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By R. V. Riley

IN the metallographic examination of the alloys of iron and silicon, several investigators1-' have reported on the occurrence of an unusual type of etched structure, particularly in the alloys of higher silicon content. This, the so-called "barley shell" structure, has been observed with iron-silicon alloys over a wide range of silicon content, and under certain circumstances it can be seen upon the micro-sections of pure iron. The barley shell structure may be demonstrated most easily with iron-silicon alloys in the range 8 to 20 pct Si after etching in a hydrofluoric acid base etchant. Two etchants which produce the structure are: Corson's reagent, which is 2 parts hydrofluoric acid, 1 part nitric acid, and 2 parts glycerol; and picric acid reagent, which is 1 part hydrofluoric acid and 1 part saturated solution of picric acid in alcohol. Both when freshly prepared and used for etching commercial silicon-iron alloys containing 14 to 16 pct Si, invariably produce the barley shell structure shown in Fig. la. It is now well known that the barley shell structure is a pseudomorph and the true structure of an alloy of this composition consists of a single phase of silico-ferrite together with graphite as shown in Fig. lb. Lower silicon alloys and even pure electrolytic iron may also be etched in the above reagents to give the barley shell provided the etchant has been either: 1—Stored in contact with glass or silica, or 2—used previously for etching an iron containing silicon. Pure iron etched in perfectly pure hydrofluoric acid base etchants free from silicon contamination gives a normal structure free from the barley shells. Therefore, although the hydrofluoric acid in the reagent primarily is responsible for the barley shells, silicon, or its compounds, also must be present, either in the etching reagent or in the specimen. It was of considerable interest to the author to read the paper by Wachtell,? in which the barley shell etch was deliberately used for the identification of the boundaries of high and low silicon areas in diffusion experiments made upon laminate bars of compacted and sintered pure iron and ferrosili-con powders. This method of utilizing the barley shell etch is novel and in the hands of the investigator gave a useful differentiation between the high and low silicon areas in those specimens. For the reasons already given, however, the technique is not to be regarded as of universal application. Misleading results might be obtained, for example, if two or more specimens were etched in the same etchant. Fresh pure reagents only must be used each time. Provided this is done and the investigators are well aware of the limitations of the method, then the barley shell pseudomorph can be made of limited use in distinguishing between higher and lower silicon areas in a microspecimen of a ferrous material. The greatest of care must be exercised in the interpretation of the results which may be regarded as qualitative only and may, in fact, not be specific to silicon alloys.

Jan 1, 1952

By R. Maddin, W. R. Hibbard

A series of X ray experiments conducted by G. I. Taylor' in 1927 and later substantiated in 1939 by J. A. Collins2 both on axially strained aluminum single crystals, revealed evidence that during single slip crystallite rotation occurs in such a manner that " all parts of the material rotated about the transverse direction in the plane of slip."l The actual method of preparing the specimens for X ray examination is not discussed in detail by Taylor except to say that "this specimen was cut parallel to the plane of slip, as calculated from measurements of marks in the surface of the specimen. It was ground and etched till the effect of the new cuts had disappeared. This was verified by applying the same treatment to an un-distorted specimen. The X ray reflectionsl in this case were perfect ones."' Collins, on the other hand, cut his crystals in a mechanical shaper. These surfaces were polished on No. 1, No. 1/0, No. 2/0 and No. 3/0 papers and on a broadcloth lap using No. 600 alundum as a polishing medium. "Finally, the surface was deeply etched in Tucker's reagent. An unde-formed crystal was prepared in the manner described and X rayed to determine whether or not the machining and polishing operations had produced any strain or distortion in the crystal. The Laue spots all seem to be sharp, free from tails and streaks indicating no detectable strains had been introduced in the crystals." Taylor's X ray technique involved the use of "homogeneous X rays from an iron anti-cathode"; whereas Collins used Ka radiation of copper at 31kv and 20 milliamperes. Glancing angle X ray photograms were taken (1) with the axis of rotation of the spectrometer table in the plane of slip and at right angles to the slip direction, and (2) with the axis of the spectrometer table lying along the slip direction. However, eight minute exposures were used in each case and the angle setting of the spectrometer table was increased by one degree for each exposure. With the discovery of the action of three slip systems3 in the plastic deformation of single crystalline alpha brass where, formerly, only one had

Jan 1, 1950

By O. Schaaber

THE existence of isothermal martensite without the presence of the athermal form thus far has been established only in a 6 pct Mn, 0.6 pct C steel' and a 23 pct Ni, 3.5 pct Mn-Fe alloy.' " Theoretical calculations, moreover, predict this phenomenon to be observable only within narrow composition limits.' In all other steels, it is generally considered that martensite inevitably forms upon cooling below the M, temperature. Even the possibility of isothermal martensite transformation has been questioned for the common steels, although Averbach and Cohen" showed that martensite formation does not stop when the cooling is arrested and that as much as 5 pct retained austenite may transform isothermally to martensite at room temperature. This note presents some observations made on a number of low alloy steels by dilatometric and inductive measurement of isothermal austenite transformation at various temperatures close to the Ms. In the dilatometer studies reported previously, austenitized specimens were immersed in a salt bath maintained at proper temperature and immediately inserted into the dilatometera8' already at thermal equilibrium with the bath. The dilation was read on a dial gage divided into 0.001 mm intervals. Induction measurements were made with a separate excitation source and a test coil, sealed together in a salt-tight case. The increase in the induced voltage caused by the transformation products was recorded at a paper speed of 4 mm per sec. The steels studied are listed in Table I. Specimens prepared from steels 1 and 2 were in the form of hollow cylinders 60 mm long, 10 mm ID, 14 to 16 mm OD, while specimens of steels 3 and 4 were in the form of notched-bar impact test specimens, DVM type. Specimens of steel 5 were in the form of strip, 7x0.3 mm. In the bainitic range, curves representing the amount of transformation vs log time have a single step appearance, as is shown by the curve of isothermal transformation at 320°C in Fig. 1.Y ransformation proceeds in accordance with the Austin-Rickett equationo P -----------= k t" 100-P where P is the percentage of transformed austenite, t is time, and k and n are constants. Near the M, temperature, however, complex curves having two steps are observed. As shown in a previous papera for steel 3 isothermally transformed at 245"C, such complex curves can be separated into two separate transformations or reactions each following the Austin-Rickett equation. The values of n in the equation for a number of such two-step transformations are listed in Table 11 for steel 1. At transformation temperatures of 250" and 235"C, evidence of a second transformation is very

Jan 1, 1956

By D. Turnbull, A. M. Turkalo

It is well known that if copper that has been severely cold-worked by rolling (70-98 pct) is heated to high temperatures a small number of large grains are formed at the expense of the fine grained structure that appears upon primary recrystallization. Dahl and Pawlek,' Cook and Mac-Quarie,2 Ward,3 and Boas and Bowles4 have studied this phenomenon in copper. It has been reported as taking place with measurable velocities in the temperature range 700-1080". Boas and Bowles have reported that the time necessary for the transformation is of the order of days at 700°C. According to Ward3 the number of secondary grains which appear in OFHC copper decrease with increasing perfection of cubical alignment after primary recrystallization; also the perfection of cubical alignment increases with decreasing grain size prior to the final reduction. In this investigation two heats, A and B, of especially high purity copper (99.999 pct) supplied by the American Smelting and Refining Co., were used. The behavior of samples prepared from the two heats was qualitatively very similar providing that the grain sizes established prior to the final reduction were about the same. We observed that in specimens prepared from bars which were relatively coarse grained prior to final reduction secondary recrystallization took place at a rapid rate at temperatures as low as 500°C. This is about 200-300°C lower than the temperature necessary to obtain fairly rapid transformation in OFHC copper. A 0.22 in. thick rectangular bar of lot B was cold-reduced 60 pct by straight rolling and given a penultimate annealing treatment at 250°C. Following this it was cold-reduced 90 pct and heated to various temperatures in the range 450-1040°C. The specimens were about 8 mils thick

Jan 1, 1950

By H. H. Rachford, W. P. Schultz

The use of computing machines to solve physical problems has made it imperative to represent physical data in a form computing machines can use. Although curve-fitting is an old and well-practiced art, there still seems to be some interest in questions regarding what methods can be used and why. Even though there are many good references on this subject, it may be of some value to discuss a particular method which has been found to be useful, and to make available the associated tables for its use in the hope that there can be saved a few of the tedious hours necessary to reduce many of the suggested methods to practice. Although a very brief discussion of the mathematical background of the tables is included immediately below, those interested only in their use can skip directly to the section on Use of the Tables. Direct Fit of a Set of Points A frequently encountered problem is: Given data which can be represented by a smooth curve +(x), to find an easy-to-evaluate function F(x), with only a few coefficients, which is a good approximation of +(x) on the interval 0 5 x 5 x,,. Consider F(x) as a linear combination of m + 1 arbitrary, single-valued, continuous, linearly independent functions, f,(x), Ff.r) = a,f,,(x) + a,f,(x) + . . . -+ aifi(x) + If the value of Q(x) is known or can be read from the curve at the points xj: +(x,), +(x,), . . . +(xj) . . . +(x.), and if n = m, then all the coefficients of F(x) can be determined, and F(x,) — +(x,) = 0 for j =. 0, 1, . . . n. This follows from the solution of the set of linear simultaneous equations. +(x<.) = aofu(x,) + aJI(x0) + . . . + a,,f,,(x,) =a, = f,,(x,) + a,f,(x,) + . . . + a,f,,(x,) +(x,,) = a,,f,(x,,) + a,f,(x,) + ... + a,,f.,(x,,) ...........(2) for the coefficients ai. Although the set a, from the solutions of the set of Equations 2 yields an fix) which gives an exact value of $(x,) for the n + 1 points, there is no restraint on ~(xj in the interval xi < x < xj+,. Indeed, if the points +(x,) are not sufficiently smooth, very serious differences may arise between F(x) in the interval and the smooth curve +(x). Least-Squares Fit It has been suggested&apos; that if n is made to exceed m, and the set a, is found to minimize the function the function F(x) is much less sensitive to small errors in +(xi), and usually provides a much better fit to the smooth function +(x). This is known as the best fit in the sense of the least-squares error. To minimize $, set £ = 0,i = 0,1,... iTi,.....(3) The m + 1 equations from Equation 3 are k—n k=n a.^p /,,(a) f,(xt) + a, X A: = 0 k=O k = n k = n k=0 k=0 +(x.) f,(x,),............(4) one equation being obtained for each i = 0, 1, . . . m. Inasmuch as the arbitrary functions f(x) may be evaluated for x,, k = 0, 1, . . . n, and the +(x,) are known values of the curve to be fitted, the simultaneous Equations 4 may be solved for the set a,. Particular Functions Given the functions fi(x) and the set +(xj), the solutions for require evaluating a number of sums of products as well as the solution of an m + 1 order set

Jan 1, 1956

By E. C. Roberts

TO facilitate some recent microscopic investigations it was necessary to devise special mounting techniques for the polishing of two quite different metallographic specimens. These techniques are extremely simple and are submitted for whatever value they may be to other investigators. The first specimen mount proved very satisfactory for the study of untempered martensite. Since it was undesirable to heat the specimen, lucite or bakelite mounting materials could not be used in the conventional manner. A cold mount was made by drilling a hole of the same diameter as the specimen in a cylindrical piece of polystyrene then press- ing the steel specimen into the hole on an ordinary vise. A prefabricated disk of lucite should work equally well. The only precautions necessary are that the hole be drilled out cleanly and the piece of steel be pressed into the plastic uniformly, otherwise the mount will crack. The second type of mount was required for the study of slag specimens by reflected light. Mounting these specimens in bakelite and then attempting to rough finish the surfaces on graded emery papers resulted in a considerable amount of chipping and breaking out of the slag particles. This made further satisfactory polishing almost impossible. It was found, however, that if the bakelite-mounted specimen was first rough finished to a point where a good specimen surface became visible, the interstices in the specimen surface could be filled and the polishing completed. This filling was accomplished by placing a small amount of lucite powder in the bottom of the steel specimen mold then reinserting the bakelite-mounted specimen on top of the lucite powder. Reheating the mold to the proper temperature and applying the required pressure resulted in the formation of a thin disk of lucite on the bottom of the bakelite specimen. By carefully grinding the lucite away a uniform surface including the slag specimen was obtained and further polishing was unhampered by slag disintegration.

Jan 1, 1951

By P. R. Hines

Diphenyl guanidine is used as an accelerator in vulcanizing rubber. Other rubber accelerators are also flotation collectors, e.g., dithiocarbamate, thiazole, and the xanthates. Urea and its derivatives are good flotation collectors,&apos; and guanidine is the nitrogen analog of urea. These two characteristics suggested testing diphenyl guanidine as a flotation collector. Diphenyl guanidine has been tried in flotation work previously, but references give no details.&apos;.&apos; Bunker Hill Co. of Kellogg, Idaho, supplied the ore sample used in these tests. The sample was typical of the ore milled in 1949 and contained 4.52 pct Pb and 1.08 pct Zn. A flotation test made by the author with potassium ethyl xanthate as a collector, the same flotation reagents, and the same grind employed in regular Bunker Hill mill practice was the standard for comparing results with the compounds and derivatives of guanidine. The compounds and derivatives of guanidine are only fair collectors of galena. However, if potassium ethyl xanthate were used in the galena float, its presence later in the sphalerite float would make it impossible to introduce another type of collector and be certain which collector contributed the result, so the compound or derivative of guanidine under test was used in both the galena and sphalerite floats in Table I. On both the galena and the sphalerite in the Bunker Hill ore, the depressing action of sodium cyanide and zinc sulfate is much greater with collectors of the guanidine type than with the xanthates. If the depressing agents are left out when a guanidine type of collector is used, but a pH of 8.6 is maintained with either lime or sodium carbonate, the depressing action is approximately the same as in the standard xanthate test. Consequently the depressing agents, sodium cyanide and zinc, were not used in the galena floats of tests 1226, 1228, and 1286, Table I, so the galena floats would be on a comparable basis with the standard xanthate test. As shown by the tests in Table I, the loss in the tail when diphenyl guanidine is used is 8.3 to 9.3 pct, as compared to 17.6 pct with potassium ethyl xanthate, or a recovery of 2.3 to 2.0 lb more zinc. Concentrate grade is 13.7 pct with potassium ethyl xanthate and increases to 22.9 and 31.8 pct with diphenyl guanidine, showing a much higher selectivity. Unless the Barrett&apos;s No. 4 coal tar creosote is considered to be a collector, no collector other than diphenyl guanidine is present in the tests, Nos. 1226, 1228, and 1286. Tests 1218, 1253, and 1263 in Table I1 were run to check the effect of the depressing agents used in flotation of the galena (sodium cyanide and zinc sulfate) upon subsequent flotation of sphalerite by diphenyl guanidine. Urea was substituted for potassium ethyl xanthate in tests 1253 and 1263 because it is a good collector for galena and a poor one for sphalerite, and the effect of the depressing agents is more marked with urea than with potassium ethyl xanthate. Test 1205 checks the effect of urea alone without any depressing agents when used for the flotation of galena. Table I1 shows that diphenyl guanidine as a collector for sphalerite is compatible with other flotation reagents used in floating galena. When the depressing agents sodium cyanide and zinc sulfate are used in the galena flotation step, the amount of lime in the sphalerite flotation must be increased (compare 1253 and 1263). Table I11 gives some of the compounds of guanidine which were tested and compared. Some of the compounds and derivatives of guanidine* are solu- * Diphenyl guanidine is in commercial production and is available on the market. ble in water and others are not. Those tested were fed dry. When an organic collector is promising, its compounds and derivatives should be tested and their comparative collecting power recorded. Eventually, in this way, it may be possible to discover some of the essential chemical characteristics of a good collector. For example, it is interesting to compare the diphenyl and dibutyl derivatives in Table IV with those of urea in Table 111, Example 3, U. S. Patent 2,664,198. All are good collectors. Table I shows some of the effects of lime on recovery of sphalerite by diphenyl guanidine. Table V

Jan 1, 1960

By W. B. Lilienthal

A considerable saving in time and money has been effected by use of a specially designed stainless steel container for laboratory drilling mud test work. This container involves use of a standard tall-form stainless steel beaker for service in which the mud sample is heated to an elevated temperature and maintained there for protracted periods of time, while undergoing agitation to facilitate mixing of mud components. Agitation is accomplished by rotating the filled containers on motor-driven rollers within an oven. Several porcelain balls are generally placed in the containers to further improve agitation. Soft glass containers (.Mason jars) were used in this service in early work, and were found to be unsuitable for the following reasons: 1. Poor resistance to thermal shock. 2. Containers could withstand only relatively low pressures. 3. Accidental breakage in handling. 4. Chemical deterioration and subsequent mud contamination from reaction of high pH muds with the glass at elevated temperatures. Pyrex containers were also considered, but, inasmuch as they provided improvement only in items 1 and 4 listed above the additional cost was not believed to be justified. A scale drawing of the container is shown in the figure illustrating details in cross-section. A pressed stainless steel lid was fabricated to match the rolled edge of the beaker

Jan 1, 1950

By E. P. Klier, Volker Weiss, George Sachs

IT has been shown that the isothermal transformation of austenite in a special steel can be modified by isothermal holding in the high subcritical transformation range.&apos; Since this treatment potentially leads to increased hardenability, limited testing has been completed to determine if the stabilization effects observed with this treatment can be used to advantage in the heat-treating of 4340 steel. As an index of the effects of the several austenitizing treatments on the hardenability of the steel, Jominy-type hardenability tests were completed for specimens 2.5 in. in diameter and 8 in. long. Since the steel studied is to be used at strength levels where notch sensitivity is of major concern, notch sensitivity after selected austenitizing treatments has been evaluated by notch tensile tests for several specimen sizes. The steel composition and the austenitizing treatments are given in Table I. The test specimens are presented in Fig. 1. The hardenability data are given in Fig. 2 and the notch tensile properties are presented in Fig. 3. The hardenability of the steel investigated when determined by use of the standard Jominy test specimen2 as high and remained essentially unchanged for the different austenitizing treatments. For the larger test specimen, as has been shown by other investigations," the characteristic hardenability indexes are changed and it becomes possible to isolate austenitizing treatments which promote maximum hardenability. The stepped austenitizing treatment promotes higher hardenability as is indicated in Fig. 2. The evaluation of notch sensitivity for very high strength steels is best accomplished by means of the notch tensile test. The experimental conditions of the test, however, modify the notch strengths measured, and in the present experimentation an effort was made to achieve a limiting notch condition by fixing the notch root radius at 0.001 in. while the specimen diameter was allowed to increase from 0.3 to 1.1 in.* For this root radius the notch strength, 0.3-in.-diam specimen, and this trend differs from that for the larger specimens. At the highest tempering temperatures the 1.1-ip.-diam specimens yield comparable results for the austenitizing treatments compared. However, as the tempering temperature is progressively lowered below 800°F, em-

Jan 1, 1958

By H. W. Paxton, C. C. Busby

IT has been shown previously&apos; that strain aging can markedly improve the tensile properties of low carbon martensites, especially the yield-tensile ratio, without seriously affecting the ductility. In view of interest in high strength steels, an investigation has been made of the effect of strain aging following tension or rolling on the tensile properties of A1S1 4340 in an attempt to obtain a tensile

Jan 1, 1957

By J. L. Wyatt

THE strain sensitivity, K, a property of metals defined as the unit change in electrical resistance per unit strain, was measured for commercial purity titanium wire to determine its usefulness as a strain gage material. A Kelvin double bridge, accurate to 0.000001 ohm, was used to make measurements from 0 to 1 pct total strain. A positive value of 0.17 for K was found. This compares with 2.15 for constantan and 3.5 for cold-worked invar, two of the more common strain gage materials. The effect of temperature also was determined. It was found that a change in temperature of 30°F caused the same resistance change as 1 pct strain. It is therefore concluded that titanium would have utility as a strain gage only if the thermal fluctuations in the specimen could be controlled to a high degree and in applications of very large total strain.

Jan 1, 1953

By N. Brown

IT has been observed that a hexagonal-close-packed crystal will undergo the same macroscopic displacements as an isotropic material if the basal plane is perpendicular to the axis of twist.&apos; Other orientations may produce both bending and twisting, but this analysis will be confined to pure torsion of a right circular cylinder. The z axis, the axis of twist, and the specimen axis are coincident. The displacements are given by Uq = rz, Ur = Uz = 0 [1] where 4 is the angle of twist per unit length. This requires rotational slip, as discussed by Frank&apos; and Wilman, which may be observed readily. The relative rotation of adjoining slip planes is simply produced by a movement of a planar grid of screw dislocations."." The screw dislocations are of the same sign and they move radially inward. For hexagonal-close-packed metals, the grid is hexagonal and the screw dislocations lie in the < 2110 > directions. The displacement of a point is the resultant of two displacements produced by intersecting screws sweeping over the point. The dislocations must pass over the point (r, o) in such a manner that its resultant displacement corresponds to the observed macroscopic displacement. If 6&apos; is measured from the [1010] direction, then for 0 < ? < ~/3, only the [1210] and 121101 type screw dislocations are needed to produce the required displacement. If n1 screws of type [1210] and n2 of type [2110] pass over a point, then, in order that Ur = 0 n, sin ? - n2 sin (/3 — 6&apos;) = 0. [2] If the tangential displacement is to be independent of 0, then n1 cos ? + n2cos (/3 —?) = N [3] where N is independent of ? and thus depends only on r. Nb is the tangential displacement where b is the Burgers vector. Since U? is a linear function of r, then N must be a linear function of r. If a2 is the outer radius and a, is the inner radius to which the plastic deformation has extended, then N = Nm2 r-a1 [4] This function meets the conditions that at

Jan 1, 1956

By Y. Wang, M. M. Singh, H. L. Hartman

Knowledge of the state of stress at the bottom of a drillhole is of practical importance in rock drilling, since the induced stresses must exceed the strength of the rock in order to cause fracture. This note reports on a numerical method to determine the stress distribution at the bottom of a borehole induced by a static bit load and overburden and fluid pressures. The procedure adopted is similar to that for the plane-strain, discrete model employed by Harper and Ang.1,2 The rock medium is considered to be homogeneous, isotropic, and elastic-perfectly-plastic. METHOD OF ANALYSIS AND PROGRAMMING The discrete model adopted consists of two types of points: mass points and stress points. The configuration and numbering notation are depicted in

Jan 1, 1967

By C. G. Dunn, M. Sharp

IN twinned crystals of the face-centered cubic metals the lattice of one twin is a mirror image of the other in a common twin boundary. When several twins appear within large grain in a sheet specimen, the twin one boundaries form a set of lines at the surface of the specimen which coincide with (111) planes of the large grain. Furthermore, for twins of the same orientation, these lines are parallel. Generally, the presence of identically oriented regions with straight parallel boundaries coinciding with a (111) plane of the surrounding crystal is strong evidence for identifying the island regions as twins of the parent crystal. However, Fig. 1, which shows the macrostructure of a large grain of copper with island regions that satisfy these conditions. is not an illustration of (111) twins. Since the reverse side of the specimen has much the same appearance, it was thought at first that these regions, which appear dark in the macrograph, actually were twins. According to X-ray data, however, these regions are second-order twins of the large crystal. With regard to their formation, these second-order twins formed by secondary recrystallization in a cube texture matrix. Growth occurred in the direction of the arrow (see Fig. 1) as the specimen moved slowly into a gradient temperature furnace as described previously.&apos; Nucleation of the second-order twins occurred, therefore, on the ends facing opposite the arrow. If the origin of the second-order twins were due to repeated twinning, some first-order twin structure should be visible on these ends. This proved to be the case, as very small twins were readily found with the aid of a microscope, and probably could have been seen, in some instances, under ideal lighting conditions without aid of a microscope. Fig. 2 shows a cross-section view taken perpendicular to both the surface and the (111) trace of the parent crystal (visible as a straight boundary in Fig. 1) at the beginning point of growth of a second-order twin and where one first-order twin was relatively thick. In the micrograph, A is the large parent grain; B is the first-order twin of A; and C, which is a first-order twin of B; is a second-order twin of A. Between A and B and between B and C the major straight portions are traces of common (111) twin boundaries. The straight portion of boundary between A and C, however, is not a common crystallographic plane to the two lattices; it is a (111) plane of A and a (115) plane of C. Without considering the mechanism of twinning itself, the origin of the second-order twins may be accounted for in terms of repeated twinning and special growth characteristics. After each nucleation, a selective growth process can be thought of as favoring growth of the first-order twin in local spots only and favoring growth of the second-order twin to an extent comparable with that of the parent grain over relatively large areas in a way similar to that described for twinning in aluminum.&apos; It has already been pointed out that the boundary between the large grain (A) and the second-order twin (C), which is responsible for the straight boundary portions in Fig. 1, involves a (111) plane of A and a (115) plane of C. The same combination of planes is not only possible in first-order twins, but actually appears quite frequently.3 Their prevalence in first-order twins and their presence here in second-order twins, together with the necessary occurrence of a large number of common lattice sites at the boundary, is an indication that this combination produces an "energy cusp"&apos; boundary. (Energy cusp boundaries have been described by Shockley and Read.") The configuration of atoms near a {Ill), (115) boundary in first-order twins is of course different from the configuration near the same type of boundary in second-order twins. References 1 M. Sharp and C. G. Dunn: Secondary Recrystallization Texture in Copper. Journal of Metals (January 1952) Trans. AIME, p. 42. 2W. G. Burgers and W. May: Stimulated Crystals and Twinning in Recrystallized Aluminum. Recueil des travaux chimiques des Pays-Bas (1945) 64, p. 5. aD. Whitwham, M. Mouflard, and P. Lacombe: Discussion of W. C. Ellis and R. G. Treuting, "Atomic Relationships in the Cubic Twinned State." Trans. AIME (1951) 191, p. 1070; Journal of Metals (October 1951). 4 W. Shockley and W. T. Read: Dislocation Models of Crystal Grain Boundaries. Physical Review (1950) 78, p. 275.

Jan 1, 1953

By E. Maxwell, C. J. Bechtoldt, H. C. Vacher

IN the course of an investigation of the properties of metals at low temperature there was occasion to determine the constitution of four iridium-osmium alloys. There is very little information in the literature1 on the constitution of synthetic Ir-0s alloys. Zvyagintzev&apos; s has made a comprehensive study of different natural Ir-0s alloys and concludes that alloys containing more than 32 pct 0s have the close-packed hexagonal structure of osmium, whereas those containing less than 32 pct 0s have the face-centered cubic structure of iridium. The alloys studied in this work were prepared by the American Platinum Works, Newark, N. J., and were received in the form of fragments approximately 1.5 mm average diameter. The fragments had been obtained by crushing ingots made by fusing charges of iridium and osmium under an arc and air cooling. The ingots were not given a homogenizing heat treatment. Sample fragments Table I. Results of X-Roy Diffraction and Microscopic Examinations Phases Present as Determined by X-ray Diffraction Osmium Alloy Close- Iridium Face- Packed Centered Osmium, Iridium, Hexagonal Cubic Mlcro- WtPot Wt Pct Structure Structure scope 0 99.9 None Present 1 23.6 76.4 None Present 1 38.7 61.3 Present Present 2 59.4 40.6 Present Present 2 79.0 21.0 Present Not detected 2 99.9 0 Present None 1 Note: Chemical analyses of the iridium, osmium, and alloys were furnished by the American Platinum Works. of the iridium and osmium used in making the alloys also were included. Several fragments of each metal and alloy were examined microscopically and by X-ray diffraction. For the X-ray method the fragments were crushed further to pass a 270-mesh screen, then sealed in evacuated fused-silica tubes, heated to 1100°C for 18 hr, and allowed to cool in the furnace. Powder X-ray diffraction patterns were obtained from the annealed fragments by means of a Norelco camera having a diameter of 114 mm, and unfiltered cobaIt radiation. For the microscopic examination several fragments in the as-received condition were mounted in Melmac, (American Cyanamid Co.) and ground using the conventional series of abrasive papers. The polishing was done with 0-2 diamond abrasive on a Microcloth (Buehler Ltd.) lap, wet with xylene. After polishing, the surface was etched electrolytically in a 10 pct solution of chromic acid or in a 10 pct solution of potassium cyanide. Both reagents attacked the osmium-rich constituent, whereas the iridium constituent was attacked slightly by the chromic acid reagent and not noticeably by the potassium cyanide reagent. The results of the X-ray diffraction and microscopic examinations are summarized in Table I. Fig. 1 shows the microstructure of a 21 pct Ir-79 pct 0s alloy. The results indicate an appreciable solid-solu-bility range of osmium in iridium as was reported by Zvyagintzev.&apos; The solid-solubility range of iridium in osmium is more restricted, apparently less than 21 pct Ir. This implies a large range of composition in which two phases can coexist that was not reported by Zvyagintzev.

Jan 1, 1955

By H. E. Stauss, E. I. Salkovitz, F. W. von Batchelder

EXISTING information regarding the structure of a spherulite in nodular cast iron is based on optical studies. According to these data, a nodule consists of an aggregate of graphite crystallites radiating from the center, with the closely packed basal planes at right angles to the radii. The c axes lie along the radii. This view faces some uncertainty in the fact that the c axis does not represent the accepted direction of fastest growth in graphite. To supplement the optical information, X-ray studies have now been made. The principle used was to screen the nodule in greater part from the X-ray beam and expose only a minor cap. As successively larger portions of the nodule were introduced into the X-ray beam, any differences in the X-ray patterns could be observed. Such photographs have been taken with chromium radiation and a Laue camera. The graphite nodule itself, about 0.010 to 0.025 in. in diam, was mounted with vaseline on a micrometer screw for control of the linear motion. The nodule rotated about 45" each time that it was translated linearly. The nodules were obtained from magnesium-treated hypereutectic iron by electrolytic solution of the iron in hydrochloric acid. In Fig. la is shown the pattern of the thinnest cap examined. In Fig. lb is shown the pattern of the same nodule moved 0.003 in. farther into the X-ray beam, and rotated 45" at the same time. Figs, la and lb indicate incomplete circles for graphite (the two outer circles arise from graphite) with the side arcs much weaker than the top and bottom ones. The arcs obtained are themselves not continuous in intensity but vary with maxima of intensity some 15" and 30" apart. The structure of the nodule that would give rise to such a pattern can be explained as follows. Basically the nodule consisted of small crystallites. The discontinuous character of the diffraction rings demonstrates that the nodule was not composed of randomly oriented crystallites. The strong vertical reflections and the weak lateral reflections show that the reflecting planes were roughly normal to the radii. The absence of sharp reflection spots suggests that the nodule did not contain large crystals. The sharpness of the diffraction rings in their radial direction shows that the variations in intensity along the arcs were not the result of line broadening resulting from extremely small crystals. In the diffraction patterns two rings corresponding to graphite were found. The third and inner ring in the figures originated in the vaseline. The graphite rings correspond to the a and ß lines reflected from the basal planes, showing that the radii of the nodules are the [0001] direction normal to the basal planes of graphite. The picture of the structure that is formed is, therefore, one of aggregates of crystallites. Within each aggregate the c axes of the crystallites tend to align themselves in the radial direction of the nodule, although these axes deviate somewhat in direction by a continuous variation of angle. Correspondingly the basal planes of the graphite crystallites are generally normal to the radii. It is a pleasure to acknowledge the assistance of M. C. Bloom and R. P. Dunphy of this laboratory.

Jan 1, 1952

By W. Rostoker, R. P. Elliott

TWO intermediate phases enter into equilibrium with the primary solid solutions of titanium.&apos; The TiMn2 phase was identified by Wallbaum2 as of the C14 type isomorphous with MgZn2. Contrary to Maykuth, et al.,¹ the phase occuring at about the 50-50 atomic proportion has been shown to derive from a peritectoid reaction.:&apos; A 30 day anneal at 900°C of an alloy containing 52 wt pct Mn developed sufficient of the new phase to give a clear and predominant diffraction pattern. The powder pattern was taken in a 14 cm diameter powder camera using filtered Cu Ka radiation. In all, 75 lines were recognized and measured. Interplanar spacing and observed intensities for the first 26 of these are given in Table I.

Jan 1, 1954

By John R. Weeks, Dan McLachlan, John R. Lewis

DURING the operation of the iron blast furnace, aggregates of hard, infusible, yellow, cubic crystals frequently form in the interstices of the lining and on the hearth of the furnace. These were first examined by Wohler&apos; and were identified by him as a complex cyanonitride of titanium, having a formula Ti(CN)2 • 3Ti3N2, or more simply Ti10C2N8. However, recent investigators have suggested that this complex compound does not exist. Recent work by Hume-Rothery, Raynor, and Little2 on the carbide and nitride particles in titanium steels suggests that a complete series of solid solutions of the general type Ti<0+y>C0Ny exists between titanium carbide (Tic) and titanium nitride (TiN). Assuming this to be true, it seems likely that Wohler&apos;s cyanonitride of titanium is in reality a solid solution of 20 mol pct Tic in 80 mol pct TiN, .the nearly consistent carbide-to-nitride ratio probably resulting from temperature and pressure conditions in the blast furnace. The object of the present work was to investigate thoroughly this possibility of a solid solution by using the single-crystal methods of X-ray analysis. A spectrographic qualitative analysis of a sample of the yellow crystals furnished by the Geneva Steel Co. sh&apos;owed, in addition to the titanium, strong lines of vanadium and moderate to weak lines of iron, magnesium, silicon, aluminum, and calcium. The last five were probably slag impurities, but the vanadium was possibly included in the yellow crystals, owing to a great structural similarity of its carbide (VC) and its nitride (VN) to the titanium compounds, Table 11. A chemical analysis was made

Jan 1, 1952

By S. Yamaguchi

IN this study of thorium and uranium minerals an x-ray shadow microscope of the Cosslett type1 was used. A flux of electrons driven with a voltage

Jan 1, 1959

By A. J. Griest, J. C. Danko

IN the course of vacuum evaporation experiments, sublimation figures were observed on the surface of a pure nickel specimen. A cubic figure, typical of those observed on this specimen, is illustrated

Jan 1, 1957