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By E. Eichen, G. S. Ansell. L. R. Sefton

A Technique for the Preparation of Thin Films of Two-Phase Alloys Suitable for Use in Transmission Electron Microscopy In order to obtain foil sufficiently thin to permit transmission electron microscopy of two-phase alloys, particularly alloys in which the second phase is present as a very finely dispersed second phase, a technique has been developed to permit the thinning of these materials without either the large degree of pitting present in the electrochemical or chemical thinning process or the slicing of the second phase particles accompanying the mi-crotoming process. The metal or alloy to be thinned is first ground to initial sheet thickness of approximately 0.002 in. by hand grinding on 4/0 emery paper. This starting sheet of material is then reduced in cross section by an air-abrasion technique using an S. S. White dental abrasive unit. This unit consists of a supply of compressed CO, which provides a stream of high velocity gas impinging on the metal surface. Incorporated in the machine is a hopper-type of device in which fine abrasive particles of alumina are introduced into this high velocity gas stream. The abrasive particles are irregular in shape, approximately 30 across. If any particles are introduced into the sample during thinning, they should be readily observable. Impingement of this gas abrasive mixture on the metal surface causes rapid removal of the metal in a rather uniform manner. The rates of metal removal may be adjusted by both regulating the gas pressure and amount of abrasive material introduced into the gas stream. By moving the gas stream abrasive mixture slowly about the specimen or sheet surface, a large area of the sheet may be uniformly reduced to a thickness which is then suitable for use in transmission electron microscopy. Attendant with this metal removal is a result in cold working of the metal surface due to the impingement of the abrasive particles. The resultant foils, therefore, if made from materials which are desirable to view in the annealed condition, have to be subsequently heat treated. If the alloy from which these foils have been made has been initially heavily worked or deformed during manufacture, then no subsequent heat treatment is, necessary as in the case of the SAP-type alloys. Following this initial abrasive thinning technique, the material is then given a final electropolish which is just sufficient to remove any oxide which has formed on the metal surface during the abrasion technique. Care has to be exercised in this technique to make sure that none of the attendant problems associated with the chemical or electrochemical removal process are encountered. An electrolyte solution which has been found suitable for aluminum-aluminum oxide SAP materials is one containing 78 ml of perchloric acid, 120 ml of distilled water, 700 ml of ethanol, and 100 ml of butylcellosolve. The current density used is 1 amp per sq cm and a polishing time of 3 sec on each side of the foil is used. Extreme care must be used in choosing the current density and time to ensure that just the oxide film on the specimen is removed. Times or current density which are greater than this will lead to perforation of the film due to the removal of the A1,0, particles or a complete loss of the film due to complete solution of the matrix. Once the oxide film is removed the specimens must be kept in alcohol until placed in the microscope to prevent any further oxidation. Fig. 1 shows -an electron micrograph at X28,000 of a thin foil of an aluminum-aluminum oxide SAP-type alloy prepared using this technique. The alloy consists of a matrix of commercial purity aluminum containing a very finely dispersed second phase of aluminum oxide flakes. In the electron micrograph, the dark patches are the aluminum oxide particles. The lighter portions of the micrograph are the aluminum matrix. Within the aluminum matrix, the dislocation structure of the alloy is clearly visible. This structure consists of intersecting twin boundaries and single dislocations. No abrasive particles were observed in the samples. In addition, thin films of commercial purity aluminum were prepared using this method and observed in the electron microscope. Here also, there was no evidence of abrasive particles introduced in the samples. The technique presented provides a satisfactory method for the production of thin films of aluminum-aluminum oxide SAP-type alloys for use in transmission electron microscopy where none of the usual thinning techniques appears to be satisfactory.

Jan 1, 1962

By John E. Latz

QUICKSAND far below the surface, stopped two attempts by the Potash Co. of America to sink a third shaft to a potash bed that lies 1000 ft below the southern New Mexico desert. Virtually all methods of grouting were employed in the two failures without any indication of consolidation of the flowing sand. Sinking the South Shaft at the Carlsbad potash mine seemed an almost insurmountable task, until freezing was employed as a final resort. This process that proved to be the answer may be defined as "the sinking of a shaft by freezing, consists of the formation, in the water-bearing strata, of a large block of frozen ground in which it is possible to sink a shaft without danger of an influx of water, providing the ice-wall between the water outside and the shaft itself is strong enough to resist the hydrostatic pressure." Freezing Method Used Extensively in Europe Successful frozen ground shaft sinking projects had been completed in Europe, and Russel G. Haworth, resident manager of the Potash Co. of America, went abroad in search of the know-how needed for the New Mexico undertaking. The freezing process, with a history of two failures at the time, was first successfully employed by Poetsch in 1885 at the Houssu Collieries near Haine St. Pierre, Belgium. Poetsch contracted to sink the remaining 64 ft of an uncompleted shaft through water laden strata from a depth of 190 ft to a depth of 254 ft. This work was in progress until 1887. The freezing and sinking consumed more than two years. As a result of early failures, the process was not favorably received until soon after the turn of the century. The accurate prediction of success in a given application was made possible by the concerted effort and study of a group of European engineers. Means of accurate deviation measurement and control were devised, the nature and properties of frozen water laden soil (the ice wall) were investigated, a thorough and rational basis of refrigeration load calculation developed, and concurrently the efficiency and dependability of refrigeration machinery was greatly advanced. Numerous shafts in Germany, Belgium, France, and England today testify to the reliability and economical surety of the freezing method. Applied to the South Shaft, which is circular in cross-section and 15-ft diam, the freezing method consisted of drilling holes 350-ft deep, through the water bearing strata into impervious ground-the freeze hole pattern being concentric with the shaft and 31-ft diam. The holes were cased with pipe closed on the bottom end. Smaller tubes were placed inside these casings and connected to a header supplying chilled brine from a refrigeration plant. The brine descended in the tubing to the bottom of the hole and ascended through the annular space between the two pipes to the top of the casing; flowed into the return header and back to the refrigeration plant. Under these conditions, each of the freeze hole casings became surrounded by a cylinder of ice

Jan 1, 1952

By Stanley J. LeFond, Langtry E. Lynd

Elemental titanium has become famous as a space age metal, because of its high strength/ weight ratio and resistance to corrosion. However, the major use is in the form of titanium dioxide pigment, which because of its whiteness, high refractive index, and resulting light-scattering ability, is unequaled for whitening paints, paper, rubber, plastics, and other materials. A relatively minor use is in welding rod coatings, in the form of the mineral, rutile. United States consumption of titanium dioxide for these applications in 1973 was as follows: pigments, 891,000 st; titanium metal, 40,000 st (=24,000 st metal) ; and welding rod coatings, 10,000 st. The only commercially important titanium ore minerals at the present time are ilmenite, and its alteration products, and rutile. Titanium was discovered by Gregor in 1790, as a white oxide which he recovered from menaccanite, a variety of ilmenite occurring as a black sand near Falmouth, Cornwall. Barksdale (1966) states that the fundamental chemical reactions on which the present day titanium industry is based were known before 1800, although it was not until 1918 that these pigments were available commercially on the American market. Pings (1972) outlines the early history of the titanium industry in the United States, referring to the work of Guise (1964) and others: "Mining of titanium minerals in the United States began sometime between 1880 and 1900, in Chester County, Pennsylvania. Small quantities of rutile were also produced during the time in North Carolina and Georgia. In 1901 rutile was mined from a deposit near Roseland, Va., and was used in making titanium chemicals and for coloring ceramics. Ilmenite in the deposit was produced as a separate item in 1913, and rutile and ilmenite were obtained from this deposit through 1921. The mining of titanium bearing beach sands began in 1916 near Mineral City and Pablo Beach, Fla., for the purpose of making titanium tetrachloride to be used in tracer bullets, flares, and smokescreens. The titanium pigment industry was founded in 1918. By 1928 a large part of the domestic production of rutile, ilmenite, and zircon came from Florida. However production ceased in 1929 in Florida with the mining of newly discovered deposits in Virginia which were mined until 1968. The discovery of new deposits in Florida, and the development of better mining and concentrating methods for lowgrade sands, led to a return of activities in this area. The large deposits near Tahawus, N.Y., were brought into production in 1942 by National Lead Co. (now N L Industries Inc.), and by 1949 this company was the lead¬ing producer of ilmenite in the world. In 1948 the extensive deposits of ilmenite and ilmenite-bearing iron ores were discovered in eastern Quebec." The beginning of the modern titanium metal industry was in 1948, when E. I. du Pont de Nemours & Co. produced the first metal. U.S. Bureau of Mines reports, which gave details of the Kroll process, together with the attractive properties of the metal for

Jan 1, 1975

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Jan 1, 1913

By Robert Job

Up to five years ago the pig-iron used by the Philadelphia & Reading Railway Co. had been obtained solely upon the appearance of the fracture; but as the service was unsatisfactory, an investigation was made to determine the quality best adapted

Jan 1, 1905

Jan 1, 1913

The technique of hard facing can be a quick and economical means of prolonging wear-life of many metals, but maintenance personnel must first select the proper alloy from the hundred that are available. Even then, roper selection is effective only when it is properly applied by the welder. To complete the successful weld, several hints are offered:

Jan 4, 1978

CLARENCE N. FENNER.-Mr. Gelstharp, chief chemist of the Pitts-burgh Plate Glass Co., has directed my attention to the fact that that company was using optical pyrometers obtained from the Leeds & Northrup Co. several months before the members of the Geophysical Laboratory arrived at Charleroi. I am glad to make this correction. The chief object of my paper was to emphasize the necessity of careful temperature control in the making of optical glass and to describe the kind of tests to which an optical pyrometer should be subjected at a glass plant in order to obtain information regarding the closeness with which its readings correspond with true temperatures under the condi-tions which prevail in each particular case.

Jan 12, 1919

By Robert W. Hunt

No matter how perfectly sectioned or skilfully manufactured the rails used may have been, or with what care the road-bed may he maintained, legitimate results from these important factors cannot be secured unless proper attention is bestowed upon the joint-fastenings. In this country, splice-bars of various patterns furnish the practically universal joint. Other forms have been used, and are now being experimentally tested, but the typical American rail-joint consists of angle-plates or splice-bars. At the same time, it is true that scarcely a railroad engineer is satisfied with his joint. He may consider it the best of which he has knowledge, but at the same time he is well aware of many of its weak points.

Jan 1, 1890

By C. D. Jardine, D. G. Patton

Rapidly increasing energy costs and more rigid customer quality requirements necessitate improved control of pelletizing processes. With the introduction of dedicated microprocessor-based controllers, sophisticated control strategies are now possible. An application of this technology at Carol Project has resulted in fuel savings, improved pellet quality, and standardization of operating procedures. This was accomplished with no production loss by using a "building block" approach to design and equipment selection.

Jan 1, 1985

[ARTICLE I. NAME AND OBJECT Section 1. This Society shall be known as the Society of Petroleum Engineers of the American Institute of Mining, Metallurgical, and Petroleum Engineers, Inc. Section 2. The object of the Society of Petroleum Engineers shall be to furnish a medium of cooperation among those interested in the petroleum-natural gas industry an to promote the advancement of this branch of mineral technology through meetings to stimulate the preparation, reading, discussion and circulation of papers connected therewith. ARTICLE II. MEMBERS Section 1. Any person who is a member of AIME may become a member of this Society by the specified process. Section 2. Local organizations may be formed by the Society of Petroleum Engineers as subsidiary units, the membership of which shall be subject to and in accordance with the by-laws of the Institute.]

Jan 1, 1961

Here are the details . . . . . of how a $2.5 million research gamble, now backed by five years of intensive development in cooperation with the Chemical Construction Corp. resulted in a hydrometollurgical process that yields pure metal powders from sulphide concentrate - a process that offers potential savings of $2.5 million a year.

Jan 6, 1953

By H. F. Walther

Basic electric-are furnace steel production mainly involves the use of two separate types of slags. The first, known as the "melt down" or oxidizing slag, which is in most cases removed from the furnace mechanically, and the heat finished under the second or deoxidizing slag, which is commonly known as the "finishing slag.'' The melt down slag is formed by the addition of lime or limestone to the charge, which combines with the oxides formed during the melting period and the product of any bottom erosion that may take place.

Jan 1, 1935

By H. F. Walther

Basic electric-are furnace steel production mainly involves the use of two separate types of slags. The first, known as the "melt down" or oxidizing slag, which is in most cases removed from the furnace mechanically, and the heat finished under the second or deoxidizing slag, which is commonly known as the "finishing slag.'' The melt down slag is formed by the addition of lime or limestone to the charge, which combines with the oxides formed during the melting period and the product of any bottom erosion that may take place.

Jan 1, 1935

Jan 1, 1957