about 0.1 to 0.2 pct N a minimum strength was reached, but there was no accompanying change in microstructure. Further increases in nitrogen resulted in the fomzation of progressively increasing amounts of a lamellar, pearlitic-type structure at the grain boundaries, with accompanying increases in rupture strength, and above about 0.25 to 0.33 pct N, the rupture strength exceeded the normally reported values. Two series of melts representing different melting stocks exhibited minimum rupture strengths at different nitrogen contents. This suggests that some unidentwed trace element not removed by vacuum melting has a strong influence on the response of this alloy to variations in nitrogen content. In a series of melts with manganese contents ranging from 0.6 to 3.2 pct, the material with the lowest manganese content had the highest 100-hr rupture strength at 1500°F. The manganese variations had no appreciable effect on the microstructure. CAST cobalt-base alloys such as X-40* exhibit high strengths at elevated temperatures (1500°F and above), but they also show considerable scatter in high-temperature properties. Since the design of parts for critical applications must be based on the minimum expected properties, this broad scatter appreciably lowers the design strength of the alloy. If the relatively poor properties exhibited by a few test parts from any given group could be improved, the spread in properties would be narrowed, and the design stress could more closely approach the average expected properties. The purpose of this research investigation was to learn what were the causes of these erratic properties and, if possible, to find methods for eliminating them. Earlier unpublished work showed that vacuum melting markedly influenced the high-temperature strength of cast X-40 alloy. There were indications that this behavior may have been the result of changes in the nitrogen or manganese content of the castings. Consequently, in the current investigation, the influence of variations in nitrogen and manganese content on the structure and high-temperature properties of cast X-40 alloy was studied. In this program, X-40 melting stock was vacuum melted to produce a base material that was very low in nitrogen content and in volatile trace elements. Additions were then made to this base material to produce alloys of the desired composition. The metal was cast into investment molds producing coupons which were machined into stress-rupture bars. These bars were subjected to stress-rupture tests and me-tallographic study to determine the influence of changes in analyses (nitrogen and manganese content) on the structure and properties. Material—The melting stock used for these experi-ments was in the form of shot from two master heats of commercial X-40 alloy. Only one master heat was used in a given series of melts. Thus, any differences in structure or properties that showed up in the specimens from a given series would be the result only of the intended variations in composition. The certified analyses of the master heats were as follows: C Mn Si Cr Ni Lot No. 2 0.50 0.71 0.66 25.44 10.53 Lot No. 3 0.54 0.73 0.70 25.95 10.00 W Fe Co P S Lot No. 2 7.45 1.34 Bal. 0.011 0.013 Lot No. 3 7.58 1.53 Bal. 0.005 0.016

Jan 1, 1960