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By C. R. Taylor, John Chipman

The study of chemical reactions of liquid steel and basic open-hearth slag involves a complex slag system of at least eight important components, and often a number of others. In initiating an experimental program on the equilibrium relationship of slag and metal, it became evident that but little progress could be expected in the interpretation of the complex slags until an understanding had been gained of the simpler liquid systems composed of a limited number of slag constituents. The simplest system that in any way resembles open-hearth slag must contain lime, silica and iron oxide. Attempts to produce in an induction furnace slags containing only these constituents have met with serious limitations because of the solubility of refractories in the slag. Thus in acid-lined furnaces the slag is always saturated with silica and consequently contains between 48 and 63 per cent of this component. In basic-lined furnaces an undesired additional component, magnesia, is introduced to the extent of some 3 to 15 per cent, depending upon the acidity, sometimes with disastrous results to the furnace. Thus in a magnesia-lined furnace, Fetters and Chipman1 found it impossible to prepare slags in which the ratio (CaO + MgO)/SiO2 was less than that corresponding to the metasilicate (approximately 0.8:I). Between this composition and that of the true acid slags lies a field of composition about which very little is known and which cannot be explored by any ordinary means. This circumstance, as well as the desire to study the more basic slags in the absence of magnesia, calls for the development of a method by which slags may be brought into equilibrium with molten metal without coming in contact with refractory. Such a technic has been provided by the rotating induction furnace developed by Barrett, Holbrook and Wood.2 Three modifications of the rotating furnace were described by these authors. The first was essentially a rotating refractory cylinder containing the magnesia crucible, which was itself heated by a graphite crucible. In the second, only the magnesia crucible rotated, the cylindrical graphite heater being stationary. In the third, the coil and crucible revolved, and the metal was heated directly by induction. Experimental Method Furnace The furnace used in this investigation differed from previous designs and may be Sci- a fourth modification of the original rotating furnace. Its essential fea tures are shown in Fig. I' The Outer case A is a fire-clay flue liner for control of the atmosphere. The top B and base 6 are alberene stone. The coil supports D are of ""Formica," a material formed from phe-

Jan 1, 1943

By Alexander L. Field

The rate of elimination of carbon largely controls the time required to make a heat of steel by the basic open-hearth process and to an important degree determines the cost of refining. Practical experience has led to the generally accepted belief that the use of slags relatively high in iron oxide, such as are required to bring about rapid refining, leads to a certain sacrifice of quality in the product. As a consequence, a compromise must be made between the exceedingly slow rate of carbon drop which would correspond to the ideal case and the rapid rate which would best satisfy the condition of minimum cost. An increase in rate of refining necessarily implies an increase in the concentration of iron oxide dissolved in the metal. However, even for the infinitely slow rate that corresponds to slag-metal equilibrium, the metal would contain a certain definite concentration of dissolved iron oxide. It is a matter of great practical importance, therefore, to determine the quantitative relation between the minimum or equilibrium concentration of iron oxide in the metal and the higher concentrations which must actually obtain in practice. The present paper is devoted to the development of certain equations, derived from the established laws of physical chemistry, which will enable this relation between rate of refining and the degree of oxidation of the metal bath to be computed from operating data. So attempt is made to exhaust the possibilities of this general method of treatment. In considering rate of refining, attention is mainly confined to rate of carbon elimination. However, the equations are of a more general nature and their application may readily be extended. The results of the preliminary calculations given herein indicate that increased rate of refining may have a decided effect in increasing the concentration of iron oxide dissolved in the metal. The uncertainty which attaches to the calculated value for this relationship arises in part from probable errors in experimental data on which the calculations are based, and in part from the lack of complete or favorably disposed information on basic open-hearth practice. When the relation between rate of refining and degree of oxidation of the metal has been more accurately established than has been done in the present paper, it will then become possible to consider what comprises

By J. W. Goss, M. J. Coolbaugh

Most grouting has been done to stop water flaw in mines and for stabilizing foundations of various man-made structures, a survey of the U.S. literature reveals. Apparently Sun Manuel is one of the first mines in this country to use grout extensively underground for strengthening and stabilizing ground in drifts, shafts, and stations. A comparison with other procedures as well as details of the Sun Manuel program are covered. The employment of pressure grouting as a ground stabilizer at the San Manuel Copper Corp. mine reduces delays in both development and production, lowers costs, and makes possible safer working conditions. It specifically reduces delays in haulage operations and permits the maintenance of normal ventilation. In development work this grouting allows faster excavation by cementing together highly fractured or broken ground that otherwise would require extensive cribbing or spiling. In drift repair, it consolidates the loose or fractured rock over the timber or steel drift supports, thus decreasing the frequency of repair, lessening the hazards from falling rock, and curtailing delays due to blockage of drifts by muckpiles and repair operations. Pressure grouting is the process of pumping an accurately controlled mixture of cement and water into loose, fractured, or porous rock. The ratio of water to cement varies according to the nature of the rock encountered, from the thinnest mixture of 30 gal of water per sack of cement, used to fill very fine fissures, to very thick grout of 5 gal of water per sack of cement, used to fill large fissures or extensive areas of loose, broken rock. The pumping pressures at San Manuel vary from about 100 to 1000 psi, depending upon the compactness of the rock, while at other mines the pressures sometimes go as high as 5000 psi. In order to grout an area in which ground water is encountered, the pumping pressure of the grout must be increased by an amount equal to the pressure of the ground water. GROUTING IN DEVELOPMENT WORK The areas under development at San Manuel include many sections of loose, highly fractured rock. Prior to the advent of the grouting program, drifts, shafts, and stations in these areas could not be excavated without utilizing extensive support such as cribbing, spiling, and breast boarding. This slowed down the development work and increased the costs considerably over that required for excavating in more competent ground. Now, when a particularly bad area is contacted, the mining is temporarily stopped while the bad portion of drift or shaft is grouted. After the grouting is completed, the excavating is resumed with an approximate decrease of 50 pct in lost time and costs. Grouting in Drifts and Turnouts: The grouting procedures and patterns used in drifts and turnouts are very similar. The standard procedure for grouting such a turnout is shown in Fig. 1. After the ground is supported as well as possible with cribbing or lagging, the gaps between the back lagging and side lagging are plugged with empty cement sacks or additional timber, if necessary. The ground surrounding the proposed turnout is then grouted in two stages. In the first stage, the broken and caved rock is drilled and grouted to a depth of 5 to 10 ft, depending on the depth of the broken rock. This stage forms a grouted seal that allows higher pressures to be used at depths beyond 10 ft without developing excessive leaks at the face. After a grout hole is drilled, a 10-ft long pipe is wedged tightly into it with empty cement sacks. Grout is then pumped into the hole until the pressure reaches 200 to 300 psi, and the pipe is subsequently removed if it hasn't become cemented in. No more than one hole at a time is drilled and grouted because the grout has a tendency to go from one hole into another, plugging up the latter. Five or six holes are usually adequate for the first 10 ft of grouting. Experience has shown bentonite to be a useful admixture to the grout, particularly when it is indicated that the grout is being lost into large fissures or voids. Bentonite increases the plasticity of the grout enabling it to remain in place more easily until it has begun to set. In the second stage, the longer holes are drilled through the previously grouted rock, after which the

Jan 1, 1961

By W. A. Olds, H. F. Yancey, M. R. Greer

John Griffen (Consulting Engineer, Pittsburgh)— This paper presents much data offering tentative answers to many technical questions that have been raised by the employment of dense-medium processes and, particularly. by use of the drum-type vessel. It is to be hoped that the Bureau of Mines will publish complete detailed data for the 50 or more tests so that it may be studied and analyzed by everyone interested. Such study will take considerable time and effort. The writer is therefore obliged to confine his discussion to a few points he has noted as being open to question. The data in Table VI which shows the recovery efficiency for the 1 to ½-in. fraction as 100 pct raised a question concerning the accuracy of these calculated figures; washability data on the washed coal and refuse show that such a figure is impossible. When the ash content of the misplaced material in the washed coal is higher than that of the misplaced material in the refuse, recovery efficiency must be less than 100 pct. A etudy of the data In Tables 111, IV, V, and VI suggest that this error probably arose from slight errors in calculating the data in Table V and more probably from the small scale used in plotting the washability curves from the Table V data. Using the size consist data and the weight and ash percentages of individual gravity fractions of each size as given in Tables 111 and IV and the reported recovery of 80 pct of washed coal, a revised Table V was calculated, carrying weight and ash percentages to hundredths of a percent instead of rounding off at tenths. This washability data for each size of Belling-ham reconstituted feed was then plotted on large scale washability curves. From this data the new Table XIV was prepared, which agrees very closely with data shown in Table VI except for two important values, theoretical yields and recovery efficiencies. As will be noted the recovery efficiencies in Table XIV are significantly lower than those given in Table VI. A study was then made of the data showing distribution of the specific gravity fractions to washed coal and refuse. This study indicated that when this distribution was based on the fractions as tested at 0.1-sp gr intervals the number of points obtained were insufficient to establish the distribution curves with reasonable precision, which in turn would affect the accuracy of the values for the specific gravity of separation and the error areas. The data in Tables III and IV of the paper and curves prepared therefrom make it possible for the specific gravity fractions to be subdivided further. This was done using 0.05-sp gr fractions and the distribution data so obtained is given in Table XIV, with resulting values for the specific gravity of separation and the error areas. The writer believes that the derived values shown on Table XIV are more accurate than the correspond-

Jan 1, 1955

Charles H. White, Harvard University, Cambridge, Mass, (communication to the Secretary*):—In answer to Mr. Jar-man's questions I am able to say that constant use (during term-time) since 1901 has shown the new appliances in our laboratory to be very satisfactory. The draft in the hoods is sufficient to lift the fumes promptly from the baths and hotplates ; and the occasional application of stove-polish,—usually about three times a year, at the recess-periods,—so well protects all iron-work in the hoods that, up to the present time, there is very little evidence of the corroding action of acid fumes. Iron should never be used in the construction of hoods above

Jan 1, 1906

By H. Cecil Spicer

The results described in this article are based On field work conducted during the periods April-May, I939, and May-July, 1940. The United States Potash Co. is mining potash on Government land under a permit from the Department Of the Interior and the geophysical investigation was completed under a cooperative arrangemerit made between that company and the Conservation Branch Of the Geological Survey. The writer, a member Of the SeCtion of Chemistry and Physics of the Geologic Branch, was assigned to this investigation. Four definite objectives were in mind for the geophysical work in the studies over the salt deposits. The first was to determine the measure Of success that could be attained in this type of work with the resistivity methods that were to be employed. These methods had been introduced into the work of the Conservation Branch by Benjamin E. Jones for the investigation of dam sites, and have been used under his direction by the author for such work. If the method proved to be be an effort was to be made to contour the top of the salt beds and also the other formation boundaries known to be present in this area. Salt-water aquifers were to be studied in an effort to determine their boundaries, and an attempt was to be made to delineate the potash-bearing beds. Earlier Studies Others have made, and reported, restivity studies over saliferous deposits in different areas. Friedell and Messrs. Schlumberger2 reported geophysical work performed in the discovery of the salt domes of Alsace; Carrette and Kelly? described the geology of the same area. Leonardon and Kelly' published a resistivity curve obtained over the Hettenschlag dome, and a further discussion of this same area was given by the Messrs. Schlumberger6 in a communication. Messrs. Alty6 described studies on salt deposits in which the single-probe method was used. sinerez7 mentions that electrical methods were tried over salt deposits in Spain. Geoffrey and Charrin8 show a resistivity curve obtained over marl, gypsiferous marl and salt which is similar to that obtained over the New Mexico salt deposits. Kelly9 reported resistivity work performed with the ground Comparaor of Zuschlag over the salt deposits near Syracuse, N. Y., where the Salina formation is at a depth of 700 to 800 ft. Some structural studies on the potash basin of Alsace are described by Poldini.10 Another single-probe resistivity study, made over salt deposits in New Mexico, is briefly described by Heiland,11 through the courtesy of Harry Aurand, of the Midwest Refining co, Geological Features OF Area Covered The area discussed in this paper is in Eddy County, southeastern New Mexico, a

Jan 1, 1946

By H. Cecil Spicer

The results described in this article are based On field work conducted during the periods April-May, I939, and May-July, 1940. The United States Potash Co. is mining potash on Government land under a permit from the Department Of the Interior and the geophysical investigation was completed under a cooperative arrangemerit made between that company and the Conservation Branch Of the Geological Survey. The writer, a member Of the SeCtion of Chemistry and Physics of the Geologic Branch, was assigned to this investigation. Four definite objectives were in mind for the geophysical work in the studies over the salt deposits. The first was to determine the measure Of success that could be attained in this type of work with the resistivity methods that were to be employed. These methods had been introduced into the work of the Conservation Branch by Benjamin E. Jones for the investigation of dam sites, and have been used under his direction by the author for such work. If the method proved to be be an effort was to be made to contour the top of the salt beds and also the other formation boundaries known to be present in this area. Salt-water aquifers were to be studied in an effort to determine their boundaries, and an attempt was to be made to delineate the potash-bearing beds. Earlier Studies Others have made, and reported, restivity studies over saliferous deposits in different areas. Friedell and Messrs. Schlumberger2 reported geophysical work performed in the discovery of the salt domes of Alsace; Carrette and Kelly? described the geology of the same area. Leonardon and Kelly' published a resistivity curve obtained over the Hettenschlag dome, and a further discussion of this same area was given by the Messrs. Schlumberger6 in a communication. Messrs. Alty6 described studies on salt deposits in which the single-probe method was used. sinerez7 mentions that electrical methods were tried over salt deposits in Spain. Geoffrey and Charrin8 show a resistivity curve obtained over marl, gypsiferous marl and salt which is similar to that obtained over the New Mexico salt deposits. Kelly9 reported resistivity work performed with the ground Comparaor of Zuschlag over the salt deposits near Syracuse, N. Y., where the Salina formation is at a depth of 700 to 800 ft. Some structural studies on the potash basin of Alsace are described by Poldini.10 Another single-probe resistivity study, made over salt deposits in New Mexico, is briefly described by Heiland,11 through the courtesy of Harry Aurand, of the Midwest Refining co, Geological Features OF Area Covered The area discussed in this paper is in Eddy County, southeastern New Mexico, a

Jan 1, 1946

By Frank T. Sisco

DURING the past year the iron and steel industry of the world as a whole operated on a satisfactory basis. No discoveries nor new processes of outstanding importance were announced either here or abroad, although rumors of such were persistent. In general, the efforts of operating and research men in the iron and steel industry seemed to be confined to improving quality and reducing cost, not a new aim, for the same efforts have been noted in nearly all of the annual reviews of the industry for at least fifty years. Most published papers on blast furnace or steel-making practice were of minor importance, at least when judged by the criterion of radical change in process or product. If the number of reports in the technical journals, or articles in the trade press, is used as a basis for comparison, continuous-mill sheet is still the most important single product of the industry; papers were published detailing the results of the investigation of various phases of the

Jan 1, 1938

By Charles T. Holland

In connection with the problems of bumps in coal mines, much has been written concerning the manner in which roof action and methods of mining enter into the pressure effects observed but little has been written upon the relationship between the physical properties of coal and associated rocks and the cause of bumps. The question of the strength of bituminous coal, of its elasticity, and the energy it can absorb and store has been neglected to a considerable extent in connection with this problem. It is generally agreed that one of the necessary conditions for bumps is a strong coal.' Therefore, since the strength of coal is an important factor, a study of this property should be made. several investigators have conducted laboratory experiments upon the strength of coal, using small cubical or rectangular test pieces. An attempt will not be made to go into all of these investigations, but they are briefly summarized in Table I. Experiments of the U. S. Bureau of Mines and of Lawall and Holland (pp. 27 and 34 of ref. 9), however, indicate that regardless of whether the coal is a soft and weak semihituminous (Pocahontas No 3) or a hard and strong bituminous (Stockton) coal, the maximum ultimate unit stress developed in laboratory tests is higher in small cubes than in larger cubes of the Same coal.

Jan 1, 1942

By Charles T. Holland

In connection with the problems of bumps in coal mines, much has been written concerning the manner in which roof action and methods of mining enter into the pressure effects observed but little has been written upon the relationship between the physical properties of coal and associated rocks and the cause of bumps. The question of the strength of bituminous coal, of its elasticity, and the energy it can absorb and store has been neglected to a considerable extent in connection with this problem. It is generally agreed that one of the necessary conditions for bumps is a strong coal.' Therefore, since the strength of coal is an important factor, a study of this property should be made. several investigators have conducted laboratory experiments upon the strength of coal, using small cubical or rectangular test pieces. An attempt will not be made to go into all of these investigations, but they are briefly summarized in Table I. Experiments of the U. S. Bureau of Mines and of Lawall and Holland (pp. 27 and 34 of ref. 9), however, indicate that regardless of whether the coal is a soft and weak semihituminous (Pocahontas No 3) or a hard and strong bituminous (Stockton) coal, the maximum ultimate unit stress developed in laboratory tests is higher in small cubes than in larger cubes of the Same coal.

Jan 1, 1942

Adolph Thies, Haile Gold-Mine, S. C.: I have little to add to what my friends Messrs. Nitze and Wilkens have said on this subject. What I have done in mining during the last fortyone years, partly in this country and partly in South Africa (though not, as to Africa, in the diamond- or the gold-fields,

Jan 1, 1896

By A. Bar-Or, G. Hirsch, P. Wynblatt

The rates of nucleation and growth at various temperatures in U-0.45, 1.1, and 1.35 at. pet Cr alloys were determined, providing a qliantitative proo-f that the transformation under study is controlled by nucleation and diffusional growth. The linear relationship, log NV US 1/T2, suggests that the nucleation of the alloys is probably controlled by the classical law of nuclei formation. The established linear relationship, log G us 1/T, in the three alloys suggests that growth in each alloy is controlled by bidimensional nuclei formation. It was established that both the rate of growth and the rale of nucleation are retarded by chromium. Using classical formulae, sApN and sApG (the ß/a apparent interphase energies) were calculated from the nucleation and growth results, respectively. It was found that their values are of the same order of magnitude. However, why sApN is unaffected by the addition of chromium, while sApG increases with it, needs further clarification. In the last few years, an appreciable amount of research has been conducted into the mechanism of the ß —a transformation in uranium and uranium alloys. Recently, Burke1 reviewed the published work concerned with this transformation. He concluded that in dilute uranium alloys it is firmly established that, at high temperatures in the a range, ß decomposes by a diffusional process. However, he based his conclusion either on experiments dealing with the over-all transformation,2 or on qualitative results.3 It was felt that a better insight into the mechanism of transformation could be gained from the quantitative measurements of growth and nucleation rates, which we aimed to carry out in the present work. In a previous work,4 we have shown that a rim of a grains is formed during isothermal transformation at the high a range. The thickening of this rim with time was used for measuring the rate of growth in U-0.45 at. pet Cr.5 This method was also used in the present work for two more alloys. For meas- uring the rate of nucleation, a method of quenching and macroetching was developed to allow differentiation between a grains formed during isothermal transformation at the upper a range and those formed after quenching, Fig. 1. EXPERIMENTAL WORK AND RESULTS The Rate of Nucleation. The measurement of the rate of nucleation was effected by counting the num-

Jan 1, 1965

By P. R. Sperry, M. L. Holzworth, P. A. Beck

The basic work of Z. Jeffries 1,2,3 has long ago established the main features of grain growth in the presence of a dispersed second phase. Working with sintered specimens of initially fine grained tungsten, to which various amounts of thoria had been added, Jeffries found that grain growth was inhibited, that is, practically prevented, up to a certain annealing temperature. When this temperature, which increased with the thoria content, was exceeded, extremely large grains developed abruptly from the fine grained matrix. such a a temperature" was later found by Gross-mann~3,14 in certain types of steel, while ~~i~ showed15 that in other steels grain growth was gradual, without inhibition and abrupt coarsening. Later work demonstrated the connection between coarsening and aluminum additions. The viewpoint that the direct cause of inhibition and coarsening in aluminum killed steels is a fine dispersion of aluminum oxide21 appears to be held quite generally, although some doubts have been voiced even very recently, 20 In steels with Ti additions the titanium carbide phase is considered responsible for the inhibition effects found.20 The coarsening temperature increases with the titanium content. That coarsening may occur, as a result of, certain heat treatments, even in low carboil rimmed sheet steel, was shown by Samuels. He also detected coarsening in a steel ingot of similar composition, after giving it the same heat treatment as that used by him for the sheet material. In this instance the identity of the inhibiting phase has not been determined. However, Tangerding found23 that even the few small carbide particles, which occur in carbonyl iron, have a very marked inhibitive effect. As a result of an oxidizing anneal at 850°C, large grains begin to form at the surface of the carbonyl iron specimen, and gradually grow inward as the subsurface oxidation of the carbide particles progresses and eliminates the obstruction. The carbide particles Can be removed also by annealing in hydrogen, with similar results. But if the oxidizing anneal of 10 hr at 850°C in air is followed between in hydrogen for 75 hr at the Same temperature, grain growth is more hibition usually the whole specimen is transformed into a single crystal (approx. 1.5 cm X 5 cm). The reversed procedure, that is, hydrogen annealing followed by oxidizing annealing leads to smaller grains. Tangerding arrived at the logical conclusion that there must have been in his specimens some additional obstruction to grain growth hibition from a minor impurity, other than carbon. It seems likely that this obstruction was caused by an oxide formed during the oxidizing anneal and gradually reduced rtain the subsequent hydrogen-annealing. Other instances of grain growth inhibition of varying severity, associated with a dispersed second phase, have been described by several authors. Notable examples: lead with 0.06 pet Cu or Ni,24 cartridge brass with 0.12 pct Cr,25 or with up to 0.15

Jan 1, 1949

By Roy T. Southin*

The finding of Wojciechowski and Chalmers that columnar crystal growth can be stopped by an already existing network of equiaxed crystals is supported by other recently reported work on both static and mechanically stirred ingots.27,28 Support for the dendrite arm fragmentation mechanism, too, can be obtained by comparing the effects of spinning on ingots cast in a material which has a dendritic solid/liquid interface during solidification with one which has a cellular interface, since no evidence of change at the interface, other than a change in growth direction, can be found in the cellular material. But there are alternative ways of producing an equiaxed zone in materials which characteristically solidify with a cellular interface. For example, interrupted spinning of a normally cast ingot can do it. In this case it has been shown28 that the equiaxed zone is caused by the showing of dendritic particles from the top surface of the ingot to nucleate a network of equiaxed crystals which forms a barrier to the continued growth of the columnar grains. This showering has also been shown to be a major effect in materials solidifying with dendritic interfaces. It has also been proposed28,29 that, for an equiaxed zone to form, not only must nuclei be present ahead of the interface but also these nuclei must grow to sufficient size to be a barrier to the further growth of the columnar grains. A further requirement is that a network of these grains continually be produced ahead of the growing interface; otherwise there is a reversion to columnar growth as found by Wojciechowski and Chalmers. In normally cast ingots it is possible for nuclei ahead of the interface to grow since during a large portion of the solidification time there is no temperature gradient ahead of the interface,30 and, in fact, the liquid may be slightly undercooled.29 This then is the major difference between the work under discussion and normal industrial solidification conditions, since Wojciechowski and Chalmers imposed a considerable temperature gradient in the liquid. The statement in the Wojcieshowski and Chalmers paper that one needs to lower the temperature gradient

Jan 1, 1969

By H. B. Aaron

DIFFRACTION micrography provides a useful tool for studying complex strain fields. Newkirk1 observed an X-ray diffraction effect due to strain interactions at the intersection of slip lines in LiF and attributed this effect to a reduction of primary extinction due to strain-gradients. It is the object of the current study to correlate the observations and rationalize the appearance of the strain fields around intersecting slip planes in x-ray extinction contrast studies by a semiempirical method. Fig. 1 shows typical strain patterns observed by Newkirk on (200) reflections in LiF using chromium radiation and a variation of the Berg-Barrett (B-B) technique. In other reflections (e.g., {220}) the strain patterns are absent. If one defines a vector 3 along the striations from the more to the less dense portion, and a vector v in the direction of the X-ray beam parallel to the reflecting plane, such that both 3 and v lie in the reflecting plane of the crystal, Fig. 1, then the positions of the striations on (200) reflections appear to be confined such that where is the angle between v and 3, Fig. 1. It will be seen later that 3 is the projection of Sb on the reflecting planes. In some instances the strain effects are observed only above the slip plane, Fig. l(C), in others only below, Fig. l(D). Where the strains appear to be both above and below the slip line, Fig. l(E), one sees that there are actually two slip lines present, Fig. 1(F) and (G). Furthermore, the strain patterns are observed in the vicinity of the intersection of emergent edge dislocations (diagonal lines on the micrograph) with emergent screw dislocations (horizontal lines on the micrograph), e.g., Fig. l(HJ) and (MN), but not in the vicinity of the intersection of two emergent edge dislocation arrays, Fig. l(HJ) and (KL). However, in the latter case the contrast of the dislocation array itself is reduced along (KL) and increased along (HJ). Line (AB) in Fig. 1 is the edge of the crystal, and the material to the left of (AB) is the side of the sample. Any empirical correlation will have to include most, if not all of the aforementioned observations. Lang2 and Newkirk1 determined that the condition for contrast is given by g-b#0 [2] where b is the Burgers' vector and g the diffraction vector (normal to the reflecting planes). If one assumes that the direction of the observed strain fields is given by the vector sum of the slip vectors (Sb1) of the intersecting slip planes, then Eq. [2] may be generalized to g-S#0 [3]

Jan 1, 1963

By J. H. Richards, G. Derge, W. Peifer

A WIDE Variety of metallurgical defects in steel have commonly been attributed to the presence of excessive amounts of hydrogen. These defects include flakes in rails and forgings, cracks in welds, and blisters in enameled ware, They have been related to hydrogen largely by circumstantiat evidence because the proper sampling and analysis of steel for hydrogen has been known to be difficult and because no general agreement has existed with regard to the relative suitability and accuracy of available methods. The need for a direct approach to these problems has been widely recognized. This general situation has been well described in the publications of the British committee on the Heterogeneity of Steel Ingots,' and current approaches to the problem were reviewed in a recent symposium of the AIME.I2 The plans described by the present authors at that meeting have now matured satisfactorily and will form the basis of this paper. The principal object of this paper will be to describe the methods of sampling and analysis which have been developed and to illustrate the usefulness and limitations of these methods by citing their application to a specific problem, The first problem selected for investigation was the behavior of hydrogen in rail steel. This was chosen because the occurrence of shatter cracks in rails has received a great deal of study over a long period of time. The defect can be controlled by the expensive procedure of slow in However, it may be hoped that a better understanding of the factors influencing the hydrogen content of rails will lead to a more efficient control of this problem. Rails provide a good starting point for a more general study of hydrogen in steel because they provide a cross-section large enough to develop cracks, Yet small enough for convenient handling and sampling. Rails were also selected because they arc made from plain carbon steel and it was felt that the initial work should not be complicated by the effects introduced by alloying elements. The considerations which determined the original planning of this study should be reviewed. The inherently complex nature of most hydrogen problems requires that a large amount of data must be collected for any particular case. This in turn means that any analytical procedure should be as rapid and simple as possible. The same objective of speed is indicated by the fact that it may finally become desirable to use hydrogen analysis in process control. It is also known that hydrogen is highly fugitive and that any procedure which facilitat~s early analysis of the sample without prolonged or irregular storage has distinct advantages. The most important previously reported methods of analysis may be classified into three general groups: (I) Vacuum fusion, (2) Vacuum extraction (without melting), (3) Total combustion.

Jan 1, 1949

By G. Derge, W. Peifer, J. H. Richards

A WIDE Variety of metallurgical defects in steel have commonly been attributed to the presence of excessive amounts of hydrogen. These defects include flakes in rails and forgings, cracks in welds, and blisters in enameled ware, They have been related to hydrogen largely by circumstantiat evidence because the proper sampling and analysis of steel for hydrogen has been known to be difficult and because no general agreement has existed with regard to the relative suitability and accuracy of available methods. The need for a direct approach to these problems has been widely recognized. This general situation has been well described in the publications of the British committee on the Heterogeneity of Steel Ingots,' and current approaches to the problem were reviewed in a recent symposium of the AIME.I2 The plans described by the present authors at that meeting have now matured satisfactorily and will form the basis of this paper. The principal object of this paper will be to describe the methods of sampling and analysis which have been developed and to illustrate the usefulness and limitations of these methods by citing their application to a specific problem, The first problem selected for investigation was the behavior of hydrogen in rail steel. This was chosen because the occurrence of shatter cracks in rails has received a great deal of study over a long period of time. The defect can be controlled by the expensive procedure of slow in However, it may be hoped that a better understanding of the factors influencing the hydrogen content of rails will lead to a more efficient control of this problem. Rails provide a good starting point for a more general study of hydrogen in steel because they provide a cross-section large enough to develop cracks, Yet small enough for convenient handling and sampling. Rails were also selected because they arc made from plain carbon steel and it was felt that the initial work should not be complicated by the effects introduced by alloying elements. The considerations which determined the original planning of this study should be reviewed. The inherently complex nature of most hydrogen problems requires that a large amount of data must be collected for any particular case. This in turn means that any analytical procedure should be as rapid and simple as possible. The same objective of speed is indicated by the fact that it may finally become desirable to use hydrogen analysis in process control. It is also known that hydrogen is highly fugitive and that any procedure which facilitat~s early analysis of the sample without prolonged or irregular storage has distinct advantages. The most important previously reported methods of analysis may be classified into three general groups: (I) Vacuum fusion, (2) Vacuum extraction (without melting), (3) Total combustion.

Jan 1, 1949

By C. M. Schwartz, A. E. Austin, W. B. Wilson

High-temperature X-ray diffraction studies were conducted with Th-U alloys with up to 10 wt pet U. The solid solubility of uranium in thorium as a function of temperature was determined by the method of lattice parameters. Thorium will dissolve up to 2.5 wt pet U at 950°, 4.5 wt pet U at 1150°, and 7.5 wt pet U at 1250°C. Determinations were made of the temperature of the transition of thorium and of the effect of uranium upon the transition. The a to ß transition for thorium was observed to occur at 1330' ±20°C. Mean coefficients of expansion were calculated for thorium and two alloys, and for ThO2 in contact with the thorium, using X-ray lattice-parameter data. Values obtained at 950° C for thorium and Tho2 were 12.1 and 9.40 X 10-6 per OC, respectively. Impurities obtained during the X-ray exposure were identified by diffraction and were essentially Tho2 and ThC, with two additional unknown phases being detected. The effect of the impurities upon the results is discussed. DIRECT investigation (i.e., high-temperature X-ray diffraction studies) of the phase diagram of thorium-rich uranium alloys has been shown to be necessary since recent work1 - has disclosed the presence of an allotropic transformation near 1400°C in pure thorium with the room temperature face-centered-cubic phase transforming to a body-cen-tered-cubic structure at the elevated temperature. The effect upon the transition of the addition of uranium to thorium and of the solubility of uranium in thorium at high temperatures remained unknown, yet was of interest in understanding fabrication procedures and elevated temperature use. The present work was undertaken to provide information in this area by determining the transition temperature, the effect of uranium on the transition temperature, and the solubility of uranium in thorium as a function of temperature. Experimental Work The high-temperature diffraction data were obtained using a camera especially designed for the purpose3 and capable of reaching temperatures in excess of 2000°C at pressures as low as 1 x 10." mm Hg. Temperature regulation was provided by regulating the power input to ±0.1 pet variation, and by regulating the water flow through the camera jacket to provide a constant thermal load. The X-ray sample was a rod nominally 80 mil diam, which was further turned down to 20 mil and then etched to 18 mil over 1/2 in. of one end. This was placed in the sample holder and mounted on the camera so that the smaller part was surrounded by a cylindrical tantalum-sheet radiation-type heating element. Diffraction from the sample was recorded on film after passing through a slot in the heating element and radiation-baffle shield and through beryllium vacuum windows. The X-ray film mounting was of the Straumanis type4 with a camera diameter of 114.59 mm. Since previous work of Chiotti' indicated that impurities considerably alter the transition temperature, chemical analysis of the arc melted iodide crystal-bar thorium samples was obtained prior to testing. The analysis disclosed the material to contain as low as 0.001 ±0,0002 wt pet H and 0.007 ±0.001 wt pet 0. Carbon was 0.003 wt pet and nitrogen less than 0.002 wt pet. This material was sealed in mild steel in an inert atmosphere and subsequently hot rolled to 3/8-in. diam rods at a temperature of 732°C. Following removal of the jacket, the material was pickled and cold swaged to 1/8-in. rods, from which the diffraction samples were prepared. The alloys were similarly prepared, with the uranium being added during arc melting. The uranium analyses of the alloys prepared appear in Table I. The experimental procedure for diffraction examination of the three samples of high-purity thorium differed from those of the Th-U alloys. The original practice, later modified, consisted of pumping down the camera with the diffusion pump on and then admitting liquid nitrogen to the cold trap of the system. This was modified for the Th-U alloys by maintaining liquid nitrogen in the cold trap at all times before and while the diffusion pump was heated. This minor change produced a reduction in the amount of carbon pickup by the sample during exposure to the diffusion-pump vapors. The sample was brought to the desired test temperature and exposed for 21/2 hr at pressures which were usually 2 x 10-6 mm Hg, or lower. Exposures were made at

Jan 1, 1959

By H. C. Fiedler

A high degree of cuhe-on-edge grain orientation and good magnetic properties were obtained in Si-Fe strip processed from laboratory heats containing vanadium nitride inclusions. The higher the nitrogen content the greater was the restraint on normal grain growth and the greater was the ability to undergo secondary recrystal-lization. The degree of restraint in a heat containing magnanese sulfide inclusions was slightly greater than that in the lowest nitrogen vanadium nitride heat. The high rate of diffusion of nitrogen in the temperature range in which the texture is developed makes it necessary to retard the loss of the inclusions until the texture has been developed. MAY and Turnbulll have shown that to develop the cube-on-edge secondary recrystallization texture in Si-Fe it is necessary that inclusions, such as manganese sulfide, be present to prevent normal grain growth. They showed that the driving force for the growth of the secondary grains is inversely proportional to the diameter of the matrix grains, and that the function of the inclusions is to maintain a small matrix grain size. Fast3has developed cube-on- edge texture in Si-Fe by nitriding the hot rolled band. The silicon nitride thereby formed promotes secondary recrystallization during the anneal of the final gage strip. To obtain the best magnetic properties, the inclusions must be removed from the strip after the grain orientation has been developed. Nitride inclusions have an inherent advantage over sulfide inclusions in that the greater diffusivity of nitrogen as comared to sulfur permits the use of shorter times and or lower temperatures for the purification heat treatment. The purpose of the work to be described was to examine the usefulness of vanadium nitride inclusions in developing the cube-on-edge texture and to determine the magnetic properties of oriented strip made from heats containing these inclusions. A comparison is made with a heat having had iden-

Jan 1, 1962

By R. Ruka, E. A. Gulbransen

ONE of the interesting questions in the understanding of the reaction of iron with oxygen is the kinetics and the mechanism of the crystal structure changes occurring in the formation and breakdown of the oxide film. In a recent work' the electron diffraction method was applied to the study of the solid phase reactions occurring internally in the oxide film on iron above 570°C and under vacuum conditions. The higher oxides which form under oxidizing conditions are reduced internally by the diffusion of iron into the oxide leaving the bulk of the oxide FeO (wüstite). This paper will ask and consider three questions. These are: (1) What is the nature of the depressed transformation temperature for the Fe3O4 + Fe ? 4Fe0 reaction in very thin oxide films?; (2) What is the mechanism of the forward transformation of Fe3O4 to FeO at or near 570°C?; and (3) What is the nature and mechanism of the slow reverse transformation of FeO to Fe3O4 and Fe below 570°C?. The composition of the oxide as well as its electrical, magnetic, mechanical, and chemical properties depends upon the kinetics of these reactions. Literature Survey The composition of the oxide film on pure iron at temperatures up to 570°C has been studied extensively by the electron diffraction method. Nelson,' Jackson and Quarrell,3 and Gulbransen and Hick-man4 have shown that Fe3O4 and a-Fe2O8 are formed in the temperature range of 225" to 570°C, while y-Fe,O, is most likely formed below 225°C for long oxidation times. In very thin films FeO (wüstite) is found to form at temperatures as low as 400°C, and its existence depends essentially upon the extent of initial oxidation. FeO is not found in the formation of thick films below 570°C. On the other hand X-ray5 and micrographic8 studies show that Fe3O4 may exist as the main com-ponent in thick films up to 650°C, well above the equilibrium temperature for the reaction Fe3O4 + Fe ? 4FeO. The kinetics of the forward and reverse trans-formations of the reaction Fe3O4 + Fe ? 4FeO have not been studied in oxide films. However, analysis of the data of Gulbransen and Hickman4 on the heat-ing and cooling of iron oxide films of known thick-nesses in high vacua shows that the forward reac-tion proceeds rapidly even for a 4000 A film at temperatures of 575" to 600°C. The reverse reaction or decomposition of wüstite (FeO) occurs at tem-peratures below 450°C. Thus, there appears to be a slow process in the decomposition which is in marked contrast to the rapid forward reaction. The decomposition of a bulk sample of FeO free from the metal has been studied extensively by Chaudron, Benard and coworkers using the micro-graphic, X-ray diffraction, and thermomagnetic methods. Chaudron7,8 first observed that the de-composition of FeO (wüstite) below 570°C occurs by the reaction 4FeO ? Fe3O4 + Fe. Later work by Chaudron and Forestier5 showed that the rate of de-

Jan 1, 1951