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By W. B. Triplett, H. I. Aaronson, G. M. Andes

THE morphology and mechanism of the proeutectoid a and the eutectoid reactions have been recently investigated in some detail in an iodide-base Ti—7.22 pct Cr alloy.' These studies have now been extended to an iodide-base Ti—10.8 pct Cr alloy in order to evaluate the effects of composition on the proeutectoid and eutectoid transformations in titanium-chromium alloys. The alloy used in this investigation had the following composition: 10.8 Cr, 0.0327 0, 0.011 N, 0.0063 H, and 0.011 pct C. Specimens of this alloy were heat treated in evacuated and internally get-tered Vycor capsules. The specimens were solu-

Jan 1, 1959

By Thunaes, Arvid

Pilot plant test work in 1942 and 1943 showed that by a combination of desliming, fine-size classification, and Sullivan deck concentration it is possible to recover heavy minerals such as cassiterite at least as fine as 10 microns in size. This appreciable improvement in gravity concentration practice has been substantiated by several full-sized plants.

Jan 1, 1950

Planning for a surface coal mine includes selecting the best means and equipment for uncovering the coal, loading it, and transporting it to the preparation plant. The machines and methods that will ensure optimum production will depend upon the location and characteristics of the seam to be mined. Stripping Techniques The choice of stripping units is influenced primarily by the system of mining, such as contour or out-crop mining as contrasted to mining in a region of rolling terrain with relatively flat upland surfaces. Factors such as the life of the mining operations production requirements, types of overburden, local and regional dip of coal, and land reclamation are other important considerations.

Jan 10, 1967

By FREDERICK LAISY

A NUMBER of new plants for the treatment of copper ores were completed or under construction during the year. Among these may be mentioned the plants of the International Nickel Co., those of the Hudson Bay Mining and Smelting Co. and of the Roan Antelope Copper Co. Three copper re- fineries have been constructed, one at El Paso, Tex., and the other two in Canada. Two more are projected, one in France and one in England. The International Nickel Co.'s plant consists of an 8000-ton concentrator and a smelting plant containing thirty 10-hearth Herreshoff roasting furnaces, five reverberatory furnaces, and eight Smith-Pierce converter5 . The smelting plant is estimated to have a capacity of 5000 tons of ore or concentrate per day. The roasters are superimposed on the reverbratory furnace plant. As a consequence of this arrangement, the furnace building is unusually high. being 183 ft. from yard level to highest roof elevation.

Jan 1, 1931

By James F. McConnell, Charles W. Statler

Pennsylvania's existing large coal-fired units are limited to 2.0, 1.8, or 0.6 lb of sulfur per million Btu fired, depending on site location. Multi-stream coal preparation can be employed on system basis to extract the highest quality fraction of coal for use in units requiring the lowest sulfur. The middling fraction can be directed to units permitted higher sulfur. General Public Utilities Corp. has concluded that it is feasible to advance the state-of-the-art of heavy media coal preparation to produce an intensively cleaned primary product of 1.3 sp gr of less than 0.6 lb of sulfur per million Btu for the new unit and a middling product of 2.0 lb of sulfur per million Btu for existing units.

Jan 1, 1977

The primary purpose of the Institute is to advance the technologic and engineering arts embraced by it through interchange of knowledge. This can best be done by the presentation and discussion of technical papers by its members. Short practical papers are especially welcome. An author should always satisfy himself that his material is of a quality that will be a credit to him and to the Institute. The preparation of a good paper frequently leads to a reorientation of the author's thoughts, and publication contributes much to the professional standing of the author. Members are urged to submit papers presenting the results of their work. Attention to the following suggestions will greatly further the prompt and efficient handling of manuscripts.

Jan 1, 1944

By J. C. Scully

In June, 1965, Sanderson and scully5 reported at the Conference on Environment Sensitive Mechanical Properties of Materials at the Research Institute for Advanced Studies at Baltimore that thin foils of titanium could be prepared by chemical polishing in a mixture of 44 pct HF and 73 pct HNO3 in the volumetric ratio 2:3. The technique is simpler than that since reported by Rice and Orava. As-received annealed titanium (containing 0.8 pct Fe and 30 ppm H) in the form of sheet 0.05 cm thick is placed in the solution and moved up and down. The reaction is violent but suitable foils are obtained very easily and consistently. A typical micrograph is shown in Fig. 3. The small precipitates were not identified. Yamane and ueda6 observed many spotlike features which they referred to as small dislocation loops. While their spots may be due to the reaction of the warm foil with the air as suggested by Rice and Orava, the precipitates in Fig. 3 are also found when foils of titanium are prepared by electro-polishing at low temperatures and subsequently examined in the electron microscope without any inter- mediate warming. Furthermore, they are not a surface effect. It is necessary to add that alloys of titanium cannot be so easily thinned by the chemical polishing solution described above since it contaminates the a, phase with hydrogen and produces y hydride. These matters are described at length in a paper7 and their relevance to stress corrosion is considered elsewhere.'-* Author's Reply The authors are grateful to Dr. Scully for bringing to our attention his hitherto unpublished technique for thinning unalloyed titanium, and deeply regret the unintended apparent duplication. The chemical thinning solution (7 parts HNO3 and 3 parts HF, by volume) reported by us is the same as that with which, for some period in the past, we had experienced success in the preparation of foils from single and polycrystalline niobium. Its subsequent effective application to titanium was a logical step, which, clearly independently of Scully, was conceived by Mr. Rice, to whom full credit is due. A few comments are warranted concerning some of the details of the preceding Discussion. It is evident to the discerning reader that the two thinning techniques under consideration are chemically almost identical, and in that sense are equally "simple". The chemical aspect is, of course, the one of primary importance in both communications. Thereafter, the relative simplicity is dictated by the mechanics of the actual thinning operation selected by the individual investigator. Our standard dimpling, or dishing, procedure was chosen with a view toward providing, for the electron transparent areas of the sample, the maximum protection from extraneous deformation during handling. That the long, straight dislocations visible in Scully's electron micrograph of a seemingly recovered structure closely resemble handling dislocations would tend to indicate the merit of our adopted technique. Features similar to those which Scully has attributed to precipitates, without any apparent diffraction contrast confirmation, were not observed in any of our clean foils taken from annealed or deformed specimens. This was admittedly somewhat surprising since the 3700 ppm (nominal) Fe in the A-70 commercial-grade titanium examined should have given rise to TiFe precipitates. Presumably these existed but were un-resolvable. Curiously, Scully's "precipitate1' density is fairly high although the iron content quoted was less than one-fourth of that in our material. One is forced to conclude from the evidence that prior thermal and mechanical treatments are responsible for the two different types of structure observed.

Jan 1, 1968

Jan 1, 1888

By C. W. Parmalee

The ideal fuel for burning ceramic wares is the one that, among other characteristics, has little or no sulfur. For that reason wood was long considered the most desirable fuel but its high cost has practically eliminated its use except in regions where it is very abundant or other circumstances warrant its choice. The fuels commonly employed are natural and producer gas, oil, and coal. The last named is undoubtedly the most important, not only in this country but abroad. Occasionally anthracite is used but the larger part is bituminous. The quality of the coal used depends on the kind and the value of the products being manufactured. For some materials, such as common brick, hollow block, etc., the quality of the coal is of less importance than in the manufacture of polychrome terra cotta, pottery, porcelain, etc. It is obvious that in burning clays that contain notable amounts of pyrite, marcasite or gypsum, as is the case with many common clays, the sulfur content of the fuel is of much less importance. The permissible amount of sulfur in the coal used will depend on the kind of product being manufactured. "A good sample1 of coal commonly used in pottery ovens has something like this quantity of sulfur: total sulfur, 1.20 per cent.; sulfur in ash, 0.11 per cent.; volatile sulfur, 1.09 per cent." This is based on English pottery practice. Correspondence with a. number of leading manufacturers in this country has produced the following figures: Sanitary Ware.—(a) 1.0 per cent, maximum, (b) 0.5 per cent. Sewer Pipe.—(a) 1.2 per cent., (b) 1.1 per cent, present run, 3.0 per cent, has been used. Terra Cotta.—(a) 0.5 per cent, basis of contract, 1.0 per cent, approximate. Pottery.—1.0 per cent, contract, 1.5 per cent, probable content. Enameled Brick.—1.3 per cent, maximum, (a) and (6) designate different firms giving figures. Since a pottery kiln for sanitary ware will require about 14 tons of coal for a bum, the quantity of SO2 that will be generated from a 1-per

Jan 1, 1920

By Myron Read

DURING the past 25 years, mining engineers have seen the development of a multitude of specialized engineering curricula in the mineral industry field. Bachelor degrees are now !ranted in the fields of mineral dressing petroleum engineering, geological engineering, fuel technology, and many others. These fields were all, previously considered to be part of a mining enginieer's work and elementary phases of them were included in mining engineering curricula. Their emergence has left some mining engineers with the fear that nothing will he left for a purely mining engineer to teach, or that mining engineering graduates will be unable to complete in any of these fields with the more specialized students and thus will have neatly restricted employment opportunies. A secondary reaction has been that if students who began to say that the pining engineering curriculum taught everything but mining, since so many of :he subjects that had always been udedAuded in the mining engineering curriculum now were fields in their own right.

Jan 1, 1946

By M. J. Blackburn

The ordering reaction and its effect on dislocation awangements in alloys based on Mg3Cd has been studied by transmission electron microscopy. Ordering occurs by the growth of ordered domains until they impinge, thus producing an antiphase domain boundary (APB) network. In the disordered alloy, slip is confined to the basal plane while in the ordered condition slip occurs on the basal, prism, and pyramidal planes. Superdislocations have been identuied on these planes and their origin and expected spacings are discussed and compared with the observations. The APBs between the dislocation pairs have been resolved and have proved useful in the identification of superdislocations. Observed slip structures are related to the changes in mechanical properties produced by ordering. At high temperatures magnesium and cadmium form a continuous series of disordered hexagonal solid solutions. At lower temperatures three ordering reactions occur; two based on the compositions Mg3Cd and MgCd3 are transformations to DO19-type superlattices while alloys based on the composition MgCd transform to a B19 lattice. The ordering process in alloys near the composition Mg3Cd has been studied by several workers'-4 and it has been shown to be a first-order type transformation. The variation of mechanical properties with the degree of order and temperature have been reported in some detail by Stoloff and Davies.5 It was shown that the disordered alloy was stronger and less ductile than the ordered alloy, the differences being attributed to changes in the number of active slip planes and to the presence of short-range order in the disordered alloy. In this investigation the ordering reaction has been qualitatively followed by transmission electron microscopy. The effect of this ordering transformation on the dislocation arrangements in deformed specimens has been studied in some detail. EXPERIMENTAL Alloys were melted in a stainless-steel crucible under a flux and chill cast; both melting and casting were performed in an argon atmosphere. The ingots were hot-rolled and tensile specimens cut from the resultant strips. Some large-grained specimens were grown by the strain-anneal method. Heat treatment was carried out in inert atmosphere furnaces and in oil baths at the lower temperatures. Thin foils for transmission electron microscopy were produced by electropolishing in a cooled solution (temp = -40°C) containing 50 cu cm of nitric acid and 180 cu cm of methanol at a potential of 10 v. The ordering reaction was followed by transmission electron microscopy, X-ray, and electrical resistivity measurements but this paper will be concerned chiefly with the electron-microscopy results. Much of the work described in this paper was performed on an alloy containing 26.10 at. pct Cd although two of the micrographs are taken from work on a 25.55 at. pct Cd alloy. RESULTS i) The Quenched Solid Solution. Specimens which were quenched from above the critical temperature showed diffuse superlattice reflections. sark-field analysis on these reflections failed to reveal the presence of ordered domains and thus the superlattice reflections were assumed to arise from regions of short-range order. Quenching from temperatures of 400" to 450°C results in the formation of dislocation loops and helical dislocations. Such defects have been observed and analyzed in detail in several hexagonal metals6-' and as the crystallography and interactions of such loops appear similar in this alloy they will not be reported in detail. Fig. 1 shows a high density of loops

Jan 1, 1968

By M. Cohen, D. J. Blickwede

Quantitative observations concerning the carbide phases in high speed steel are of importance for two general reasons: (1) the carbides, being inevitable constituents of the final structure, exert a direct influence on the properties of the steel; and (2) a substantial proportion of the total alloy content is tied-up in the carbides, and hence the extent of their solution on austenitizing governs the composition of the steel matrix. The latter relationship has a vital bearing on the response of the steel to tempering as well as on its performance in subsequent service. Accordingly, in the course of a long-term study of the behavior of high speed steels, the authors were confronted with the problem of securing quantitative data on the carbide phases. The obvious method for acquiring such information is to isolate the car-bides from the steel and subject them to chemical, X ray diffraction and other measurements. There are well-known extraction techniques which involve the chemical or electrolytic solution of the less noble matrix (ferrite, marten-site or austenite), thus leaving a residue of the carbide phases. However, the results obtained must be scrutinized carefully1,2 since the carbides may be affected by the chemical or electrolytic action. It is the purpose of the present paper to describe the experiments leading to an electrolytic-extraction technique for quantitatively isolating the carbides from both I and hardened high speed steel. Particular attention is paid to the amount, as well as the composition, of the carbides so that the matrix analysis becomes ascertainable by subtraction from the overall steel composition. Illustrative results are given for the M-2 grade of tungsten-molybdenum steel. Review of the Literature The chemical method of dissolving the matrix selectively with respect to the carbides makes use of dilute non- oxidizing reagents such as hydrochloric or sulphuric acid. Although this simple procedure has led to the determination of the cementite composition,3,4 it achieved only limited success because of the interaction between the acid and the carbide residue. Some of the carbides may not only be destroyed in this way, but the hydrogen released is likely to remove part of their carbon as hydrocarbon gases. The electrolytic technique of isolating carbides has the advantage of rapidly dissolving the specimen (anode) in the presence of less reactive solutions than are practicable with the chemical method. This reduces the possibility of chemical attack on the carbides, and furthermore, the hydrogen evolved during the electrolysis is released at the cathode which is not in close proximity to the carbides. The common electrolytes adopted for this purpose are hydrochloric and sulphuric acids.5-l1 Aqueous solutions of ferrous salts have also been used.12,13 A considerable advance in experimental technique was introduced by Treje and Benedicks14 who developed a double-compartment cell for electrolytic extraction, the anode and cathode chambers being separated by a porous diaphragm. A solution of 15 pct sodium citrate, 2 pct potassium bromide and 1 pct potassium iodide was selected for the anolyte, while the catholyte consisted of a 10 pct solution of copper sulphate, with copper serving as the cathode. This type of cell has a number of desirable characteristics: 1. The anolyte has a pH value close to 7, at least at the beginning of the run. 2. The iron that dissolves from the anode-specimen forms a water-soluble complex ion with the citrate, thereby preventing the precipitation of iron hydroxide (which would contaminate the carbide residue) despite the neutrality of the solution. 3. Copper deposition instead of hydrogen evolution occurs at the cathode, and this avoids an increasing concentration of hy-droxyl ions which (in an otherwise neutral solution) might cause the precipitation of insoluble hydroxides. 4. Contamination of the anode chamber by copper sulphate is inhibited by the porous diaphragm. Houdremont and coworkers15 applied the above method (with the further refinement of excluding oxygen during the electrolysis, washing and drying) to the extraction of carbides from a series of plain carbon steels after various heat treatments. They had quantitative success only with specimens in the annealed condition, and concluded that the size and shape of the carbide particles play an important role in the isolation process, with large spheroids exhibiting the least tendency to decompose during the electrolysis. Up to the present time, the citrate double-cell has not been used to any extent for isolating the carbides of high alloy steels, apparently on the grounds that the complex carbides are more resistant than cementite to attack in the simpler acid electrolytes. In particular, Bain and Grossmann7 and Gulyaev10.10a have employed the hydrochloric acid cell for their investigations of the carbides in high speed steel.* It will be demonstrated here that this type of cell is capable of yielding quantitative results in the case of high speed steel, and actually has certain advantages over the more complicated double cell. However, in order to provide a rigorous test of the quanti-tativeness of electrolytic procedures for the problem at hand, both methods were studied in considerable detail.

Jan 1, 1950

By Harold Markus, Gerhard Derge

THE first paper1 of this series described a technique of careful surface preparation by means of which reproducible results may be obtained from potential measurements of the behavior of tin in carbonate solutions with a pH range from 8.4 to 11.2. It then went on to establish the behavior of pure tin electrodes under these conditions and showed that the metal remains active at all times, though the steady potential attained after several hours decreases from I.I2[t] volts at a pH of 12.6 to 0.6 volts at a pH of 8.4. This behavior may serve as a norm with which all other data can be compared. In the second paper,2 small amounts of other anions were added to the carbonate solutions and the conclusion was reached that the common impurities encountered in alkaline materials packaged in tin do not increase corrosion. In fact, in some cases these anions may actually promote the formation of protective films. The present paper rounds out this survey by presenting data on the influence of cations added to the carbonate solutions, as well as the effect of alloy additions to the tin. In many cases the potential data are supplemented with weight-loss measurements. Information is also presented on the effects of some additional anions, the influence of gases above the electrolyte, the behavior of high-purity tin, and the effect of atmospheric oxidation on the corrosion resistance of the above-named alloys. Analysis of the entire body of data discloses some general rules applicable to corrosion in carbonate solutions. The experimental methods used are the same as those previously described. EXPERIMENTAL DATA Cations.-The carbonates of the cations K+, Li+, NH4+, which are soluble, were studied in the same way as the anions, by adding 0.01 mol of the metal carbonate to one liter of 0.2 M sodium carbonate solution, pH 11.2, or to 0.1 M sodium bicarbonate, pH 8.4. The other metallic carbonates are only slightly soluble, of the order of 0 7-3 mols per liter or less, and the sodium carbonate solutions were saturated by adding excess reagent several days before the experiment, shaking frequently, and filtering just before use. The chemicals were c.p. grade in each case except the indium salt. This salt was prepared by solution of the metal in hydrochloric acid and precipitation by addition of Na2CO3. These cations may be divided into two classes, according to their effect on the potential behavior of the tin: (I) normal, (2) passive. To offer a basis of comparison, curves I of Figs. I and 2 are given to illustrate the behavior of tin in carbonate solutions saturated with CaCO3. These curves are the

Jan 1, 1941

By P. S. Kotval, H. Hahell

PRECIPITATION of M23C6 carbides at grain boundaries in austenitic steels and nickel base superalloys has received considerable attention. Hatwell and Berghezan,1 in a study using carbon extraction replicas, observed that dendritic growth of the M23C6 carbide phase occurred at grain boundaries in austenitic steels. Merrick and Nicholson2 have observed that in thin foils of "Nimonic 75" alloy the precipitation of M23C6 carbide was discontinuous at grain boundaries. Lewis and Hattersley3 have suggested that the type of M23C6 precipitation observed in Ni-Cr austenites represented the early stages of discontinuous precipitation. In a more recent study, Singhal and Martin4 have concluded that grain boundary M23C6 precipitation involves the migration of an austenite grain boundary by a mechanism very similar to that proposed by Tu and Turnbull.5 Tu and Turnbull's suggestion essentially involves grain boundary migration under the driving force arising from the difference between the surface free energies of the opposite sides of the plate. Thus, Singhal and Martin's observation4 implies that the first stage of discontinuous precipitation has taken place and that the grain boundary has provided a diffusion short circuit for the sub-stitutional solute atoms (principally chromium) which assist the preferential growth of the M23C6 plate in contact with the grain boundary. However, no evidence of the characteristic cellular morphology typical of discontinuous precipitation was found in Singhal and Martin's studies. Presumably, this is due to the low volume fraction (i.e., low supersaturation of solute) of the precipitating carbide reported by Singhal and Martin.4 Recently, Raymond6 has studied precipitation of the M23C6 carbide in Incoloy alloy 825 and shown that the growth of this phase is perpendicular to grain boundaries at 1400°F and in the plane of the grain boundary at 1700°F. The former aging condition resulting in discontinuous or "cellular" precipitation. Raymond has suggested an explanation for this behavior based on the relative rates of chromium diffusion by volume and grain boundary diffusion at the two different aging temperatures. In the course of a recent investigation on precipitation behavior in several ' strengthened superalloys, precipitation of M23C6 carbide at grain boundaries was studied. Under conditions of a high degree of supersaturation, the M23C6 carbide precipitates in the discontinuous or cellular morphology in Waspalloy (Ni-18.51 Cr-2.0 Fe-3.53 Mo-1.16 Al-2.78 Ti-0.09 C). This note presents electron microscopy observations of this mode of precipitation and its effect on mechanical properties. Specimens of Waspalloy after "solution" heat treatment at 1950°F show essentially single phase matrix with a few residual particles of "primary" MC carbide. In normal commercial heat treatments, precipitation of Ni3(Al,Ti) ordered fcc r' phase occurs throughout the matrix and M23C6 precipitates as globular particles at the grain boundaries. In these commercial heat treatments the degree of supersaturation during precipitation is low. However, if specimens of Waspalloy are quenched from the solution heat treatment temperature of 1950°F and then aged at an aging temperature where the degree of supersaturation is high, discontinuous precipitation of M23C6 occurs. Figs. 1 and 2 show thin foil micrographs of Waspalloy, solution heat treated at 1950°F, water quenched, and aged at 1292° and 1598°F, respectively, for 500 Fig. 1—Thin foil of Waspalloy, solution heat treated at 1950°F for 1 hr, water quenched, and aged for 500 hr at 1292°F. Magnification 15,500 times. Fig. 2—Thin foil of Waspalloy, solution heat treated at 1950°F for 1 hr, water quenched, and aged for 114 hr at 1598° F. Magnification 13,000 times.

Jan 1, 1970

PUGET SOUND SECTION SIMON H. ASH, Chairman, I. F. LAUCKS, Vice Chairman, CHARLES SIMENSTAD, Sec.-Treas., 425 Lyon Building, Seattle, Wash. GLENVILLE A. COLLINS, JOHN N. POTT. The Puget Sound Section met at the Arctic Club, Seattle, Wash., on Jan. 20, 1917. Sixteen members and five guests were present. Dinner having been served, the meeting was called to order. A letter from secretary of Associated Engineering Societies was read, requesting payment of this section's assessment to the quarterly budget, and upon motion it was voted that the Secretary-Treasurer be instructed to pay this assessment. It was moved and carried that this section join with the Chemical Society in a meeting. At the, close of the business meeting, Mr. Asa C. Baldwin gave an illustrated lecture on the "Alaska Boundary Survey." On Feb. 24, the Puget Sound Section again held a meeting at the Arctic Club, 16 members and three guests being present. Chester F. Lee, as member of a committee representing this section in the joint council of the Associated Engineering Societies, reported that by lots it had been decided that the term of service of said committee would be as follows: Chester F. Lee, two years; George. Watkin Evans, one year. Following adjournment of the business meeting, Prof. Joseph Daniels, of the University of Washington, delivered a very interesting lecture on "Milling Practice of The Alaska-Castineau Mining Company." CHAS. SIMENSTAD, Secretary.

Jan 5, 1917

By James R. Finlay

SOMETIMES the American Institute of Mining and Metallurgical Engineers appears to be a strictly technical society, and if so my paper should deal with the technical operations of finding and producing gold. But I have not been engaged in practical gold mining since 1910. What I have been doing mainly for the last 25 years is to try to figure out what the income of a mine-gold, or any other-would be worth to an investor. So I have been in contact with gold mining, in one way or another, for some 42 years. I say that with a purpose. In that time the industry has been through one of its cycles. The value of gold mines is very dif¬ferent at different points in one of these cycles. For this reason the cycle of gold mining is a highly practical study. The cycle of gold is a more or less rhythmical change in its value or purchasing power measured in the grand average of other commodities, which is the same thing as its price. Taking the price of gold in 1897 as a stand¬ard, a dollar at that time declined to 55c. in 1913, to 26.8c. in 1920, and since then it has risen to 47.4c. in 1930 and to about 64c. in 1932. It is worth about 21/ times as much now as it was in 1920, but less than two¬thirds as much as in 1897. When this change is applied to the value of a gold mine still greater differences are evident. The cost of producing gold is of course measured in labor and other commodities, and as that cost goes down the margin of profit measured in the gold itself increases. Thus a mine which might make only 10 per cent profit in 1920 on its gross output may easily make 25 per cent now. The stockholder gets 2 ½ times more gold that is worth 2 1/2 times as much in purchasing power, therefore the real value of his holding has risen by the one factor multiplied by the other, giving him 61/4 times as much goods or services as he had in 1920.

Jan 1, 1933

By Wilbur A. Nelson

In 1839, Gerard Troost,1 the first State Geologist of Tennessee, reported the occurrence of zinc ores in east Tennessee, in connection with the iron ores at Embreeville; in 1844,2 he refers to the zinc deposits of east Tennessee, especially the apparently rich deposits occurring in Jefferson and Claiborne Counties, while his ninth annual report 3 s a description of the zinc deposits of Jefferson County and a description of the most improved processes by which zinc is extracted from its ores. Yet, only during the last few years have these ores been successfully worked. As far as can be learned, prior to the systematic development of the Mascot district in 1911, no large-scale or successful operation of any of the zinc deposits was carried on. But in that year, after several companies had made considerable progress in developing the Mascot area and had proved a relatively extensive body of low-grade sulfide ore, the American Zinc Co. entered the field. It introduced modern methods of prospecting and mining and from the first was successful. Too great credit cannot be given this company for its pioneer work in a previously unimportant field. Throughout the history of its operations, the American Zinc Co. has confined its efforts to underground mining of the sulfide ore, sphalerite. This company has found that successful results in zinc mining in east Tennessee can be achieved only by expending large sums in prospecting and blocking out bodies of pay ore in sufficient magnitude for large-scale operations. At Mascot are located the mines of the American Zinc Co. of Tennessee, the mines being situated along the Southern Railway in the Ilolston River Valley, Knox County, about 13 miles northeast of Knox-ville. At first only open pits, which were worked for oxidized ores, were operated and the production was small. In 1900, the Roseberry Zinc Co. was organized and sank to a depth of 187 ft. what is now known as No. 3 shaft of the American Zinc Co. The upper 30 ft. was in residual clay,

Jan 1, 1925

By Robert G. Johnson, Richard J. Prosen

THE present work was done in connection with a program for investigating metal-to-ceramic braze techniques using the well-known reactivity of titanium with certain ceramic oxides. The investigation extended over the range of 0 to 30 pct Ti. The indium was obtained from the Indium Corp. of America and was specified to be 99.97 pct pure. The titanium was supplied by Metals Disintegrating Co. and was stated to be 99.5 pct pure. Each 2 to 4 g quantity of the alloy compositions studied was prepared using a mixture of 300 mesh powders pressed into pellet form. The pellets were heated in thin-walled molybdenum crucibles using a resistance-wound furnace in a vacuum less than 10-4 mm of Hg. Little reaction occurred between the molten alloy and the crucibles at the temperatures and short time intervals used. Only slight spectroscopic traces of molybdenum were found in the melt after a typical period of heating. The points shown on the phase diagram of Fig. 1 represent thermal arrest measurements. The phase boundaries shown are consistent with the thermal arrest and X-ray data obtained. The temperatures were determined using a Pt-Pt 10 pct Rh thermocouple with the junction spot-welded to a short molybdenum rod. The rod was almost completely immersed in the liquid metal, so that good thermal contact with the melt was achieved. The small mass of the crucible and its contents made it possible to obtain many heating and cooling curves in a few minutes time, an advantage which helped to minimize the effects of indium evaporation at the higher temperatures. A Brown strip chart recorder was used to display the thermal arrest curves. To check the technique, the melting point of 99.999 pure Al was measured and found to be within 1 of 660.2c, the accepted melting point. The upper limit of temperature with this technique was about 900°C beyond which the evaporation rate of indium became great enough to alter appreciably the alloy composition during the runs. A peritectic transition was found at 796°+ 5°C from 1.5 to 30 wt pct Ti. It was not found at 0.5 or 1.0 pct. A small super-cooling effect was observed. The melting-point transition to the B + L phase was found up to 20 pct Ti but not at 25 pct. Within the 1 deg accuracy of the measurement, the transition temperature was that of pure indium, 156°C. The liquidus line to the left of the 1.5 titanium point was located only approximately. The two crossed circle points at 1.0 and 0.5 pct Ti place a lower limit on the liquidus line and were determined by observing visually the cessation of vibrations in the melt caused by the damping effect as B-phase crystals were formed during cooling. The B-phase boundary was found at 23.8 pct Ti by X-ray analyses of small single crystals of the B phase isolated from 2 pct Ti melts. The compound was found to be Jetragonal with lattice dimensions of c = 3.052A and a = 10.094W. From the unit cell dimensions and the measured density of 6.42 i 0.05 g per cc, the compound was determined to be In4Ti3 which has 23.8 pct Ti. The calculated density of 6.44 g per cc is obtained assuming 2 mol

Jan 1, 1962

NEW MEMBERS The following list comprises the names of those persons who became members during the period of Feb. 10, 1918, to Mar 10, 1918. ADKINSON, HENRY M., Min. Engr Walker Bank Bldg., Salt Lake City, Utah. BARKE, A. C., Min. Engr., United States Smelt., Refin. & Min. Exploration Co., 1503 Hobart, Bldg., San Francisco, Cal. BARKER, F. L., Prof. of Min. and Geol., Pei Yang University, Tientsin, China. BEASLEY, ALFRED F., Supt. Of Refinery, Bunker Hill & Sullivan Min. & Cone. Co., Kellogg, Idaho. BEEKLY, A. L Chief Geol., Cosden & Co., Tulsa, Okla. BELLIS, ARTHUR E Met., N. E. Westinghouse Co., Springfield, Mass. BRAIN, ELMER C Mgr., United Gold. Min. Co., Granite, Ore. BRUNER, CRANE S., Engr., American Zinc, Lead & Smelting Co., Carterville, Mo. COLLINS,. HARRY R Mech. Engr., Fuller Engineering Co., Allentown, Pa. CRANKSHAW, ALDEN, Experimental Met., New Jersey Zinc Co. (of Pa.), Palmerton, Pa. GALLIGAN, EMMET F., Mine Supt., Homestead-Iron Dyke Mines Co., Inc., Homestead, Ore. GREENE, FRANK C Geol., Cosden Oil & Gas .Co., Tulsa, Okla. HALSEY, HOWARD G Field Engr., 0. M. Bilharz Min. Co., Miami, Okla. HARROUN, DOUGLASS HOUGHTON, Supt.., Aguascalientes Metal Co., Asientos, Aguascalientes, Mexico.

Jan 4, 1918

By I. B. Cadoff, J. C. Bilello, R. Rosenberg

Diffiusion of magnesium into the surface of LiF crystals to controlled depths and subsequent heat treatments provided a wide range of surface zone harahesses and structure, The bend strength of the LiF crystals was increased by as much as an or-dev of magnitude. Ductility was achieved when dislocation generation occurred in the diffusion zone or when dislocations penetrated to the surface from the intevior. A critical surface hardness of 130 to 140 kg per sq mm was found helozu which generation could take place in the diffusion zone and ahoue which the zone was impenetrable, This hardness was obtainable by several methods, among them the aging of quenched MgF2 -LiF solutions to produce MgF, precipitation. Maximum hardness was ohtained in quenched specimens with no visihle evidence of MgF,. Diffusion-zone formation followed a parabolic rate law and an activation energy of 20.9 kcal per mole was obtained for the process. RECENTLY, the properties of ionic crystals as related to surface condition have been receiving much attention, specifically the transitions between ductile and brittle behavior. Originally Joffe 1 showed that NaCl crystals could be made ductile by immersion in water and related this to the elimination of surface microcracks. Aerts and DeKeyser 2 and Gorur 3' have subsequently shown that ionic crystals are inherently ductile and are embrittled through contact with air. Machlin and Murray4 hypothesized that a layer of NaCIO3 produced by contact of ozone with NaCl induced embrittlement by acting as a barrier to outward dislocation flow. westwood,' Rosenberg and Cadoff,9 and Bilello and cadoff' have reported surface strengthening of LiF crystals by coating with a magnesium compound and then heat treating for adherence. The major effect of the coat was to inhibit dislocation-slip lines from reaching the specimen surface. westwoods showed microcrack formation and fracture to be caused by slip-band interactions at the surface. The material presented in this paper is an extension of the work reported earlier by Bilello, Rosenberg, and cadoff'6,7 and illustrates the wide range of surface properties and bulk behavior obtainable by use of heat-treated magnesium-diffused surface regions in LiF crystals. EXPERIMENTAL PROCEDURE The LiF single crystals were obtained from the Harshaw Chemical Co. Some batch to batch variation was observed; therefore all specimens for a given test series were cleaved from the same crystal. The typical dimension used was 1 by 0.1 by 0.40 in. Surface damage resulting from cleavage was removed by chemically polishing in a 2 pct NH4OH solution. Each group of specimens was given a vacuum anneal at 700°C for 4 hr to provide a base standard for measuring comparative effects of various surface treatments. To produce the reacted surface zone, the annealed specimens were immersed in a boiling suspension of MgF, in doubly distilled HzO, agitated slbwly for 30 sec, removed, and dried at room temperature. Uniform coatings of MgF, were deposited with a thickness of approximately 5 mils. It should be noted that this technique can be modified for use with crystals which are soluble in water by using boiling absolute alcohol as the dissolving medium. This was found effective for the coating of NaCl with MgF2. The diffused surface zone was obtained by annealing the coated samples at elevated temperatures in a vacuum of lob4 mm Hg. Penetration depth was controlled by varying the annealing time from 1/2 to 28 hr. After heat treatment, the samples were tested for bend strength and hardness. Load was applied by four-point bending in a hard-beam testing jig. Four-point rather than three-point bending was used to provide a wide area of constant stress and to minimize the effect of localized inhomogenities in the specimen. The deflection rate was 8 x min-' and the distance between knife edges was 1/4 in. Load-time curves were obtained from a chart recorder coupled to the machine and converted to resolved shear stress on the shear plane vs deflection, as plotted in the figures. The unstressed portions of the sample outside of the two outer knife edges were used for the microhardness studies. Microhardness measurements were made with a Bergsman tester attached to a Reichert metallograph. All hardness impres-

Jan 1, 1964