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By E. R. Morgan

A series of manganese-rich ferromagnetic alloys has been studied. The alloys are based upon an interstitial solution of carbon in manganese. In each of the systems investigated, the ferromagnetic phase was found to be face-centered-cubic in structure. This magnetic phase is based upon the composition (Mn, X)4C; where X is a metallic element which has both a positive size factor with respect to manganese and a high positive valence. Typical elements of this type are aluminum, indium, and tin. Preliminary magnetic measurements indicate that the effective magnetic moment of manganese in the alloys is at least 1.0 Bohr magneton per atom. It is emphasized that the critical atomic separation beyond which ferromagnetism can occur will be governed by the electronic configuration of the manganese atoms. Lattice parameter measurements show that the ferromagnetic condition in the present alloys is associated with an increased atomic separation of only 3 to 6 pct compared with a hypothetical face-centered-cubic lattice of pure manganese. MANGANESE which is paramagnetic and not ferromagnetic in the pure state can become ferromagnetic if suitably alloyed. Under favorable conditions manganese can have an effective ferromagnetic moment of the order of 3.41,2 or even 4.0 compared with a moment of 2.2 Bohr magnetons for iron. The incidence of ferromagnetism is believed to be controlled by the degree of atomic separation.4,5 This is consistent with the fact that the atomic separation, when considered in terms of the ratio of the atomic diameter R to the diameter r of the 3d-shell, is larger in the ferromagnetic metals. The values of R/r calculated by Slater,' for metals of the iron group are given in Table I, and Slater has suggested that the critical ratio of R/r is 1.5. Consideration of the criterion of atomic separation alone would suggest that there are three classes of possible ferromagnetic manganese alloys: 1— Ordered structures, of either solution or compound types, such that manganese atoms are not near neighbors; 2—Structures in which the separation of near-neighbor manganese atoms is sufficiently increased by the presence of suitable solute atoms; and 3—Dilute solutions of manganese. Typical ferro- magnetic alloys of types 1 and 2 are the Heusler alloys and Mn4N, respectively. There are no recognized ferromagnetic alloys of type 3. In view of the proximity of the ratio R/r for manganese to the critical ratio of 1.5, the present work was concentrated on manganese-rich alloys rather than on ferromagnetic alloys of low manganese content, several examples of which are already known. Calculation of the distance of closest approach of manganese atoms in each of its allotropic forms, Table 11, indicates that the high temperature ? phase provides the most suitable basis for ferromagnetic alloys of high manganese content. However the high temperature forms of pure manganese cannot be retained on quenching, although a face-centered-tetragonal form apparently can be produced by electrodeposition. Since the critical separation which must be exceeded in order to obtain ferromagnetism is dependent upon the number of electrons in the d-shell, no exact critical value of R/r can be assumed. Not only will this separation vary from one pure metal to another, but it will also vary with the valency of the given type of atom when it is in an alloy. Raynor8 has shown that metals of the iron group probably

Jan 1, 1955

By C. A. Heiland

IN the third year of war, geophysical oil exploration broke all records to keep pace with the demand for increased reserves. Geophysical prospecting for strategic and other minerals also grew in scope. The trend of geophysical oil exploration throughout the war is indicated in Fig. 1. This figure resembles the one presented in the last annual review issue of M&M (February 1944, p. 62), corrected for data on-operations in the last months of 1943 and extended into 1944. The average number of geophysical oil prospecting crews in the field in 1944 was 451, whereas the total in 1943 was 340. An upward trend in the use of all geophysical methods is clearly evident throughout the year. Seismic operations were 67 per cent, gravimeter surveys 28 per cent, and other methods 5 per cent of the total. Seismic reflection and refraction crews increased 181/2 per cent over the 1943 average, gravimeter operations increased 73 per cent, and other methods gained 92 per cent. The increase in seismic and gravimeter operations, particularly the latter, is probably due to an increased production of equipment and the organization of new service companies. Miscellaneous methods gained largely through a revival of magnetometer work, and an increase in the use of torsion balances and electrical equipment. In comparison with the prewar average of 1941, it is noteworthy that seismic operations increased 58 per cent, gravimeter operations 88 per cent, and miscellaneous other methods gained as much as 283 per cent. Unfortunately the expansion in the number of geophysical crews does not indicate a proportionate increase in efficiency or in areal coverage, as will be brought out later.

Jan 1, 1945

By Frances H. Clark

IN wartime, the fabrication and use of metals assumes increased importance, for a modern war of sizable proportions cannot be undertaken with- out a vast supply of this material. Light alloys of aluminum and magnesium, which were comparatively unknown in the last war, will play an important role in this one. Due to research on a vast scale in the interim of years, industry is today well equipped to fabricate metals on an enormous scale. Research for the past year has been most productive and a comprehensive survey in the space of this article would be impossible. It is hoped that the stressing of a few items here and there out of a great quantity of able work will indicate in a small way the advances made within recent times. Specific references to the literature will be omitted at the Editor's re- quest but some authors of papers that I have found of special interest are mentioned.

Jan 1, 1940

By D. G. Westlake

Polycrystalline tensile specimens of various Zr-0-H alloys have been tested at 298°, 178°, and 77°K. Solute oxygen and hydride precipitates in quenched alloys made individual contributions to the yield strength at 0.2 pct strain which combined to produce a resultant strength increment, a,., Ductility changes which were ohserved can he interpreted in terms of the various oxygen and hydrogen concentrations, testing tem -peratures, and dispositions of the hydride. ADDITIONS of oxygen in solid solution were known to increase the yield and tensile strengths of polycrystalline zirconium as early as 1951.' More recently, the critical resolved shear stress (CRSS) for prism slip in zirconium single crystals was also shown to be affected by the solute oxygen impurity.' This latter work also demonstrated that large increments of strength could be contributed by the finely dispersed zirconium hydride precipitates that are present in quenched Zr-H alloys.3 It was concluded that the combined strengthening due to alloying could be expressed by where to is the increase in the CRSS due to solute oxygen alone and TH is the increase due to finely dispersed hydride precipitates. Eq. [I] is analogous to one used to express the combined strengthening effects of work hardening and neutron radiation damage.4 Eq. [1] was verified only indirectly and for only small amounts of the impurities—up to 0.14 at. pct 0 and 0.63 at. pct H. The present investigation was undertaken to obtain a more direct verification of the validity of the form of Eq. [1] for this system and also to determine the combined effects of oxygen and finely dispersed hydride precipitates on the tensile strength and ductility of polycrystalline zirconium. EXPERIMENTAL PROCEDURE Tensile specimens were machined from the same rolled billet of Kroll zirconium used in the earlier study.' These measured 38 by 4.7 by 0.5 mm and had 10-mm gage lengths which were 2.8 by 0.5 mm. Each specimen was ß-annealed in vacuo at 1173°K for 15.5 hr and a-annealed at 1073°K for 4 hr to D. G. WESTLAKE, Member AIME, is Associate Metal l ur-gist, Metallurgy Division, Argonne National Laboratory, Argonne, III. Manuscript submitted July 17, 1964. IMD______________ give an equiaxed structure with grain diameters averaging 0.06 mm. Oxygen was added by allowing the metal to react with a known quantity of oxygen during the 0 anneal and known quantities of hydrogen were added during the a anneal. Each alloy was encapsulated in Pyrex under vacuum, annealed at 873°K for 4 hr, quenched into ice water, and polished by immersion in a solution of 46.75 vol pct H2O, 46.75 vol pct concentrated HNO3, and 6.5 vol pct HF (49 pct) at 298°K. Special heat treatments given to a few specimens are described in the results below. Tensile tests were done on an Instron machine and were begun within 20 min after the quench, except where specified otherwise. Tests at 298°K were in air, at 178°K in acetone, and at 77°K in liquid nitrogen. All tests were at a strain rate of 8x sec-1. RESULTS AND DISCUSSION Yield Stress at 298°K. The compositions of alloys and the corresponding yield stresses (0.2 pct strain) are given in Table I. A plot of the yield stresses of the oxygen alloys, A, B, C, and D, indicates that varies linearly with CO1/2, where Co is the oxygen concentration, Fig. 1. This is in accord with Fleischer's6 theory for solution strengthening if the oxygen atoms do not cluster, or the cluster size remains constant with increasing oxygen concentration. In Fig. 1, it appears that if one could prepare some oxygen-free zirconium its yield stress would be very low. Therefore, we shall assume that for the oxygen alloys is equivalent to O0, the strength increment contributed by the presence of oxygen. The relationship between0.2and Co is expressed by 0.2 = 31.3 CO1/2, when the yield stress is in kg per sq mm and the concentration is in at. pct. Each of the hydrogen alloys, Al, A2, A3, and A4, contained 0.081 at. pct 0 as an impurity. In Fig. 1, it appears that this small amount of oxygen makes a significant contribution to the strength which cannot be ignored when we evaluate the contribution of the finely dispersed hydride. Let us assume the validity of the following equation: a0.2 = (a2o+a2R)1/2 [2] which is analogous to Eq. [I] for single crystals, and calculate values of UH for the hydrogen alloys by using the experimental values of 0.2 and o (0.081 at. pct) = 8.9 kg per sq mm. For 0.36 at. pct H, oH = 6.47; for 0.72 at. pct H, OH = 11.30; for 2.16 at. pct H, OH = 19.4; and for 3.60 at. pct H,

Jan 1, 1965

By E. W. Davis

THIS nation has been depending upon the Lake Superior iron ranges for most of its iron ore requirements for over half a century. Furthermore, it can continue to draw the major portion of its ore requirements from the same source for another century or more, but to accomplish this, great changes must take place in the present ore mining industry. Preliminary preparations for these changes are now underway and in the next few years decisions of far-reaching importance must be made. But to understand the situation, it is first necessary to know something of the nature and occurrence of the Lake Superior iron formation. So far as is known, the merchantable grades of iron ore remaining in the various Lake Superior ranges are as shown in Table 1, which shows that

Jan 1, 1947

Brushy Creek mine is located near the center of a linear, 40 mile long belt of mineralization that extends south from St. Joe Minerals Corp.'s Viburnum division. The mine area includes a segment of 5.4 miles long of this new mining region along which eight mines are presently operating. The geology of the area is relatively simple; the rock formations have not been disturbed through folding or extensive faulting.

Jan 7, 1973

By S. A. Falconer

Much attention and publicity has been given, during recent years, to grinding, classification, flotation, and thickening. The various technical papers, and symposiums held to discuss these important phases of milling, have contributed to a better under- standing of the fundamental principles and operating variables involved. Another important part of milling- to the flotation operator-is a treatment step to which frequently too little attention is given-" conditioning," or the treatment the ground mineral pulp receives before it enters the flotation machines. Conditioning" is a hackneyed and frequently misused term, commonly employed to describe the pretreatment of surfaces of minerals in ore pulps or mill pr6ducts prior to froth flotation. In general, such pretreatment is for the purpose of changing the flotation characteristics of these mineral surfaces to enable them to respond in some desired predetermined manner when subjected to flotation. Taggartl states that the function of conditioning is "either to insure selective collector coating of one mineral species while another species is not; or to take such steps as will compensate for departure there from."

Jan 1, 1949

By Pierre R. Hines

Diphenyl guanidine is used as an accelerator in vulcanizing rubber. Other rubber accelerators are also flotation collectors, e.g., dithiocarbamate, thiazole, and the xanthates. Urea and its derivatives are good flotation collectors,1 and guanidine is the nitrogen analog of urea. These two characteristics suggested testing diphenyl guanidine as a flotation collector. Diphenyl guanidine has been tried in flotation work previously, but references give no details.2-4

Jan 2, 1959

By C. B. Sclar and

A graphical solution is presented for the equation v =v &-cU where vb is the volume of liquid b of density 6 that must be added to liquid a of volume va and density d, in order to obtain a heavy-liquid solution of preferred density dm for mineral fractionation. The equation is valid only for pairs of liquids whose volumes are additive, but empirical density-composi-tion data show that this condition is met over wide compositional ranges by all of the heavy solutions that are commonly used for mineralogical analysis. The chart is a nomograph which consists of two horizontal volume scales ad a vertical density scale arranged so that one volume scale occurs on each side of the density scale. All the scales are linear. For two liquids of density d, and &, respectively, each volume scale has an independent level on the density scale, ad the graphical solution for vb on the nomograph is obtained by construction of one straight line. The chart can be prepared easily to cover any density range with any desired accuracy by proper selection of the scales. Heavy-liquid separation of particulate samples is an indispensable analytical procedure in the mineralogical and mineral-process ing laboratory. Heavy liquids may be used 1) to isolate specific minerals in the form of high purity products or to fractionate samples into several products with density limits for petrographic, chemical, spectrographic, and X-ray diffraction analysis,'-' 2) to determine the density of minerals,'-l4 3) to facilitate the recognition and identification of optically similar associated minerals,15 and 4) to determine quantitatively the degree of liberation of ore minerals in ores and mill products at various limiting sizes." The preparation and recovery of heavy liquids suitable for mineralogical analysis are discussed fully in the literature and operational procedures and special equipment for heavy-liquid separation are described in numerous references.'747837' 13,18,25-42 Useful tabulations of heavy liquids for mineralogical analysis are given by Tickell, Mil-ner,' Twenhofel and Tyler,' and Lange and a very complete up-to-date list of minerals arranged according to increasing density is given by Mursky and Thompson. USEFULNESS OF THE DENSITY CHART For any particulate sample, the limiting densities selected for its fractionation by means of heavy- liquid separation depend on the respective densities of the constituent minerals and the specific objectives of the separation. In many instances, the densities of readily available and practicable heavy liquids do not coincide with those that are required, and suitable liquids of the proper density are obtained by dilution with miscible liquids. In the general case, one may wish to mix either a pure liquid (A) or a solution of two miscible liquids (AP,,) of known density with either a pure liquid (B) or a different solution of the two miscible liquids (A,B,) of higher or lower density in order to obtain a final liquid of the preferred density. In conventional practice, the latter is reached empirically by trial-and-error addition of increments of one liquid to the other. The density of the final solution may be determined either by accurately weighing a known volume of the final liquid,'' 532;4;40, or by means of I)a Westphal balance, 2)a hydrometer, a refractometer in the case of binary liquid systems for which density-refractive index data are available,15 4) natural or synthetic .indicators of known density, a pycno-meter. Like all trial-and-error methods, these procedures are time consuming and many require special equipment which may not be available, The purpose of this paper is to show that the volume of a liquid of known density which is to be added to another liquid of known volume and density in order to obtain a solution with an intermediate preferred density may be determined rapidly and accurately by a graphical method provided that the two liquids form ideal or quasi-ideal solutions whose volumes are additive. Empirical data47'8~'8~4B'49 show that solutions prepared from pairs of miscible

Jan 1, 1961

By H. C. Fiedler

Heats of high purity iron containing 3.1 pct Si and be -tween 0.0003 and 0.0295 pct N were prepared by vacuum melting ad then pouring while in a nitrogen atmosphere with the pressure between 0 and 90 psi. Strip from a heat with 0.0184 pct N underwent complete secondary recrystallization during the final anneal. Heats with less nitrogen had too few Si3N4 particles to restrain normal grain growth, and the heat with higher nitrogen had too many particles to allow complete secondary recrystallization. In the hot-rolled structure, Si3N4 precipitates only at the grain boundaries, with the consequence that annealing after hot-rolling diminishes the ability to subsequently undergo secondary recrystallization. In contrast to this behavior, ALNprecipitates uniformly in the hot-rolled structure. Under 1 atm of nitrogen, Si3N, in 3.1 pct Si-Fe dissociates between 900" and 950°C; the solubility of nitrogen increases from 0.0010 pct at 900" to 0.0030 pct at 1200°C. The solubility of nitrogen in Si-Fe has been the subject of many investigations. Corney and Turkdogan1 heated a 2.83 pct Si alloy in nitrogen and found the solubility, under 1 atrn of nitrogen, to be 0.0019 pct at 900°C. They claimed that Si3N4 did not form in the alloy above 705°C in 1 atrn of nitrogen. Fryxell et al.2 heated samples of 3.25 pct Si-Fe containing 0.0025 pct N over a range of temperatures and then analyzed for total nitrogen by vacuum fusion and for nitrogen in solution by a modified Kjeldahl technique. At 900°C, they reported the solubility of nitrogen in equilibrium with Si3N4 to be 0.0011 pct. pearce9 found the solubility of nitrogen at 900°C under 0.95 atrn of nitrogen to be 0.0017 pct in a 3.06 pct Si alloy. He reported that Si3N4 does not form above 770°C in 1 atrn of nitrogen. Although internal friction measurements have given somewhat higher values for the solubility,4-6 if the solubility of nitrogen is as low as has been reported by most investigators, and if Si3N4 is stable up to at least 945°C at 1 atrn pressure of nitrogen as reported by Seybolt,7 a small amount of nitrogen in properly processed Si-Fe should be effective in promoting secondary recrystallization. The requirement is that in the final heat treatment there be enough small, well-dispersed particles of Si3N4 to restrain normal grain growth. Fast8 has obtained secondary recrystallization by nitriding high-purity 3 pct Si-Fe after hot-rolling to a thickness of 0.118 in., followed by processing to 0.012 in., and annealing. A large amount of nitrogen, 0.076 pct. was introduced during the nitriding heat treatment, but he has since reported9 that "a few hundredths of a percent" is sufficient. Small amounts of aluminum10 or vanadium" nitride are capable of promoting secondary recrystallization. Heats containing as little as 0.010 pct A1 or 0.042 pct V and from 0.006 to 0.009 pct N underwent complete secondary recrystallization at final gage, whereas heats with lesser amounts of aluminum or vanadium did not.l2 To be reported is the behavior of nitrogen in high-purity 3.1 pct Si-Fe, and the relation of this behavior to the ability to undergo secondary recrystallization. PROCEDURE Ingots weighing 1 lb were made by vacuum melting high-purity electrolytic iron (A104, Glidden Co.) and high-purity silicon (Monsanto Co.). The latter was used in preference to ferrosilicon to insure a low aluminum content. The design of the melting furnace permitted pouring with the furnace atmosphere either below or above atmospheric pressure. Accordingly, at the completion of melting, nitrogen was admitted to the desired pressure and the heat then immediately poured. The ingots were sound, with no indication of porosity. In Table I are listed the heats investigated, the nitrogen pressure at pour, and the nitrogen and oxygen contents as determined by vacuum fusion with a platinum bath at 1850°C, a procedure which insures measurement of the total nitrogen.13 In addition, all heats contained 3.1 pct Si and not more than 0.002 pct C, 0.003 pct S or 0.005 pct Al. It was subsequently found that the quantity of nitrogen contained in the heats in Table I does not necessarily represent that obtained under equilibrium conditions. For example, the ingot poured immediately after 1 atrn of nitrogen was admitted to the chamber contained 0.0093 pct N, whereas an ingot poured 3 min after the nitrogen was admitted contained 0.021 pct N and another poured after a 6-min delay contained 0.029 pct N. While some bleeding of the hot top occurred in the latter instance, the ingot when examined in cross section appeared sound. The ingots were heated to 1325°C in hydrogen and rapidly rolled to 0.080 in. in 3 passes. The roll speed of the final pass was reduced so as to increase the quenching effect of the rolls. The hot-rolled pieces were processed both as-hot-rolled and after heating for 3 min at 900°C in hydrogen. After cold-rolling to 0.026 in., the strips were heated for 2 min at 900°C in hydrogen, then cold-rolled to the final gage of 0.012 in. The loss of nitrogen in going from the ingot to cold-rolled strip was no more than 10 pct. The final heat treatment, which was for the purpose of develop-

Jan 1, 1970

By J. L. O’Brien, M. Suenaga, K. M. Ralls, V. F. Zackay

The effecls of aging a1 400°C on tile resistive transition at 4.2°K of a superconducling 70Zr-30Nb alloy are reporled. Microstrclural changes were studied by critical temperature, resistiue critical field, residual resistiuily, and microhardness measurements and by X-ray diffraction, optical microscoby, ad replication electron microscopy. The result of the aging treat- A defect-free Type 11 superconductor in a magnetic field above Hc1 cannot sustain a transport current runt is a fine array of w-phase pavticles with a mean center to center interparticle spacing of about 800A. At an aging time of 300 hr the maximum onset critical current density is rcached. The particle size at the maximum current density if about 4202. At times longer than 300 hr effective particle impingement leads to lower onset critical current densities. perpendicular to the applied field without power loss in the sample.'-3 This power loss is due to flux line motion caused by the Lorentz force and is manifested by a longitudinal voltage.4-6 When defects are present in the material, flux lines are pinned until the Lorentz force exceeds the "pinning force". That is, it is thought that flux lines reside in free-energy wells existing at the defects, and the critical Lorentz force is that which when integrated over distance will supply the free-energy difference necessary to move the flux

Jan 1, 1968

By C. Laird, C. E. Feltner

May different kinds of dislocation structures have been observed in strain-cycled metals and alloys. In order to understand their pattern and causes, an experimental program has been carried out to determine the influence on the dislocation structures of the three variables: 1) slip character of the material, 2) test temperature, and 3) strain amplitude. The results show that at high strain amplitudes cell structures me formed when the slip character is wavy, and that these are progressively replaced by uniform distributions of dislocations as the stacking fault energy is decreased. At lower strains, dislocation debris is formed which consists primarily of dipoles in wavy slip mode materials and multipoles in planar slip mode materials. Temperature merely acts to change the scale of the structure, smaller cells, and clumps of dislocation debris being associated with lower temperatures. It is shown that the results for many metals fit this pattern, which Parallels that occurring in unidirectional deformation. DISLOCATION structures produced by cyclic strain (fatigue) have been examined in a number of metals by transmission electron microscopy. These studies have produced a variety of interesting and often seemingly conflicting results. For example, different investigators have reported such structural features as cells.le4 bands of tangled dislocations,4'5 dense patches or clusters of prismatic dislocation loops, planar arrays,4'10 and various combinations or mixtures of these different structures. Most of these observations have been made on materials which were initially annealed and cyclically strained at low amplitudes resulting in long lives. Recently we have reported observations of the dislocation structures produced in copper and Cu-7.5 pct Al cycled at large amplitudes, resulting in lives of less than 104 cycles.4 These results, examined in combination with those in the literature, have suggested that a common or consistent structural pattern exists. Variations in this pattern appear to be determined chiefly by the three variables, namely, the slip character of the material,4,11 test temperature. and the strain amplitude. To verify this interpretation, we have studied [he influence of the above three variables (in different combinations) on the resultant structures in cyclically strained metals. Copper, fatigued at room temperature, was chosen as a reference state to which all other observations can be compared. The effect of slip character has been investigated by employing fcc metals of different stacking fault energy. Thus aluminum which has a more wavy slip character than copper, and Cu-2.5 pct A1 having a more planar slip char- acter, have been examined. The aluminum samples were fatigued at 210°K thus making their homologous temperature equal to that of copper at room temperature. The influence of temperature has been evaluated by examining the structures in copper at room temperature and 78°K. Finally the effect of strain amplitude was studied by looking at the structures at amplitudes giving lives ranging from 104 to 107 cycles. All of the specimens were examined at the 50 pct life level at which stage the structures have reached a stable configuration.12 I) EXPERIMENTAL PROCEDURE Strip specimens, 0.006 in. in thickness, were prepared from base elements of 99.99 pct purity or greater. Specimens were fatigued by cementing the strips to a lucite substrate which was subjected to reverse plane bending. This method of testing has been described e1sewhere.7 After fatiguing, specimens were thinned and examined in a Philips EM 200 which was equipped with a goniometer stage capable of ±30-deg tilt and 330-deg rotation of the specimen. On the basis of separate calibrations,13 allowances were made for the relative rotation and inversions between the bright-field images and the diffraction patterns. II) RESULTS AND DISCUSSION The life behavior of the materials under different test conditions is shown in Fig. 1 in the form of plots of total strain range vs cycles to failure. Comparisons of structures produced in the different materials were made at amplitudes which produced equal numbers of cycles to failure. The influence of strain amplitude on the structures produced in the reference state material (copper tested at room temperature) is shown in Fig. 2. At the 104 life level the structure produced comprises cells similar to those previously observed.3,4 They are approximately 0.5 p in diam and the cell walls are generally more regular or sharper than those produced by unidirectional deformation.14 At the 10' life level the

Jan 1, 1969

By K. E. J. Rapperport, C. S. Hartley

The only slip system observed in zirconium crystals deformed at 77", 575", and 1075OK was (1010) [1210] with a critical resolved shear stress in tension of 1.0 kg per sq mm at 77°K; 0.2 kg per sq mm at 575 °K; and 0.02 kg per sq mm at 1075 OK. The active twin planes were {1012}, (1121}, (11221, and (11233) with varying temperature dependence. A detailed analysis for the slip direction using Laue spot asterism is appended. NeARLY all metals of the hexagonal close-packed structure exhibit basal slip, i. e.,(0002)<1120>- type slip. This is true of magnesium,&apos; zinc,&apos; cadmium,3 beryllium,4 titanium,= yttrium,6 and rhenium.Many of these such as titanium 5&apos;8-&apos;0beryllium,4&apos;" magnesium, and zinc13&apos;14 display other slip modes even at room temperature, and nearly all have been reported to slip on other systems under particular loading or temperature conditions of testing. As is shown in this paper, basal slip was not found at any of four test temperatures from 77" to 1075°K in hexagonal close-packed zirconium under the simple loading conditions of tension and compression, even though in one case the resolved shear stress on the inactive (0002) <llgO> system was twenty-five times higher than the critical resolved shear stress on the active (1010) [1210] system. This result is consistent with prior studies on the active deformation processes in zirconium deformed at room temperature. &apos;&apos;-I7 SPECIMEN PREPARATION A) Material—The zirconium used in this work was of two types: 1) as-deposited reactor grade crystal-bar, and 2) arc-melted and forged reactor grade crystal-bar. Typical chemical and spectrographic analyses of these materials as received, and after hydrogen removal and crystal growth are given in Ref. 17. Crystals of type 1) above have the letter prefix (A) and those of type 2) have the prefix (B) throughout this paper. B) Crystal Growth— he zirconium was machined into rectangular parallelepipeds about 0.2-in. scl in cross section and 2 in. iong. These were hand polished through 4/0 abrasive paper, electropolished, given a hydrogen removal anneal, and subjected to long-time anneals at 840 °C in vacuo to produce usable crystals.&apos;7 A second technique used to obtain large crystals was to cycle the samples two or three times between 1200" and 840°C, allowing them to remain at the higher temperature for about 4 hr and at the lower temperature for 5 days.17 These techniques yielded some grains which occupied the entire cross section of the bar and were as long as 3/4 in. C) Orientation Determination—After the growth of large crystals by thermal cycling, the samples were repolished with extreme care through 4/0 abrasive paper and electropolished. Metallographic examination after polishing showed the surfaces to be free of visible deformation traces. Standard Laue back-reflection X-ray techniques were used to find the crystallographic orientations of selected large grains with respect to a specimen face and edge. Fig. 1 shows the stereographic projections of the stress axes for the crystals used. The sharpness of the spots on the Laue photographs indicated that the crystals were of good quality. EXPERIMENTAL METHODS Nine crystals were deformed in tension at 77"K, nine in tension and five in compression at 300°K in previous tests,17 fifteen in tension at 575"K, and eleven in tension at 1075°K. All specimens were stressed by load increments. After a predetermined load was applied, the specimen was removed from the loading appratus and metallographically examined for deformation traces. An attempt was made to initially stress each bar so that some crystals slipped a small amount and others not at all. This was done to bracket the critical resolved shear stress. One bar of special orientation (B-11) was repolished and annealed at 1075°K for 1 hr after lower temperature deformation, before final deformation at 1075°K. In the other bars the loading by increments, followed by metallographic examination, was continued until the surface distortion would interfere with analysis, or until fracture. One example of a crystal pulled to fracture is shown in Fig. 2. This photograph shows a crystal (B-14C) which was pulled at 1075°K and failed by slip on two (10i0) planes. The approximate orientation of this crystal is illustrated in the figure. Specimens were deformed at 77°K in liquid nitrogen on a tensile machine using an insulated bucket with an internal hook to accept a clamped specimen.

Jan 1, 1961

By C. C. Harris

The 3-parameter equation* was introduced1 as having the necessary form and flexibility for describing the major features of size distribution curves. Also, Eq. 1 was shown to contain most of the widely used 2-parameter equations as special cases. Special methods are necessary in order to determine the parameters of 3-parameter equations by graphical means. The procedure given previously required double graphical interpolation followed by regraphing the interpolated data. The theoretical basis of the method was a difference equation eliminating y. Several other methods for obtaining the parameters have been under development and one method appears to overcome the disadvantages of the earlier method and satisfies several procedural requirements. The points in favor of the new method as compared to the earlier method are as follows: 1. Estimation of the quality of fit is direct, and is in fact an essential part of the procedure. 2. The data is plotted directly without the necessity of interpolation from a graph. 3. The method makes use of Rosin-Rammler2 paper which because of expanded scaling in the coarse sizes leads to improved accuracy1 as compared with the log-log plot for the Gates3-Gaudin4-Schubann5 representation. 4. There is a gain over the earlier method in overall accuracy and in simplicity.

Jan 1, 1970

By Daniel Martin

THE dendritic pattern of steels shown by deep etching is used exten-sively as a guide in the inspection and control of the great majority of steels used in ordnance construction and for many applications in indus-try. The value of macroexamination lies in the fact that it enables a qualified observer to make deductions concerning the general quality of relatively large pieces of metal. Not the least of these general character-istics is the nature and extent of the dendritic segregation in the steel, either in the cast condition or after mechanical or thermal treatments. PREVIOUS WORK Detailed methods for macroetching were outlined by Yatsevitch1 and have been standardized by the American Society for Testing Materials. A comprehensive study of the occurrence, origin, and the chemical and crystalline nature of the dendritic structure was given by Keshian.2 The marked persistence of dendritic segregation in nickel steels is fully recognized and has been discussed by Sauveur and Reed&apos; and by others. Very little, however, has been written on the effect of the various elements on the macrostructure of steels, and the purpose of this report is to submit evidence concerning the influence of chromium, nickel and molybdenum on the macrostructure of some 4 by 4-in. ingots cast and treated under closely controlled conditions.

Jan 1, 1939

By C. G. Dunn, W. W. Martin

Various X ray diffraction techniques have been developed for determining orientations of crystals. Transmission and back-reflection Laue methods1,2,3 in particular have been found to be very useful. In many applications, however, a need still exists for a simplification of the details of analysis so that orientations can be determined more rapidly, and operators with little or no training in crystallography can be easily instructed in the necessary procedures. Filling this need in part is a system of analysis that has been in use for several years in the Metals Section of the Laboratory, General Electric Co., Pittsfield, Mass. This method is an extension of the one of Majima and Togino,4 which uses fifty-five indexed standard transmission Lauemams to cover the entire range of crystal orientations. Greater rapidity in determining the orientation of a crystal is achieved by using a slightly larger set of standard Lauegrams and by systematizing the steps followed. This system of analysis in its present form constitutes the subject matter of the present paper. Although the method uses transmission X ray Laue patterns, many of the operations are applicable to the analysis of back-reflection Lauegrams. Very briefly the method is based on the fact that Bragg and azimuthal angles for two or more identified Laue diffraction spots completely determine the orientation of a crystal, and standard Laue photographs of the Majima and Togino type provide a ready means for identifying Laue spots. After a preliminary analysis, which consists of identifying the pattern in terms of one of the standard patterns, a correctly marked Lauegram is selected to carry out the final analysis. From measured Bragg and azimuthal angles, the normals (poles) of the reflecting planes for the selected Laue spots are located on a stereographic projection and the orient.at.ion of the crystal determined (in terms of the positions of cube poles for example) by a few additional operations on a \I1ulff net. The actual procedure followed will be illustrated in detail after a brief treatment or X ray problems connected with orientation determinations and a discussion of useful principles and techniques. X Ray and Plotting Problems RELATIVE ADVANTAGES OF BACK-REFLECTION AND TRANSMISSION LAUE DIFFRACTION METHODS In the back-reflection Laue method it is easy to make a direct measurement of the tilt of a zone of Laue spots. Specimen thickness also is generally no problem. In the case of thin specimens, however, the time of exposure is less for the transmission Laue method. For example, with silicon ferrite this advantage holds up to a thickness of 0.6 mm if tungsten radiation at 40 kv peak voltage is used. Furthermore, the transmission photograph represents the entire thickness of the crystal whereas the back-reflection picture represents only a surface layer (a thickness of less than 0.05 mm for silicon ferrite), the deeper layers supplying a negligible amount to the diffraction pattern. If a crystal is distorted, the transmission Laue pattern gives more information particularly with regard to the orientation of the crystal and the overall amount of spread in orientation. Finally a 3 1/4 X 4 in. film suffices for transmission photograms; a 4 X 5 in. or 5 X 7 in. film with a central hole is needed for back-reflection patterns Not only is the manipulation of film easier because of the size of film, but

Jan 1, 1950

By M. F. Goudge, R. V. Tomkins

Sodium sulfate is an important chemical raw material that is being used in ever increasing quantities in modem industry. It comes on the market mainly in three forms: (1) Salt cake (Na2SO4), a relatively crude form of the anhydrous salt containing up to 3 pct impurities, and comprising about three-quarters of the North American production; (2) anhydrous sodium sulfate (Na2SO4), a refined form containing less than 0.3 pct impurities; (3) Glauber&apos;s salt, the decahydrate (Na2SO4.10H2O) containing 55.9 pct water of crystallization. Competing with salt cake from natural sources is byproduct salt cake from a number of industrial operations. For instance there is Mannheim cake resulting from the manufacture of hydrochloric acid by the reaction of salt (NaCl) and sulfuric acid in Mannheim furnaces; rayon cake, a high-quality product, resulting from the process of making rayon by the viscose process; chrome cake from the processing of sodium chromate to dichromate; phenol cake from the manufacture of phenol; also byproduct sodium sulfate resulting from the conversion of lithium sulfate to lithium carbonate; from the processing of sodium tetraborate to boric acid; from converting sodium formate to formic acid; and in the manufacture of cellophane. Sodium sulfate is also obtained as a byproduct in the manufacture of isosebasic acid. In addition strong competition has resulted from imports of byproduct salt cake from the chemical industries of a number of highly industrialized European countries. However in recent years due to technological changes the output of byproduct salt cake is rapidly diminishing and the natural deposits are becoming the most important source of sodium sulfate used in North America. For instance, the production of hydrochloric acid in Mannheim plants has become obsolete and thus the greatest single source of byproduct salt cake will disappear. Also viscose rayon is meeting strong competition from nylon and other synthetic fibers and production of byproduct salt cake from this source may do little more than remain at the present level. These factors together with increasing demand for sodium sulfate point to increased production from natural sources. In 1958, 36 pct of the total United States production was derived from natural sources and in addition 97,000 short tons was imported so that over 40 pct of the total consumption was supplied by natural sources whereas in 1953 the proportion was only 24 pct. The rapid growth in production is shown in Table 1. Principal Sodium Sulfate Minerals There are many minerals in which sodium sulfate is a constituent but those of commercial importance at the present time, and consisting wholly of sodium sulfate in either the hydrous or anhydrous states, are mirabilite and thenardite. Minerals of potential importance but consisting in part of compounds other than sodium sulfate are glauberite in which sodium sulfate is combined with calcium sulfate, and blödite in which sodium sulfate is combined with magnesium sulfate. Mirabilite (Na2SO4.10H2O) the decahydrate, consists of 24.8 pct SO3, 19.3 pct Na2O, and 55.9 pct H20. It is a colorless to opaque, soft, water-soluble mineral with a slightly bitter taste. It has a hardness of less than 2 and a specific gravity of 1.48. It forms long needle-

Jan 1, 1960

By V. R. Garfias, R. V. Whetzel

It is estimated that world consumption of petroleum, its products and related fuels during 1935 will reach an all-time peak of 1,592,000,000 bbl. —about 5.4 per cent higher than in 1934. Demand increased within the United States approximately 6.1 per cent during 1935 and in foreign countries about 4.1 per cent. The figures in Table 1 indicate that during the past five years world&apos;s production of crude petroleum and related fuels exceeded demand every year and that the aggregate difference is approximately 239,000,000 bbl. The supply in the United States exceeded consumption by some 134,000,000 bbl. over the same five-year period, while outside the United States the excess over demand is shown to be 105,000,000 bbl. Table 2 combines the excess production in the United States with its favorable balance of exports over imports, showing that the United States has reduced its storage over the five years by about 132,720,000 bbl., and indicates that, including its excess of imports from the United States, the rest of the world may have an unfavorable balance of some 371,000,000 bbl. over the five-year period. Such difference in foreign countries is largely due to increase in stocks, and partly at least remains in our imperfect knowledge of consumption statistics as an unfavorable balance. Table 3

Jan 1, 1936

By V. R. Garfias, R. V. Whetzel

It is estimated that world consumption of petroleum, its products and related fuels during 1935 will reach an all-time peak of 1,592,000,000 bbl. —about 5.4 per cent higher than in 1934. Demand increased within the United States approximately 6.1 per cent during 1935 and in foreign countries about 4.1 per cent. The figures in Table 1 indicate that during the past five years world&apos;s production of crude petroleum and related fuels exceeded demand every year and that the aggregate difference is approximately 239,000,000 bbl. The supply in the United States exceeded consumption by some 134,000,000 bbl. over the same five-year period, while outside the United States the excess over demand is shown to be 105,000,000 bbl. Table 2 combines the excess production in the United States with its favorable balance of exports over imports, showing that the United States has reduced its storage over the five years by about 132,720,000 bbl., and indicates that, including its excess of imports from the United States, the rest of the world may have an unfavorable balance of some 371,000,000 bbl. over the five-year period. Such difference in foreign countries is largely due to increase in stocks, and partly at least remains in our imperfect knowledge of consumption statistics as an unfavorable balance. Table 3

Jan 1, 1936

The Colorado School of Mines, Golden, Colo. M F Coolbaugh, President. Since 1906 the School of Mines has issued a journal, known as the Quarterly of the Colorado School of Mines, which carries many articles on matters of general interest as well as other articles of a technical nature There is no regular subscription price to the School of Mines publications Anyone interested in back numbers should write and find out the conditions under which individual copies may be obtained, whether a price is set on them or whether they are free Some back numbers are not now available but efforts will be made to supply copies from the files of alumni or other friends of the School Vol 23, No. 3 of the Quarterly (July, 1928) is an index of the publications complete from July, 1906 to July, 1928. A selected list of the technical articles appearing in the Quarterly is given here: Vol 3, No. 3, Rare metals. uranium and vanadium, by H. Fleck (1909), vol 3, No 4, Tungsten in Colorado, by H R Van Wagenen, vol 4, No 3, Preliminary report of the radioactivity of the carnotite of southwest Colorado, by H Fleck and W. G Haldane (1909), vol. 8, No 1 (1913), Some recent developments at Leadville, by G. M Butler, vol 8, No. 3, Physiography of

Jan 1, 1933