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By Charles S. Barrett

This paper is a progress report covering metallographic applications of the electron microscope that have been made during the past year at Carnegie Institute of Technology. An account is presented of the techniques that have been most satisfactory, the difficulties encountered, the resolution obtained, and the peculiarities that have been noted in the microstruc-tures. About 1200 exposures have been made during the year on the instrument, which is an RCA type B2 transmission microscope,' and a number of these have been selected to illustrate the results obtained. prints are also included showing the common types of falsities—to borrow a term from the biological field, the "artifacts." ln brief, the paper is a record of our attempt to determine the value of the electron microscope in the study of the structure of metals and alloys. In addition to comments on techniques and the quality of photomicrographs obtainable with them, the paper discusses the nature of the etch attack on a few metals, and the possible relation between the fine structure revealed by etching and the mosaic block structure of the grains, since numerous papers and reviews are available on the subject of imperfection in crystals, the comments here may be very brief; in fact, are restricted almost entirely to points having to do with recent theories relating the strength of metals to imperfections and to spacings of slip lines. Specimen Preparation and Photographs Mechanical polishing by hand was used throughout this work. Precautions that must be taken in microscopy at high magnification, which have been well explained by Vilella in his book on Metallographic Technique for Steel, are likewise important with the electron microscope. This applies particularly to the need for these polishing and etching (each successive polish becoming less severe and each etch lighter), since the fina1 etch should in general be no heavier than is used for oil-immersion optical microscopy and in many instances should be much lighter (compare Figs. 6a and 7a, 6d and 7b). An extremely light etch, of course, is incapable of cutting through a flowed layer of appreciable thickness. Unquestionably it would be very advantageous in each instance to compare the structures obtained by electrolytic polishing with those obtained by mechanical polishing, but difficulties with the electrolytic method have prevented this in the following collection of prints. The choice of etchant is important, of course; for example, picral proved superior to nital for tempered martensite. With the exception of Figs. Ib and 16, the replicas used were of silica, deposited upon polystyrene and floated from the polystyrene in ethyl bromide according to the method of Heidenreich and Peck.2 The samples were mounted in Bakelite, polished and etched, then the polished Bakelite

Jan 1, 1944

By Charles S. Barrett

This paper is a progress report covering metallographic applications of the electron microscope that have been made during the past year at Carnegie Institute of Technology. An account is presented of the techniques that have been most satisfactory, the difficulties encountered, the resolution obtained, and the peculiarities that have been noted in the microstruc-tures. About 1200 exposures have been made during the year on the instrument, which is an RCA type B2 transmission microscope,' and a number of these have been selected to illustrate the results obtained. prints are also included showing the common types of falsities—to borrow a term from the biological field, the "artifacts." ln brief, the paper is a record of our attempt to determine the value of the electron microscope in the study of the structure of metals and alloys. In addition to comments on techniques and the quality of photomicrographs obtainable with them, the paper discusses the nature of the etch attack on a few metals, and the possible relation between the fine structure revealed by etching and the mosaic block structure of the grains, since numerous papers and reviews are available on the subject of imperfection in crystals, the comments here may be very brief; in fact, are restricted almost entirely to points having to do with recent theories relating the strength of metals to imperfections and to spacings of slip lines. Specimen Preparation and Photographs Mechanical polishing by hand was used throughout this work. Precautions that must be taken in microscopy at high magnification, which have been well explained by Vilella in his book on Metallographic Technique for Steel, are likewise important with the electron microscope. This applies particularly to the need for these polishing and etching (each successive polish becoming less severe and each etch lighter), since the fina1 etch should in general be no heavier than is used for oil-immersion optical microscopy and in many instances should be much lighter (compare Figs. 6a and 7a, 6d and 7b). An extremely light etch, of course, is incapable of cutting through a flowed layer of appreciable thickness. Unquestionably it would be very advantageous in each instance to compare the structures obtained by electrolytic polishing with those obtained by mechanical polishing, but difficulties with the electrolytic method have prevented this in the following collection of prints. The choice of etchant is important, of course; for example, picral proved superior to nital for tempered martensite. With the exception of Figs. Ib and 16, the replicas used were of silica, deposited upon polystyrene and floated from the polystyrene in ethyl bromide according to the method of Heidenreich and Peck.2 The samples were mounted in Bakelite, polished and etched, then the polished Bakelite

Jan 1, 1944

By L. A. Willey, William L. Fink

TWO of the aluminum-alloy systems previously studied—the aluminum-titanium and the aluminum-chromium—exhibit a peritectic reaction at the extreme aluminum end of the diagram. Preliminary work indicated that the aluminum-zirconium and certain other aluminum systems were similar in this respect. The present paper, the twentieth of a series from the Aluminum Research Laboratories, reports the results of a recent investigation of equilibrium relations in aluminum-zirconium alloys of high purity, which confirm the preliminary observations. Previous Investigations There has been only one investigation of the aluminum end of the aluminum-zirconium system. Sykesl prepared and studied alloys containing 0 to 70 per cent Zr. The lowering of the freezing point of aluminum by the addition of zirconium was found to be very little, if any (less than 2" C.). He placed the solid solubility of zirconium in aluminum at room temperature between 0.57 and 0.97 per cent. A few other investigators have attempted to determine the composition of the intermetallic compounds occurring in this system. Honigschmid2 obtained the compound ZrAla as a by-product during the preparation of ZrSi2. He made no attempt to prepare other aluminum-zirconium compounds. Weiss and Newmann3 prepared an alloy by heating aluminum with a double fluoride of potassium and zirconium. When this alloy was treated consecutively with caustic soda and hydrochloric acid, there was a residue, which contained approximately 72 per cent Zr and 28 per cent A1 (Zr3AI4). Marden and Rich4 prepared an alloy in the same way, treated it with caustic soda, and obtained a residue of silver-white crystals, which contained 70 per cent Zr and 30 per cent A1 (Zr3A14). Alloys Materials Used.—Electrolytically refined aluminum was employed for thc preparation of all alloys used in this investigation. The chemical

Jan 1, 1939

By William L. Fink, L. A. Willey

TWO of the aluminum-alloy systems previously studied—the aluminum-titanium and the aluminum-chromium—exhibit a peritectic reaction at the extreme aluminum end of the diagram. Preliminary work indicated that the aluminum-zirconium and certain other aluminum systems were similar in this respect. The present paper, the twentieth of a series from the Aluminum Research Laboratories, reports the results of a recent investigation of equilibrium relations in aluminum-zirconium alloys of high purity, which confirm the preliminary observations. Previous Investigations There has been only one investigation of the aluminum end of the aluminum-zirconium system. Sykesl prepared and studied alloys containing 0 to 70 per cent Zr. The lowering of the freezing point of aluminum by the addition of zirconium was found to be very little, if any (less than 2" C.). He placed the solid solubility of zirconium in aluminum at room temperature between 0.57 and 0.97 per cent. A few other investigators have attempted to determine the composition of the intermetallic compounds occurring in this system. Honigschmid2 obtained the compound ZrAla as a by-product during the preparation of ZrSi2. He made no attempt to prepare other aluminum-zirconium compounds. Weiss and Newmann3 prepared an alloy by heating aluminum with a double fluoride of potassium and zirconium. When this alloy was treated consecutively with caustic soda and hydrochloric acid, there was a residue, which contained approximately 72 per cent Zr and 28 per cent A1 (Zr3AI4). Marden and Rich4 prepared an alloy in the same way, treated it with caustic soda, and obtained a residue of silver-white crystals, which contained 70 per cent Zr and 30 per cent A1 (Zr3A14). Alloys Materials Used.—Electrolytically refined aluminum was employed for thc preparation of all alloys used in this investigation. The chemical

Jan 1, 1939

By H. A. Schwartz

FROM time to time, one of the authors has had occasion to investigate the graphitizing reaction and has published the results mainly as discussion1 of the work of other investigators. In view, therefore, of the diversity of both observations and interpretation, it seemed well to attempt a revision of the entire subject in the Research Laboratory of the National Malleable Castings Co. The work consisted of a careful study of a single, impure, iron-carbon alloy. The material, which may be considered typical low-carbon white cast iron of the malleable industry, was an air-furnace iron of the following composition: carbon 2.30 per cent., silicon 1.20 per cent., manganese 0.29 per cent., phosphorus 0.156 per cent., sulfur 0.048 per cent. The freezing range extended from 1213° to 1132° C., the latter figure agreeing with Gontermann's data .2 We have attempted to define the equilibrium diagram of this alloy, in the stable condition as related to the metastable diagram, from a temperature somewhat below the eutectic freezing point to a temperature below Ar1 and for a graphitic-carbon content from practically nothing to the original total carbon of the specimen (see Fig. 6). More especially we desired to locate the line in the stable diagram corresponding to the Acm line of the metastable system, which is designated by analogy, the Atm line (tm from temper carbon) ; also to determine the location of Aim with respect to Acm toward their lower extremities at Ar1 in order to determine whether or not graphitization is completed by the separation of an iron-carbon eutectoid analagous to pearlite in the iron-cementite system. This would involve further a comparison of the locations of the stable and metastable A1 points.

Jan 8, 1922

By Francis A. Thomson

DO the curricula of our mineral technology schools prepare their graduates to meet properly the full range of their responsibilities in after life? An unequivocal "no" could be returned to this question, because training and experience in professional work are quite as important as adequate college preparation. Furthermore, a had curriculum with a splendid corps of men doing the teaching and a competent body of students doing the learning will produce a better result than an ideal curriculum in the hands of unqualified teachers and poorly prepared students.

Jan 1, 1937

By AIME AIME

ON May 5, the Washington, D. C., Section, A.I.M.E., devoted its meeting to the many-sided and perplexing question of mineral stock-piling for peace. Opening the symposium, Harry J. Wolf, of the War Production Board, outlined the problem under six heads: (1) Technical. Mechanical, chemical, or metallurgical importance of specified materials, emergencies that might arise, relative scarcity, and critical value of stock piles during emergencies. (2) Economic. Cost to Government, influence of Government stocks on commercial relationships and markets, effect of availability of items as a con¬structive influence on industry, Administration policies now and during postwar period. (3) Legislative. Need for immediate legislative action, need for legislation on postwar conditions as well as on current requirements, a constructive basic policy to prevent political manipulation. (4) Military. Consideration of re¬quirements and supplies bearing on national safety and needed for manufacture of equipment, and adequate reserves of scarce materials for research or experimentation by military agencies. (5) International. Interests of the United Nations in contradistinction to those of the United States; effects of nonisolation policy on nature, location, and administration of stock piles. (6) Negative stock-piling. Question of United Nations' legislation to prevent stock-piling by Axis nations after the war and who shall purchase stock-pile materials and during what periods.

Jan 1, 1943

By CHRIS A. HARTNAGEL

For the second consecutive year, the production of crude petroleum in New York has fallen below the 5,000,000-bbl. Mark that had prevailed previously since 1937. In 1945, the output totaled 4,658,000 bbl., a decrease of slightly more, than one per cent from the 1944 production. This total represents 2 per cent of the stripper-well production of the United States, which in turn is I 3 per cent of the total annual yield of the nation's petroleum.

Jan 1, 1946

By Frederick M. Becket

SHORTLY after the Armistice there appeared a few references to numerous attempts that had been made to produce steel without the aid of manganese, or at least with manganese in abnormally low percentage. Some years later, during two consecutive days of train travel, I had excellent opportunity to read Sir Robert Hadfield's book, entitled "Metallurgy-Its Influence on Modern Progress," and also his paper, "The Metal Manganese and Its Properties : Also the Production of Ferro-Manganese and Its History," presented at the spring meeting of the Iron and Steel Institute, 1927. Both the book and the paper are most interesting historically to makers of alloy steels and

Jan 1, 1931

By E. A. Anderson

THIS seems to be the year for superlatives in A.I.M.E. meetings. The programs of the various Divisions and Institute committees offered an abundance of interesting and valuable information in the form of technical papers, symposia. and lectures to large and interested audiences. The Institute of Metals Division may hold up its head with pride for its own program. With six technical sessions, three full-day symposia, and the annual I.M.D. dinner, four meeting days were not enough and many simultaneous sessions were required. The quantity and quality of the paper were equaled by the numbers and interest of those attending.

Jan 1, 1944

By N. L. ALISON

MUCH has been published on the general subject of metal mine ventilation but, so far as I can discover, few specific data on selection of fan equipment to meet the requirements of a given mine ventilation problem are available. This article is intended to point out some of the more important considerations which influence the selection of such equipment. It will be assumed that the mine operator is able to determine the quantity of air which is necessary in the various parts of his mine to produce the required results and the pressure in inches water gage needed to circulate this quantity of air through the mine. There may be instances in which this assumption is not justified, but the fact remains that, with proper engineering talent, these data can be approximated sufficiently close for practical purposes.

Jan 1, 1930

Sailing westward from the Society Islands in the fall of 1774, England's noted explorer Captain James Cook discovered New Caledonia-that long, linear island that has played such an important and varied role in the history of nickel. Upon his return to England the following year, Cook's announcement of this uncharted island generated governmental interest, but its distance from the Island Empire, the troubles in the colonies, and the difficulties with France combined to keep English interest indirect and in the background of the then-current events.

Jan 10, 1968

By MERLE HOWARD GUISE

WHEN I was a boy I walked into Fairbanks in 1905. I was but a soft chechako, and arrived with blisters covering my feet, as a result of "mushing" the 400-mile trail on foot. Because of them, the display windows of the trading posts were first to catch my eye-dog and horse collars, harness and sled parts! And because of my enthusiasm for things adventurous, I looked long upon the prospectors' gold pans, shovels, rifles, camp equipment, and what not. Today those windows are filled with motor car accessories, tires and repair parts; yes, even thermos bottles and vacuum cleaners! There were many chance meetings with little parties of prospectors in my youth, and it always set my blood to tingling. Sometimes it was a 70-year-old sun-baked son of the Arizona desert, wrangling his stubborn, faithful jenny away from some outfitting store, at others a shovel-ended poling b0at in northern Canada, \vith the partners and the dogs towing upstream along the bank, or an old sourdough, with tug-rope around neck and hand on the spruce sapling gee-pole, mushing along behind his two or three old, plodding malamutes, dragging a little Yukon sled piled high with rusty sheet-iron stove, pick and shovel, cross-cut saw and axe, rifle, bales of dog salmon, and other paraphernalia. These meetings envisioned the panning of old creek beds and draws in the search for as yet undiscovered pay-channels; they meant the toughest kind of work sinking a hole to bedrock in some far-away valley of promise; they suggested wood fires to thaw the frozen muck and gravel and crude windlass and hand-made tub to hoist the water and the mud; but loudest of all they spoke of Adventure.

Jan 1, 1929

By J. A. Putnam, A. D. K. Laird

In laboratory research on the behavior of oil, gas and water in porous materials, no direct method has been devised to measure saturation without disturbing the flow. Indirect methods involving various forms of radiation have been developed for measuring one or two components. The X-ray absorption method for two components has been described previously1-3. The possibility of three component measurement has also been mentioned1. Since two component measurement still requires considerable care to insure accuracy, the fact that three components can be measured satisfactorily is not generally appreciated. The fraction of the energy of an X-ray beam of one wavelength transmitted through a material is given by the transmission factor. in which 1 is the beam's path length through the fluid. p is the fluid density, and 1,. is its mass absorption coefficient. Eq. 1 implies that all parts of the beam pass through equal amounts of the fluid. Practical applications are, therefore, limited to systems in which the fluid is distributed so that I varies negligibly over the cross-section of the beam. Typical variations of the transmission factor with X-ray tube potential arc shown in Fig. 2 from which experimental points have been omitted for clarity. The X-ray absorption of low pressure gases in a core is practically zero so it cannot he distinguished from that a vacuum by instruments that will differentiate between liquids. The transmission factor of a gas in a core is. therefore, unity. Consequently, the saturation of only one gaseous component can be found. If two fluids completely fill a core, their two saturations add to unity and, therefore, only one value of the transmission factor, T, is needed to determine both of them. When two liquids do not completely fill the core, their saturations do not add to unity and transmission factors at two wavelengths must be measured. At one of these wavelengths, 7 for one liquid must be different from T or the other liquid. The change of T for one liquid us the wavelength is changed between the two values must be different from the corresponding change of T in the other liquid. The two values of fluid saturation will also give that of the gas because the three saturations must add to unity. In Fig. 2 it can be seen that there are many large differences of T between various oil solutions and water solutions at any one potential, and between potentials for any one solution. Consequently, conditions for optimum accuracy of measurement of the saturations of a gas and two liquids can be chosen. Once the operating potentials have been selected, however. it is more convenient to cross plot the data from Fig. 2 on transmission factor-solution concentration coordinates for the chosen potentials, as shown in Fig. 3. Fig. 3 was used to plan the experimental procedure for Core N-38-1. Since the voltage control at 45 kv was good, the slopes of the curves in Fig. 2 at this potential would cause little error. At low potentials, however, the voltage control was not good, so 33 kv was chosen because the small slopes of the curves made voltage control less critical. The lowest strength beam that could be measured reasonably at 33 kv corresponded to a minimum T factor of 0.385. Fig. 3 shows that both 4.80 weight per cent of cadmium chloride in water and 24.0 per cent of iodobenzene in crystal oil had this T value, and, consequently, were indistinguishable to the X-rays at 33 kv. Thus, at 33 kv, the liquid saturation was given by the same curve regardless of the relative amounts of oil and water solutions present. This simple calibration curve from which the gas and liquid saturation can be read, is shown in Fig. 4. Fig. 3 also shows that at 45 kv, T for the aqueous solution is 0.610. and that T for the oil solution is 0.220. These values were transferred to Fig. 4 to give the triangular calibration plot from which the brine and oil saturations can be found, after the gas saturation has been determined at 33 kv.

Jan 1, 1970

By E. J. Ripling

TUBES may be produced by a large number of forming processes, the most common of which will be discussed analytically in this paper. In no case will the stress analysis for any given tube producing process be derived formally for where such analyses are available, they may be referred to readily. Rather, emphasis will be placed on the interpretation of the theory of the different processes, few of which are developed to a state that will allow rigorous mathematical analyses, in an attempt to give a rational description of the effects of the different variables involved in each method. Tube producing methods can be divided into two groups: Those used to form shells, and those used to further work these shells into a shape more suitable for their final use. Among the first group are included roll piercing, extrusion and cupping for seamless shells, and bending with welding for welded tubes. The re-forming processes include sinking, drawing with a plug, and drawing with a rod. Only the plastic forming operations will be discussed here; other forming processes such as casting shells will not be considered. PRODUCTION OF SHELLS Shells for Seamless Tubing Piercing: The extremely important process of forming an axial hole in a billet by oblique rolling never has been analyzed satisfactorily, although a certain amount of experimental work relating to this process has been conducted. There are a number of factors that make piercing difficult to analyze; one of these is the fact that piercing is not a problem in plasticity, but one in fracturing, and the laws of fracturing are even less well understood than those of plasticity. If, however, it is assumed that fracturing occurs on a surface as a result of tensile stresses acting normal to this surface, piercing can be analyzed qualitatively by examining the stresses established in the oblique rolling process. To determine the origin of the tensile stresses that are thought to effect piercing, it will be necessary to know the angular relationships between the maximum stresses that are established in piercing. These angles quite frequently can be determined in a plastic deformation process by an examination of the deformed product. For example, consider the stresses established when a tensile test is conducted on a rectangular cross-sectional specimen of pearlitic steel. When stretched, this material first flows plastically, exhibiting the well-known yield jog on a stress-strain curve. The formation of the slip areas that give rise to the yield jog can be detected during the straining, since these flowed areas cause depressions on the specimen surfaces which can be seen if the surfaces are polished highly. The plastically strained areas also can be found after the specimen has been stretched to a strain not exceeding the yield jog, by sectioning the test piece and. etching these sections with Fry's etch. With this etchant, it is possible to dis-

Jan 1, 1951

Jan 1, 1968

By Franklin H. Sharp, Kenneth L. Clifford

During the last few years the New Lead Belt of Southeastern Missouri has become the main source of lead in the United States. It also produces significant amounts of zinc, copper and silver. The mines are located on a narrow, mineralized trend extending southward from Viburnum, MG. for about 35 miles. The ore occurs as replacement deposits in the Bonneterre lime- stone formation which is about 1000 ft below the surface. In most of the mines, enough water is produced to supply the milling requirements without any reuse. There are dry areas, however, and at least two mills must rely on water reclaimed from their tailings lake to augment the mine water. These mills have no choice but to utilize recycled mill water.

Jan 7, 1973

By C. H. Green

. RECENTLY two papers on the structure of eutectics were read before the British Institute of Metals, one by F. L. Brady1 and the other by A. Portevin.2 In the preparation of photomicrographs of laboratory specimens as illustrations for student work, and in connection with various researches; the writer has been working along the same line for some, time and, therefore, was much interested in the results given, especially those of Portevin. He has correlated the information on the subject and has outlined a broad scientific basis for future work along this line. It is largely with the idea-of adding something by way of illustration to the work already done that this paper is written. The eutectic is generally understood to mean the alloy having the lowest melting point of any alloy of the system, and in which the melt becomes supersaturated with reference to the two or more phases which, separate out simultaneously (or alternately). From the surface pattern, the eutectic means; a structure with no primary crystals. It is not always easy to get the exact eutectic composition in making any alloy; in fact, a slight range in composition may be expected and some of the coarser particles may be richer in either of the composing metals. Even when chemical analysis shows the right composition, differences in density of the pure metals may cause segregation, or. supercooling resulting from different crystallizing properties may give a surface pattern the appearance of being on one side of the eutectic point. However, the alloys on either side of the eutectic composition, showing primary crystals of one of the phases and the effect of the pro-eutectic form on the surface pattern of the eutectic make a very interesting study, which is slightly touched upon in this paper. The phases, or microconstituents, of a eutectic may be pure metals (Pb-Sb, Tl-Au), solid solutions (Cd-Zn), a pure metal and a solid solution; (Ag-Sn), or a pure metal or solid solution with an intermetallic compound (Sb-Mg, Sb-Cu, As-Cu, Bi-Te, etc.).

Jan 2, 1925