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By N. Tiner

THE mechanical properties of magnesium-alloy castings are greatly improved by grain refinement, and at present considerable attention is being paid to methods of obtaining fine-grained castings. One method of achieving this end is the use of proper melting and superheating techniques. These have been employed commercially to a great extent, but no comprehensive study of the subject appears to have been published at present. Numerous investigations found in the literature include some reference to superheating techniques, 1-4 and Achenbach, Nipper and Piwowarsky,5 based principally on thermal analysis, ascribe the grain-refining action of superheating to the influence of solid foreign particles or dissolved gases present in the melt upon the course of crystallization. The primary purpose of this paper is to present the principal facts concerning the effect of superheating on grain size of magnesium alloys. Attempts are also made to explain the experimental results in terms of a general hypothesis. The investigations are limited chiefly to common commercial casting alloys. In order to carry on this work, it was necessary to determine the factors influencing grain size and to develop a proper technique for the preparation of samples. The preliminary tests made by the author indicated that the grain size of magnesium alloys resulting from the solidification of a melt is determined by alloy composition, presence of impurities, rate of cooling during solidification, thermal history of the melt and to some extent the structure of the charge used. The rate of cooling is in turn dependent upon the mass of the melt, pouring temperature, and dimensions, properties and temperature of the mold into which the melt is poured. The final grain size of the alloys is still further modified by heat-treatment subsequent to casting. It is not within the scope of the present paper to discuss all of these factors, and it would suffice to note here that when equal amounts of magnesium alloys are prepared from the same alloying materials, melted in graphite crucibles under the same thermal conditions, then cast into graphite molds at a constant temperature, the .resultant solids have the same grain size. By maintaining all other factors constant, it is thus possible to vary thermal conditions of a melt and to examine the grain size of resultant castings. PREPARATION OF SAMPLES AND GRAIN-SIZE TESTING The alloys investigated in this paper were taken from ingots made by Permanente Metals Corporation or prepared by the author with pure carbothermic magnesium and necessary alloying elements. Melting was carried out under a flux in a graphite crucible heated uniformly by an

Jan 1, 1945

By J. L. Gillson

In a brief summary of the many occurrences of fluorspar in our western states, it is not possible to go into detail in regard to the geology, mining and milling methods, and reserves about individual deposits. Rather a broad review is made of the occurrences and an analysis of how the western deposits may fit into our future domestic economy is presented. General Statement on Fluorspar Situation Fluorspar has been used for years as a flux in the manufacture of basic open-hearth steel, in foundry cupolas for melting pig iron, in the manufacture of opalescent glass and in the preparation of hydrofluoric acid. In 1880 the annual production of fluorspar in the United States was around 4000 tons per year. By 1900 it was up to 21,656 tons and between 1902 and 1908 it averaged about 40,000 tons annually. Prices were then so low, by present standards, that it seems impossible to believe now that mining could have been performed profitably at the price levels then prevailing. In 1890 fluorspar sold at the mines for $6.70 per ton, in 1901 for $5.81, in 1916 for 85.92. When the United States entered World War I, flyorspar production and price skyrocketed; the production reached 263,817 tons in 1918, with prices above $20.00 per ton, and prices were even higher in 1919 and 1920. After 1920, the domestic production fell from the 1918 level to about 125,000 tons annually and the average price dropped back to about $18.00 per ton. By 1935 the average price had fallen to $15.00, but in 1940 with a rising demand the average price of all grades had gone back up to $20.31. Today it is 75 per cent higher than in 1940 and presumably the price of acid grade at .least would be even higher if it were not for price ceilings. The first subsequent year that the domestic production exceeded that of 1918 was 1941, and the 1944 production is expected to exceed 400,000 tons, or over one and a half times that of 1918. In five-year periods, average production and imports were as are shown in Table I. Many people concerned with the consumption of fluorspar believe that the postwar period ahead will show a repetition of price trends of the last such period. They believe that imports will be again an important factor in the available supply and the price will fall back gradually toward the prewar level. The following basic factors are pertinent in analyzing this conclusion:

Jan 1, 1948

By J. L. Gillson

In a brief summary of the many occurrences of fluorspar in our western states, it is not possible to go into detail in regard to the geology, mining and milling methods, and reserves about individual deposits. Rather a broad review is made of the occurrences and an analysis of how the western deposits may fit into our future domestic economy is presented. General Statement on Fluorspar Situation Fluorspar has been used for years as a flux in the manufacture of basic open-hearth steel, in foundry cupolas for melting pig iron, in the manufacture of opalescent glass and in the preparation of hydrofluoric acid. In 1880 the annual production of fluorspar in the United States was around 4000 tons per year. By 1900 it was up to 21,656 tons and between 1902 and 1908 it averaged about 40,000 tons annually. Prices were then so low, by present standards, that it seems impossible to believe now that mining could have been performed profitably at the price levels then prevailing. In 1890 fluorspar sold at the mines for $6.70 per ton, in 1901 for $5.81, in 1916 for 85.92. When the United States entered World War I, flyorspar production and price skyrocketed; the production reached 263,817 tons in 1918, with prices above $20.00 per ton, and prices were even higher in 1919 and 1920. After 1920, the domestic production fell from the 1918 level to about 125,000 tons annually and the average price dropped back to about $18.00 per ton. By 1935 the average price had fallen to $15.00, but in 1940 with a rising demand the average price of all grades had gone back up to $20.31. Today it is 75 per cent higher than in 1940 and presumably the price of acid grade at .least would be even higher if it were not for price ceilings. The first subsequent year that the domestic production exceeded that of 1918 was 1941, and the 1944 production is expected to exceed 400,000 tons, or over one and a half times that of 1918. In five-year periods, average production and imports were as are shown in Table I. Many people concerned with the consumption of fluorspar believe that the postwar period ahead will show a repetition of price trends of the last such period. They believe that imports will be again an important factor in the available supply and the price will fall back gradually toward the prewar level. The following basic factors are pertinent in analyzing this conclusion:

Jan 1, 1948

By L. D. Jaffe, J. H. Hollomon

The effect of tempering temperature and time upon the properties of quenched steel is clearly a subject of great practical importance, as well as of considerable theoretical interest. It would be very desirable to be able to predict the properties of a quenched steel when given any selected tempering cycle, with a minimum of experimental work upon that heat or even type of steel. Two problems are involved: one consists of relating the structure obtained to the physical properties, and will not be discussed here; the other, with which this paper deals, involves the relations of time, temperature and composition with the structure obtained 011 tempering. Indentation hardness is perhaps the most convenient quantitative measure of the tempered structure, or of what might be called the "degree of tempering." Undoubtedly, it is not an exact measure, and in some cases (as when temper-brittleness occurs) pieces of the same quenched and tempered steel may have widely differing properties at the same hardness. However, hardness has the advantage of being simple to determine and is certainly the most widely used indication of the degree of tempering. Moreover, for fully quenched steels that are not temper-brittle and do not contain retained austenite when quenched, it appears that, in general, if the hardness of the steel is the same, the tensile and impact properties will also be identical, whether a high or a low tempering temperature is used. The tempering charts available in the metallurgical literature usually give the hardness as a function of tempering temperature for only one tempering time. However, in practice, tempering times frequently vary, and a method of converting tempering curves for one time to tempering curves for some other time would be very valuable. It is also advantageous, in determining the tempering treatment necessary for a given part, not to have to temper samples at several temperatures for the time used for the commercial tempering operation. A more satisfactory procedure would be to employ times of the order of 10 to 30 min., rather than 5 or 10 hr., and if possible to use only one temperature. Furthermore, it is frequently desirable, for reasons such as temper-brittleness,* to obtain a given hardness with short times at relatively high temperatures, and it would be convenient to be able to compute without tests the time required to produce this hardness. Remarkably few quantitative studies of the hardness of quenched steel tempered over wide ranges of temperature and time

Jan 1, 1945

By William J. Craig, Harold L. Walker

INDUSTRY has for many years recognized the dependence of certain mechanical and physical properties, as well as workability, upon grain size variations in brass. Although the dependence of properties upon grain size has been recognized there are not many instances where a planned program of testing has been conducted and where the only intentional variable has been grain size. In particular the literature is limited with respect to the effect of grain- size on the endurance limit, though there are many industrial applications where the brasses are subjected to cycles of repetitive stresses. LITERATURE A number of the physical and mechanical properties of a given brass sheet, in the annealed condition, will depend upon: (I) The ready-to-finish grain size before final rolling, (2) the percentage deformation by cold working, and (3) the time and temperature of annealing, The first and second variables affect the recrystallized grain size, and the third variable affects the coalesced grain size. Gibbs1 has shown the effect of two different ready-to-finish grain sizes upon the tensile strength and hardness of deep drawing brass strip after a definite amount of cold rolling. The smaller the ready-to-finish grain size, the higher the tensile strength and hardness, but with lowered ductility, Gibbs also demonstrated, for a given time and temperature of anneal, that the tensile strength, hardness, and elastic limit are higher for the smaller ready-to-finish grain size, but the elongation is lowered, Townsend and Greenall2 have reported data which show that cold working increases the tensile strength, hardness, and load carrying ability of deep drawing brass sheet under reversed stress. Greenall and Gohn3 have reported data which show that the smaller grain sizes have higher tensile strength and hardness properties, and the data also show that increased cold working increases the tensile strength and hardness properties of deep drawing brass sheet. Kommers4 has reported data for tests of brass of known ready-to-finish grain size, a specific amount of cold reduction, and annealed at different temperatures above and below the recrystallization temperature. Kommers' results indicate that annealing below the recrystallization temperature does not change the tensile strength and hardness properties, but the endurance limit may be increased from 22,000 to 28,000 psi. The increased endurance limit is explained as resulting from the reduction of internal stresses by a stress-relief anneal. Burghoff5 and associates have reported data on creep tests, over

Jan 1, 1948

By E. I. Larsen, E. F. Swazy, F. R. Hensel

EXPERIENCE has indicated that hard bronzes are not suitable for bearing applications where high bearing loads and speeds are involved. It is the general practice to utilize softer materials for these purposes, such as copper, lead, silver, babbitt, lead-base alloys, and more recently aluminum-base alloys, preferably supported by a steel backing. It was the objective of the present investigation to study a new material produced by powder metallurgical methods susceptible to precipitation-hardening. TEST MATERIALS Preliminary tests were made with compacts containing copper, nickel and silicon in quantities sufficient to form 3 to 5 per cent nickel silicide. It was found that this type of alloy was susceptible to the formation of a soft surface shell when sintered in tank hydrogen. The depth of the shell depended on the length of sintering time and sintering temperature, and varied in thickness from a few thousandths to as much as one eighth inch. This soft shell resulted from the preferential oxidation of silicon, thereby reducing the efficiency of age-hardening by the nickel silicide compound. The body of the sintered compacts below the soft shell could be precipitation-hardened to a hardness of 70 to 85 Rockwell B, by quenching from. 900°C. and age-hardening at 450°C. A series of tests was made with various addition agents, in order to decrease the rate of preferential oxidation, and it was found that phosphorus was most beneficial in this respect. After considerable experimentation, the following nominal composition was accepted as standard: 2.4 per cent nickel; 0.8 silicon; 0.3 phosphorus; balance copper. The physical properties and certain bearing properties of this alloy are described in the present paper. PREPARATION OF COMPACTS Several methods of incorporating the hardening ingredient (nickel silicide) were studied. Compacts formed from copper, nickel and silicon powders were found to be inferior to those fabricated from prealloyed nickel silicide master alloys, because of the rapid oxidation of pure silicon during sintering. The use of a prealloyed nickel silicide hardener containing 25 per cent silicon and 75 per cent nickel could be further improved by preparing a master alloy, incorporating nickel, silicon, phosphorus and copper, having the following nominal composition: 25 per cent nickel; 7 silicon; 3 phosphorus; 64 copper. This alloy is brittle in. the cast condition and can be readily powdered. SINTERING PROCEDURE The blended powders were pressed at 25 to 40 tons per sq. in., the pressure depending on the size and shape of the compacts. Sintering was carried out in hydrogen or cracked ammonia atmospheres at

Jan 1, 1946

By Herbert H. Kellogg, Hugo Vasquez- Rosas

Recently the long-chain primary amines have been used extensively for the flotation of silicate minerals. The use of amines to float sulphide minerals has been investigated by several authorsl-5-l8 but most of this work has been done with the short-chain (less than six carbon atoms) primary amine compounds or the more expensive secondary, tertiary and quaternary amines. Perhaps the fact that the long-chain amines are good collectors for the common gangue minerals has led investigators to omit them from consideration as collectors for the selective flotation of metallic sulphides. The work reported in this paper was designed to investigate the use of a typical long-chain amine salt, laurylamine hydro-chloride, as a collector for the flotation of galena-sphalerite ores. The results show that laurylamine hydrochloride (LAmHCl), when used in small amounts, is a good collector for the selective flotation of sphalerite and galena from the common gangue minerals. The differential flotation of sphalerite from galena was not accomplished but the amine flotation of sphalerite after the standard xanthate flotation of galena is possible. The experimental work reported herein is not complete enough to be able to say whether amine flotation of lead-zinc ores would prove superior to xanthate flotation, or whether the method is even applicable to a more complex ore than the one used for this work. However, the apparent reagent costs for the flotation operations described in this paper seem to be less than for xanthate flotation. This fact alone should be sufficient to encourage the millman to investigate the use of these amine reagents, especially as these reagents are available on a commercial scale at a reasonable price. This paper has as its secondary purposes to illustrate how contact-angle measurements have aided in this investigation, and to bring forward some evidence concerning the mechanism of the collecting action of primary amines. Contact-angle Tests The contact-angle measurements were made by the method described by del Giudice6 and used in recent work by Taggart and his collaborators.7-9 The mineral specimens for the contact-angle tests were carefully chosen, to avoid cracks and inclusions of other minerals. All specimens were mounted in "transoptic" plastic mounts and the surfaces were cleaned by polishing with levigated alumina on a cloth-coverkd glass polishing wheel. Distilled water was used on the lap during the polishing and at all subsequent steps in the contact-angle tests. The mounted mineral specimens were handled with glass forceps and special care was exercised to prevent exposure of the clean surface to air or any other source of contamination.

Jan 1, 1947

By Herbert H. Kellogg, Hugo Vasquez- Rosas

Recently the long-chain primary amines have been used extensively for the flotation of silicate minerals. The use of amines to float sulphide minerals has been investigated by several authorsl-5-l8 but most of this work has been done with the short-chain (less than six carbon atoms) primary amine compounds or the more expensive secondary, tertiary and quaternary amines. Perhaps the fact that the long-chain amines are good collectors for the common gangue minerals has led investigators to omit them from consideration as collectors for the selective flotation of metallic sulphides. The work reported in this paper was designed to investigate the use of a typical long-chain amine salt, laurylamine hydro-chloride, as a collector for the flotation of galena-sphalerite ores. The results show that laurylamine hydrochloride (LAmHCl), when used in small amounts, is a good collector for the selective flotation of sphalerite and galena from the common gangue minerals. The differential flotation of sphalerite from galena was not accomplished but the amine flotation of sphalerite after the standard xanthate flotation of galena is possible. The experimental work reported herein is not complete enough to be able to say whether amine flotation of lead-zinc ores would prove superior to xanthate flotation, or whether the method is even applicable to a more complex ore than the one used for this work. However, the apparent reagent costs for the flotation operations described in this paper seem to be less than for xanthate flotation. This fact alone should be sufficient to encourage the millman to investigate the use of these amine reagents, especially as these reagents are available on a commercial scale at a reasonable price. This paper has as its secondary purposes to illustrate how contact-angle measurements have aided in this investigation, and to bring forward some evidence concerning the mechanism of the collecting action of primary amines. Contact-angle Tests The contact-angle measurements were made by the method described by del Giudice6 and used in recent work by Taggart and his collaborators.7-9 The mineral specimens for the contact-angle tests were carefully chosen, to avoid cracks and inclusions of other minerals. All specimens were mounted in "transoptic" plastic mounts and the surfaces were cleaned by polishing with levigated alumina on a cloth-coverkd glass polishing wheel. Distilled water was used on the lap during the polishing and at all subsequent steps in the contact-angle tests. The mounted mineral specimens were handled with glass forceps and special care was exercised to prevent exposure of the clean surface to air or any other source of contamination.

Jan 1, 1947

By Walter H. Munk

Generation of Waves by storms, and the transformation of waves in shallow water by local bottom topography are briefly reviewed. A detailed description of water motion in waves explains the nature and distribution of wave forces. A numerical example dealing with forces and moments against vertical piles summarizes the principles involved. Introduction The oil industry is moving into the open waters of the Gulf of Mexico. The design and construction of offshore drilling rigs present a number of difficult problems, among them problems involving the action of waves on fixed and floating structures. This paper deals with our present knowledge of ocean waves as it pertains to these problems, and the principles involved in computing wave forces against fixed structures. It is hoped that the more difficult case pertaining to floating structures can be discussed at a later time. None of the engincering aspects of the problem are entered upon in this paper, yet an understanding of the principles presented here should be helpful in the solution of practical problems. Waves are capable of exerting almost unbelievable forces. During a gale, waves at the harbor entrance of Amsterdam Canal in Holland lifted a 20-ton concrete block, which was resting on the bottom in 12ft of water, and deposited it on top of a pier which was 5 ft above the high water mark. At Wick Breakwater in Scotland, a mass of large stones in cement and bound together with iron rods, weighing 1350 tons, was broken loose and moved bodily! But one need not go to Holland or Scotland to find evidence of damage that waves are capable of inflicting (Fig I and 2). What is the mechanism by which waves are capable of exerting such enormous forces? To answer this, we must consider briefly the nature of wave motion. When a wind blows over a wheat field, waves appear to travel across the field, whereas the wheat itself remains rooted, slowly swinging back and forth. Similarly, in the case of water waves, the waveform travels swiftly over the water surface, whereas the water particles oscillate back and forth, but scarcely advance. The speed of the wave form is called wave velocity, the speed of the water particles is called orbital velocity. This fundamental difference between wave velocity and orbital velocity was already recognized by Leonardo da Vinci. Orbital velocity is generally much slower than wave velocity except for a breaking wave, a case which is of particular importance in the application to engineering problems. Forces exerted by the waves on obstacles

Jan 1, 1949

By R. S. Wagner, C. E. Miller, H. Brown

A dc field was applied to liquid BI-Sx or Au-Ge alloys of eutectic composition. The liquid alloys were kept at a temperature slightly above the eutectic. The concentration changes due to electrodijfusion are large enough to cause nuclcation and growth of the primary phases at the respective electrodes. Nearly complete separation of Bi-Sn eutectic was obtained as well as substantial separation of Au-Ge eutectic. The effect of an electric field on the solute distrihn-tion was itluestignted itt tlirectiortally solidified rods of a dilute Bi-Sn (0.5 al. pc,t Bi) alloy. Field-freezing was carried out in small-diameter cupillay tubes to avoid cotuectice mixing -of the liquid. The relative sollcte corzcentratioi, Cs/Co , was rneusred by n radioac1il.e tracer netlod. Cs/Co can be made both largev than unity or srialler than the equilibiuwz distvibrrlion c.oejyicienl, k, , oiler a substattiul portion of the soliclifi&apos;erl rocls. A direct current, passed through a liquid-metal solution, can cause substantial concentration changes by electrodiffusion. The magnitude of the change depends on the difference in ionic mobilities of the atomic species in solution. Electrodiffusion has been studied in many binary and ternary liquid alloys.&apos;y2 It was found that the rate of material transport decreases with time for a constant applied field, as a concentration gradient is established in the solution. A steady-state concentration profile is achieved when electro-diffusion is compensated by chemical diffusion. This may seem to limit the use of electrodif fusion for metallurgical application. However, a way of utilizing the effect of electrodiffusion is to combine it with crystallization or controlled freezing. rakin was first to propose this as a new method of separating metal alloys of eutectic composition at temperatures slightly above the eutectic temperature. It was possible by this method to separate Bi-Sn and Bi-Cd eutectics into their component phases. Angus et al discussed the possibility that the effective distribution coefficient, keff, could be varied by proper application of an electric field during solidification. The combination of electrodiffusion and solidification, called field-freezing, was discussed in detail by Pfann and aner. It was shown that field-freezing can be used as a crystal-growth process, an efficient method for eutectic separation, and a new means of changing the effective distribution coefficient. k,ff, beyond the usual range of ko < k,ff < 1. The liquid layer adjacent to the solid-liquid interface can be either increased or depleted in solute due to

Jan 1, 1967

By Gerhard Derge

Metallurgists have used borax as a fluxing agent traditionally, but until recently elemental boron has played an insignificant role as an alloying element. Neither the metal nor its compounds have been regarded as important metallurgical materials and there is a surprising lack of knowledge concerning their metallurgical behavior. The new applications to steel-making of both boron and borates, which arose in part from wartime incentives and restrictions, have been seriously handicapped by this lack of data. For example, rasorite, a naturally occurring sodium borate, has been shown to be an effective substitute for aluminum as a ladle deoxi-dizer in rimming steels.&apos; Likewise, the effectiveness of boron as an alloying agent has been demonstrated,2,3 giving deep hardening when used in restricted amounts. The exploitation of both of these uses has been retarded by the difficulty of attaining suitable metallurgical control. Recognizing that the most important information required was a knowledge of the equilibrium between boron and oxygen dissolved in liquid iron. Gurry4 calculated this relation from the best thermal data available. However, estimates of the entropy of melting of boron, the activity coefficient of boron in liquid iron and the activity coefficient of B2O3 in slag were involved, and experimental work on this problem was obviously desirable. The experiments to be described were planned to establish the boron-oxygen relations in liquid iron and to demonstrate at the same time the ferroborate slag compositions in equilibrium with various amounts of oxygen in liquid iron. Accordingly, slags containing varying proportions of iron and boron oxides were held in contact with molten iron, and samples of both slag and metal were analyzed. The limitations upon the accuracy of the data will be considered, but in a practical sense the oxygen levels that can be attained in iron by iron borate slags, and the amounts of boron in iron at these oxygen levels were established. Experimental Procedure No entirely suitable refractory was found for the mixtures of iron oxide and boron oxide used as slags. Crucibles of silica, magnesia, Ramix, beryllia, and zirconia were all tried unsuccessfully. The must satisfactory method discovered for handling them was the rotating-crucible technique, which creates a parabolic crucible of liquid iron.5,6 Even this was not entirely successful, for at steelmaking temperatures (1600°C.) the slags had such a low surface tension that they crept up to the refractory and slowly dissolved it. These difficulties made it impossible to maintain a constant slag composition for an unlimited period Of time. However, by using the rotating technique, short runs could be made in

Jan 1, 1947

By R. C. Ku, R. G. Davies

The stress-strain behavior of Fe-C and Fe-Ni solid-solution alloys has been investigated at 25°C. It is found that the rate of solid-solution strengthening is dependent upon the strain at which the yield stress is measured, the macroyield stress being much more concentration-dependent than the microyield stress. In fact the addition of nickel does not lead to any increase in the microyield stress of iron. The primary effect of increasing the carbon or nickel content is to increase the slope of the stress-strain curve in the microyield region; this effect has been correlated, by means of transmission electron microscopy, with a decreased ability of the dislocations to cross-slip. It is concluded that the Mott-Nabarro theory is a good description of true solid-solution hardening in these and other iron-base alloys. A.LL theories of the solid-solution strengthening1-4 indicate that the flow stress of an alloy increases both with solute concentration and "misfit" between the solvent and solute atoms. The functional relationship between strength, solute concentration, C, and misfit depends upon the particular theory. Mott and Nabarro1,2 and Schoeck and Seeger3 both predict a linear increase in strength with concentration, while Fleischer4 indicates that the strength should be proportional to C1/2; there are in the literature experimental observations to support both these compositional dependencies.1&apos;8 The experimental evidence used to support the theories is the change in macroscopic yield stress (strain, e, = 10-3) with composition. However, recent investigations have revealed that solid-solution strengthening in a Cu-Al single crystals7 and in Fe-V polycrystal-line" alloys depends upon the strain at which the flow stress is measured; a flow stress in the microplastic range (e = 10-6 to 10-5) is much less concentration-dependent than the macroyield stress. Since the theories of solid-solution strengthening are concerned in particular with the stress to move a dislocation in a dislocation-free matrix, they should only be compared with microyield-stress data; it will be shown that in a material deforming homogeneously the microyield stress (e = 10-6) is approximately the stress to move through the matrix those dislocations which have been nucleated by stress concentrations such as particles or grain boundary ledges.9-11 In contrast, the macro-yield stress is more complex in that it is affected by several phenomena: dislocation multiplication, dislocation interactions, and the ease of propagating slip across grain boundaries. For example, it is experimentally observed that when long-range order12&apos;13 or solute effects10 restrict cross alip the grain boundary

Jan 1, 1967

By Gerhard Derge

Metallurgists have used borax as a fluxing agent traditionally, but until recently elemental boron has played an insignificant role as an alloying element. Neither the metal nor its compounds have been regarded as important metallurgical materials and there is a surprising lack of knowledge concerning their metallurgical behavior. The new applications to steel-making of both boron and borates, which arose in part from wartime incentives and restrictions, have been seriously handicapped by this lack of data. For example, rasorite, a naturally occurring sodium borate, has been shown to be an effective substitute for aluminum as a ladle deoxi-dizer in rimming steels.&apos; Likewise, the effectiveness of boron as an alloying agent has been demonstrated,2,3 giving deep hardening when used in restricted amounts. The exploitation of both of these uses has been retarded by the difficulty of attaining suitable metallurgical control. Recognizing that the most important information required was a knowledge of the equilibrium between boron and oxygen dissolved in liquid iron. Gurry4 calculated this relation from the best thermal data available. However, estimates of the entropy of melting of boron, the activity coefficient of boron in liquid iron and the activity coefficient of B2O3 in slag were involved, and experimental work on this problem was obviously desirable. The experiments to be described were planned to establish the boron-oxygen relations in liquid iron and to demonstrate at the same time the ferroborate slag compositions in equilibrium with various amounts of oxygen in liquid iron. Accordingly, slags containing varying proportions of iron and boron oxides were held in contact with molten iron, and samples of both slag and metal were analyzed. The limitations upon the accuracy of the data will be considered, but in a practical sense the oxygen levels that can be attained in iron by iron borate slags, and the amounts of boron in iron at these oxygen levels were established. Experimental Procedure No entirely suitable refractory was found for the mixtures of iron oxide and boron oxide used as slags. Crucibles of silica, magnesia, Ramix, beryllia, and zirconia were all tried unsuccessfully. The must satisfactory method discovered for handling them was the rotating-crucible technique, which creates a parabolic crucible of liquid iron.5,6 Even this was not entirely successful, for at steelmaking temperatures (1600°C.) the slags had such a low surface tension that they crept up to the refractory and slowly dissolved it. These difficulties made it impossible to maintain a constant slag composition for an unlimited period Of time. However, by using the rotating technique, short runs could be made in

Jan 1, 1947

By W. Crafts, J. L. Lamont

Selection of an alloy steel for a heat-treated article has been facilitated by methods for the calculation of harden-ability,&apos; as-quenched hardness and tempered tensile strength.2 Ductility and toughness may also be estimated if the steel is completely hardened on quenching, 5,6 and the present study was carried out in order to develop a basis for estimating the Izod impact strength of partially hardened steel. The investigation was directed toward the prediction of Izod impact strength in steels of normal commercial quality without consideration of special compositions or heat-treatments that might produce abnormal brittleness. It was found that Izod impact strength of alloy steel is controlled by hardness, degree of hardening on quenching, and grain size. In finegrained steels the impact strength for any given degree of hardening is inversely proportional to the tempered Rockwell C hardness, and the relation of impact strength to hardness is lowered by incomplete hardening. Calculation of the tensile strength and impact strength of heat-treating steels has shown that, except at very high strengths, tensile strength is raised by alloys without loss of impact strength whereas the tensile strength gained by higher carbon contents tends to be accom- panied by a disproportionate loss of toughness. Plain carbon steels give relatively low and unpredictable impact strength. The calculation is sufficiently accurate to be helpful in the selection of alloy steel, and common grades of alloy steel have been evaluated with respect to combinations of tensile strength and impact strength attainable after heat-treatment in sections from I to. 4 in. in diameter. Procedure The study of the relation of hardness to impact strength was based on test data derived from 24 heats from four producers. The steels included the following SAE and AISI compositions: 1020, 1030, 1040, 1340, 3310, 33167 4320, 43.30, 4340, 8620, 8630, 8640, 8720, 8730, 8740, 931°, 9317, 9440, 9917 and three high-alloy chromium-nickel-molybdenum steels. As far as is known, the steels tested were of normal commercial quality. They were supplied in 4-in. sections, which were forged to smaller sizes, prenormalized, and machined to final dimensions. Heat-treatment was carried out by heating to the usual austenitizing temperature for the grade of steel, holding for one hour per inch of thickness and quenching in still oil at room temperature. Previous work had indicated that this quenching treatment approximates a severity of H = 0.3; The bars were tempered as follows: 34 in., I in., and 1% in., 2 hr; 235 in., 3 hr; 4 in., ; hr. All bars were air-cooled from the tempering tem-

Jan 1, 1948

By J. L. Lamont, W. Crafts

Selection of an alloy steel for a heat-treated article has been facilitated by methods for the calculation of harden-ability,&apos; as-quenched hardness and tempered tensile strength.2 Ductility and toughness may also be estimated if the steel is completely hardened on quenching, 5,6 and the present study was carried out in order to develop a basis for estimating the Izod impact strength of partially hardened steel. The investigation was directed toward the prediction of Izod impact strength in steels of normal commercial quality without consideration of special compositions or heat-treatments that might produce abnormal brittleness. It was found that Izod impact strength of alloy steel is controlled by hardness, degree of hardening on quenching, and grain size. In finegrained steels the impact strength for any given degree of hardening is inversely proportional to the tempered Rockwell C hardness, and the relation of impact strength to hardness is lowered by incomplete hardening. Calculation of the tensile strength and impact strength of heat-treating steels has shown that, except at very high strengths, tensile strength is raised by alloys without loss of impact strength whereas the tensile strength gained by higher carbon contents tends to be accom- panied by a disproportionate loss of toughness. Plain carbon steels give relatively low and unpredictable impact strength. The calculation is sufficiently accurate to be helpful in the selection of alloy steel, and common grades of alloy steel have been evaluated with respect to combinations of tensile strength and impact strength attainable after heat-treatment in sections from I to. 4 in. in diameter. Procedure The study of the relation of hardness to impact strength was based on test data derived from 24 heats from four producers. The steels included the following SAE and AISI compositions: 1020, 1030, 1040, 1340, 3310, 33167 4320, 43.30, 4340, 8620, 8630, 8640, 8720, 8730, 8740, 931°, 9317, 9440, 9917 and three high-alloy chromium-nickel-molybdenum steels. As far as is known, the steels tested were of normal commercial quality. They were supplied in 4-in. sections, which were forged to smaller sizes, prenormalized, and machined to final dimensions. Heat-treatment was carried out by heating to the usual austenitizing temperature for the grade of steel, holding for one hour per inch of thickness and quenching in still oil at room temperature. Previous work had indicated that this quenching treatment approximates a severity of H = 0.3; The bars were tempered as follows: 34 in., I in., and 1% in., 2 hr; 235 in., 3 hr; 4 in., ; hr. All bars were air-cooled from the tempering tem-

Jan 1, 1948

By Hsun Hu

Three single crystal strips of a 3 pct Si-Fe alloy with approximately (110) [001], (210) [001], and (100) [001] orientations were rolled at room temperature to 30, 50, and 70 pct reductions in thickness. Their deformation and annealing textures were studied. In most cases, the change in texture upon recrystallization and subsequent growth can be described as rotations around the <I10 > axes. A < WO > rotational relationship was also observed. The temperature dependence of recrystallization textures was discussed. WhILE considerable data have been published on the rolling and annealing textures in silicon-iron crystals, very little study has been made on the texture formation at various stages of rolling deformation, and during the process of recrystallization. Dunn&apos; in some of his early works had studied the orientation of recrystallized grains in crystals cut out from lightly rolled (10 to 20 pct reduction) large grained sheets. He found that in most cases a third-order twin relationship exists between the crystal and the recrystallized grains. This orientation relationship actually corresponds to rotations around the <110> axes. The more recent studies of Dunn &apos; and of Dunn and Koh &apos;5 on the rolling and annealing textures in various silicon-iron crystals were concerned mostly with a cold-rolling reduction of 70 pct and annealing at 980OC for recrystallization. Reductions of similar magnitude were also employed by Walter and Hibbard in rolling columnar crystal aggregates of a silicon-iron ingot. A systematic study of the effect of rolling reduction on the deforma- tion and annealing textures is still lacking. Regarding the effect of annealing temperature on the texture formation, Dunn3 has observed a change in therecrys-tallization texture by annealing a 70 pct rolled (1 10) [001] crystal first at a low temperature then atahigh temperature. But the details of texture formation during the annealing treatments were not thoroughly investigated. The present investigation was undertaken to study the texture developments at various stages of rolling deformation and of the recrystallization process, so that a better understanding on the texture formation in silicon-iron crystals may be obtained. EXPERIMENTAL PROCEDURE The three single crystals used in the present investigation were selected from the group of single crystal strips previously prepared7 from a high grade commercial Si-Fe alloy with 3 pct Si. The thickness of these single crystal strips was 0.040 in. The orientations of the three crystals as determined by the X-ray back-reflection Laue technique are shown in Table I. Each of the three crystals was rolled at room temperature along the strip direction to 30, 50, and 70

Jan 1, 1962

By C. S. Barrett, P. Coheur

AXnealing twins are common in the microstructure of copper that has been rolled and recrystallized. In such samples it follows that a twin relationship should exist between components of the re-crystallization texture,&apos; and several examples of this have been reported. For example, twin relationships have been found in recrystallized electrolytic copper sheet, as indicated in Fig. I, from a paper by Coheur and Lejeune.2 In this pole figure the cube texture (100) [001] is indicated by the hollow squares in the lower half of the figure (the pole figure for 200 reflections) and in the upper, (III), part of the figure. The texture contains, in addition to this orientation, the first-order twins of it, shown in the figure by the filled triangles. This orientation relation has been suggested by others also, under certain annealing conditions,3&apos;4 although pole figures have not been published to confirm it. Some orientations in recrystallized sheets are identical with their twins, because of the symmetry elements of the texture— this is true, for example, with the (113) [ZII] texture so commonly reported for brass—hence it appears impossible in such samples to decide whether the twin relationships result from twinning or merely from the symmetry of the deformation process. The present investigation of a commercial copper strip seems to yield an example in which annealing twins account unambiguously for the principal orientations present. It proves to be a case, also, for which the recrystallization texture cannot be viewed as derived from the deformation texture by a first or second-order twinning mechanism. Materials and Methods The samples investigated were of secondary copper (melted in belgium) to which 0.19 per cent iron had been added to raise the recrystallization temperature. How much the orientation characteristics of this metal can be ascribed to the iron content and how much to other impurities or to melting and pouring practice have not been investigated.* The rolling was done in one direction only, on a mill with rolls of about 20-cm diameter. A strip I. cm wide was reduced from 5 mm thickness to 0.05 mm by several cold passes at commercial speeds. The samples cut from this 99 per cent reduced strip were X-rayed throughout their entire thickness. A pole figure made soon after rolling and annealing was identical, within experimental error, with one that was made when a two-year interval occurred between rolling and annealing. X-ray patterns were made on a camera2 that traversed

Jan 1, 1947

By C. S. Barrett, P. Coheur

AXnealing twins are common in the microstructure of copper that has been rolled and recrystallized. In such samples it follows that a twin relationship should exist between components of the re-crystallization texture,&apos; and several examples of this have been reported. For example, twin relationships have been found in recrystallized electrolytic copper sheet, as indicated in Fig. I, from a paper by Coheur and Lejeune.2 In this pole figure the cube texture (100) [001] is indicated by the hollow squares in the lower half of the figure (the pole figure for 200 reflections) and in the upper, (III), part of the figure. The texture contains, in addition to this orientation, the first-order twins of it, shown in the figure by the filled triangles. This orientation relation has been suggested by others also, under certain annealing conditions,3&apos;4 although pole figures have not been published to confirm it. Some orientations in recrystallized sheets are identical with their twins, because of the symmetry elements of the texture— this is true, for example, with the (113) [ZII] texture so commonly reported for brass—hence it appears impossible in such samples to decide whether the twin relationships result from twinning or merely from the symmetry of the deformation process. The present investigation of a commercial copper strip seems to yield an example in which annealing twins account unambiguously for the principal orientations present. It proves to be a case, also, for which the recrystallization texture cannot be viewed as derived from the deformation texture by a first or second-order twinning mechanism. Materials and Methods The samples investigated were of secondary copper (melted in belgium) to which 0.19 per cent iron had been added to raise the recrystallization temperature. How much the orientation characteristics of this metal can be ascribed to the iron content and how much to other impurities or to melting and pouring practice have not been investigated.* The rolling was done in one direction only, on a mill with rolls of about 20-cm diameter. A strip I. cm wide was reduced from 5 mm thickness to 0.05 mm by several cold passes at commercial speeds. The samples cut from this 99 per cent reduced strip were X-rayed throughout their entire thickness. A pole figure made soon after rolling and annealing was identical, within experimental error, with one that was made when a two-year interval occurred between rolling and annealing. X-ray patterns were made on a camera2 that traversed

Jan 1, 1947

By A. A. Smith, J. S. Smart

THE elements silver, cadmium, tin, antimony and tellurium either are found as impurities in commercial coppers or are intentionally added to produce coppers for special uses, When present in small quantities, each of these metals exerts a significant effect on the properties of copper, but despite considerable experience and investigation much remains to be learned about their specific behavior. The presence of extraneous elements, particularly oxygen, complicates the study of individual additions of impurities in the range 0 to 0.05 per cent, and the use of high-purity copper has been found extremely helpful in circumventing these difficulties. It has also been found that individual behavior can be satisfactorily determined from measurements of two commercially important properties, conductivity and softening temperature, according to methods that have been described previously.1,2 Data of this type, obtained in the course of a general investigation of the effects of impurities on the properties of both oxygen-bearing and oxygen-free copper are presented herewith. All samples except those containing cadmium were prepared as 3/8-in. continuously cast oxygen-free rod from pure copper and weighed amounts of a similarly synthesized master alloy. Composition was checked by chemical methods, which in every case verified the calculated analyses. Test wires were cold-drawn one B. and S. number per pass on a string-up machine using four 30-min. 600°C. anneals at 0.3125, 0.257, 0.204 and 0.162 in. and a final cold reduction of 75 per cent to 0.081 in. Some oxygen-bearing samples were produced directly from the 3/8-in. oxygen-free rods by diffusion from a surface scale at 850°C. and drawn to size as listed above, but most of the alloys were remelted in pure graphite and cast through air into a I-in. round mold, The slugs were then hot-rolled to 5/16 in., drawn to 0.162 in., annealed as listed above, and drawn to 0.081 inch. Conductivity wires were annealed for I hr. at 100°C. intervals between 300° and 800°F., using a hydrogen atmosphere for oxygen-free samples and purified nitrogen for the oxygen-bearing type, All samples were quenched from the annealing temperature in 10 per cent H2SO4 and conductivity was measured on a Hoopes bridge that had been checked against a Kelvin bridge. The softening temperatures represent the half-hard stage of the annealing curve as determined by a standard procedure.1 EFFECT OF SILVER Numerous excellent studies of the argentiferous coppers are found in the literature, and these have been adequately

Jan 1, 1943

By M. Cohen, W. J. Harris

The recent application of lineal analysislt2 to the austenite-martensite reaction has made possible a quantitative study of the kinetics of this transformation during rapid cooling. Martensite range curves can thus be constructed to portray the onset of the reaction at Ma and its subsequent progress as a function of temperature down to and below the ambient. It now seems in order to investigate other aspects of the martensite transformation, using this quantitative method of approach. One of the least understood characteristics of the austenite-martensite reaction is that of stabilization which has been defined by Troiano and Greninger3 as &apos;la lowering of Ma, resulting from aging, without change in chemical composition of the parent solid solution." In other words, if the hardening quench is arrested at a predetermined subcritical temperature (TA) for a sufficient period of time, more austenite may be retained at a given lower Or reference temperature (Tr) than if the steel had been cooled directly and rapidly to Tr in the first place. For the purposes of the work at hand, the extent of stabilization produced by the isothermal treatment at Th is measured explicitly in terms of the excess austenite (6) that exists in the steel at T,, over and above the amount that is normally present after direct quenching to T,. T, is conveniently taken to be room temperature, but this choice is not essential and is sometimes undesirable. The holding temperature (TA) may be above or below M,, and still cause stabilization depending upon the themistry of the austenite. stabilization has been found to occur in the presence of bainite4 and of martensite6,6,7,8 as well as in the absence of either,g The phe-nomenon of stabilization is not concerned with (and may even be obscured by) ferrite formation or any other type of phase change occurring at T~ that alters the chemistry of the remaining austenite. Such a structural change would obviously influence the martensite transformation during subscquent cooling. Stabilization, however, is more subtle; it appears to manifest itself without detectable variation of the austenite composition, whether in the presence or absence of transformation products. There are relatively few direct references to stabilization in the literature. The stabilizing effect of room temperature aging and tempering on the subzero transformation of retained austenite has been clearly shown in plain carbon,6,8 low alloy6s7.8 and high alloy tool steels.10&apos;5 ssa- with the as-hardened steel, the degree of stabilization increases with tempering time and temperature through

Jan 1, 1949