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By William Fink

THE investigation of the phase relations of high-purity aluminum-base alloys is a part of the fundamental research program of the laboratories of the Aluminum Company of America. The results of a number of binary and ternary systems have previously been published in the transactions of this society. The aluminum end of the binary aluminum-titanium system has been studied. This system has received relatively little attention. To the authors' knowledge, there are two previous papers on this subject. E. van Erckelens1 determined the constitutional diagram reproduced in Fig. 1. .According, to this diagram, the liquids represents the separation of TiAl4 (Ti = 30.7 per cent.). He concluded that this is the composition of the compound, because in his work the eutectic horizontal terminated at 30.7 per cent. titanium and the metallographic examination of a sample of this composition revealed only one phase. According to the constitutional diagram developed by W. Manchot and A. Leber,2 reproduced in Fig. 2 from data given in their article, the liquidus represents the separation of the compound TiAl3 (Ti = 37.2 per cent. ). The composition of the compound was derived in a manner similar to that utilized by van Erckelens. Moreover, Manchot and Leber confirmed the composition of the compound by analysis of the constituent left as a residue after dissolving the alloys in weak sodium hydroxide solution. Although these are the only publications describing the constitution of the system, other investigators have studied the composition of the titanium compound. L. Wöhler3 says that there is a compound TiAl3 which was later confirmed by W. Manchot and P. Richter4 and by

Jan 1, 1931

By G. T. Jackson

The Alaska Gastineau Mining Co.'s mine is located at Perseverance, about 4 mi. east of Juheau, Alaska. Its property consists of a group of claims, the lode system traversing these claims for a distance of 11,000 ft. (3352 m.). It is shown in Fig. 1. The ore deposits occur in what is known as the Juneau gold belt. This gold belt can be traced for about 50 mi. northwest of Juneau and 40 mi. southeast. It consists of a single band, several hundred feet wide, in which stringers and veins of quartz, carrying gold, occur in a slate formation near its contact with some altered volcanic rock known as greenstone. The Perseverance orebody consists of stringer lodes, having a strike northwest and southeast, dipping about 60° to the northeast. These

Jan 1, 1920

The regulations governing the filing of claims under the War Minerals Relief Act have been amended so as to allow claimants to file a brief with the questionnaire. It has been decided that hearings will be conducted by the War Minerals Relief Commission when good reason for such action can he shown. When justified, the Commission will conduct the hearing at a point easy of access from the mining district concerned. Applications for relief are beginning to reach the Commission in considerable volume. Thirty claims have been filed in such condition as has permitted of their formal filing with the Commission. Many others have been returned with instructions as to the information required and the procedure it is necessary to follow.' An effort was made to induce the Secretary of the Interior to open a Pacific Coast branch office of the War Minerals Relief Commission; this he has declined to do, claiming that it is impracticable to divide the work.

Jan 5, 1919

J: H. POLHEMUS, New York, N. Y. (written discussion*).-The Joplin .mining and milling practice has largely influenced operating methods in the Wisconsin district. Milling equipment is essentially of the same type with the notable exception that no tables are used. The treatment of the flue 'sands has been attempted several times but without commercial success. Table material coming from any one mill is low both in tonnage and zinc content. The iron is comparatively high as the pyrite-line "chat" is much more prevalent than the zinc-lime attached particle. In the finer sizes the zinc occurs mainly as free mineral. These condi-tions make the production of good-grade table concentrates very diffi-cult. The accompanying tabulated results from several mill tests indi-cate the character of the mill tails. I think the average mill tails in the district assay nearer 1.5 per cent. zinc than under 1 per cent., as stated by Messrs. Boericke and Garnett.

Jan 10, 1919

GWILLIAM H. CLAMER (Philadelphia, Pa.).-About 16,000 tons of tin is used annually in the production of white metals. The real reason for using the so-called genuine babbitt, which is a high-tin base babbitt, perhaps in the majority of cases, is that tin has always been. a high-priced metal and people naturally believe that what they pay a high price for must be good. Mr. Jones has shown that the common metal, lead, is a superior base for most purposes for Which babbitt metal is used. The addition of lead is often looked upon as adulterant to genuine babbitt, and specifications for this reason rigidly restrict the lead content. A sub-committee of the Society for Testing Materials, at the meeting in June, presented tentative specifications on babbitt metal, in which were included twelve formulas, containing from zero to: 20, per cent. of tin, and several containing from 65 and 92 per cent. Babbitts. containing

Jan 1, 1919

FROM newspaper reports circulated in Indonesia, it seems quite obvious that many people, even the left-wingers, have serious doubts concerning the wisdom of the Indonesian Government in nationalizing the Bangka Island tin mines, formerly operated by the Dutch Billiton Co. Chief source of American dollars for Indonesia has been the 34,000 ton tin production of its mines. Right now, both left and right are concerned with whether the Government will be able to maintain and increase current production. The right wing Moslem party newspaper, Mimbar Indonesia, stated: "It will no longer be possible any more for radical labor leaders to find foreign scapegoats and tell the workers they are working only for foreign interests and foreign managements. It is up to labor now to increase its labors for the national good. It will be a new experience, and the problem is whether we are capable enough to manage these important mines."

Jan 4, 1953

By Ferron A. Olson

Occasionally it is good to consider the past, assess the present and project the future. Curriculum, enrollment, matriculation of graduates and changes in industry which influence mineral education are all relevant for determining what changes will be needed in educational institutions to support growth and development in the United States. It would appear likely that with environmental pressures, energy needs with present stress in fossil fuels and general societal needs for metals and minerals that mining and metallurgical engineering faces a period of growth and may be on the threshold of a new era with a vitality that has not been enjoyed for several decades. The following information is based on material obtained through questionnaires received from twelve schools accredited in mining or mineral engineering (out of 18 in the U.S.), 2 not accredited and 5 which no longer have mineral engineering disciplines. The schools presented do not include the smaller nor larges of the undergraduate programs in mining engineering.

Jan 8, 1972

PHILIP L. GILL, New York, N. Y. (written discussion*).There is one feature of the fire-refining of electrolytic copper which I believe should be mentioned when the relation of oxygen content to the "pitch" or "set" of refined copper is under discussion; that is, the segregation of impurities. Variation of "pitch" or "set" is frequently noted in castings of different shapes, cast at the same time from the same furnace, though the oxygen content remains identical. For instance, it is possible to cast two wire-bars in the same shaped molds from the same ladleful of copper, the one 2 in. thick showing a good level set, the other, 4 in. thick, being overpoled. Also, when two bars are cast of the same weight and at the same time from the same furnace, one bar in a copper mold at the proper temperature, the other in a mold that has been allowed to get overheated, the bar in the hot mold will show

Jan 8, 1918

By H. Krueger, H. N. Hersh

USE of autoradiography in diffusion studies offers the advantage that no repeated sectioning is necessary and that the analyses are performed in a simple manner over the continuous range of penetration depths. As part of a program of solid-state physics, it was desired to develop the autoradio-graphic method' quantitatively for use in diffusion studies. Results are reported here for the self-diffusion of silver. Silver was chosen because the existing data are good enough to evaluate the technique." The silver used in this investigation was obtained in the form of ¼ in. diam rods of polycrystalline material, 99.99 pct purity. The radioactive silver, Ag110 (ß, y), was obtained as the nitrate and converted to the chloride for use in a standard cyanide plating bath. The diffusion specimens were 1/2 in. lengths of the rod. They were mounted in bake-lite and the exposed circular face carefully ground and polished. Prior to electrodepositing radioactive

Jan 1, 1956

With the coming of the month of 'October the various sections are beginning active work for the winter. The Colorado, Washington, Montana, and New York Sections are all doing good work in raising funds for the hospital bed at Rheims which is to be a memorial to the members of the A. I. M. E. who gave their lives in the great war. We hope that all the other sections will begin to work with this object in view and will make even a better record than they did with the Belgian Relief Fund. It was with much regret that the President, Mrs. James F. Kemp, and the Secretary, Mrs. Sidney J. Jennings, were obliged to forego the pleasure of attending the Chicago meeting in September. They were, however, ably represented by Mrs. Arthur S. Dwight who gave an informal talk after which was formed the Illinois Section, which has our best wishes for all success-" Over the top and the best of luck!"

Jan 11, 1919

By A. G. Paithankar, G. B. Misra

Although certain physical mechanical properties of rocks have been claimed to give an estimate of penetration rate in percussive drilling, the authors' work shows that the correlation of penetration rate with individual rock properties is Poor. The authors have developed a good correlation between penetration rate and a set of rock properties but the relation is complex. Energy per unit volume has been used as a measure of penetration rate in percussive drilling by Hustrulid and Fairhurst; however, their test setup is large wing a full size drill bit. The authors determined the minimum energy for unit volume Ev min for any rock at the optimum index angle in a simple laboratory drop tester wing a sharp microbit with a tip angle of ll0°. This Ev min has been found to correlate well with penetration rate obtained in controlled laboratory drilling in different rocks for different stages of bit wear. A comprehensive relation has been developed between penetration rate and Ev min.

Jan 1, 1981

By N. V. Hansell

l. INTRODUCTION. THE last few years have shown an increasing interest in the subject of beneficiating iron-ores -in all iron-producing countries. In the United States, this movement has been slower than in certain parts of Europe, for the obvious reason that the abundance and relative cheapness of the Lake Superior iron ores has hindered the development of enterprises for the preparation of low-grade ores. Gradually, however, conditions have changed. The world's consumption of iron is increasing enormously. Being in 1900 about 40,000,000 tons, in 1910 ii was already 60,000000; and there is no reason to doubt that for the near future the increase in iron-consumption will continue at the same rapid rate, especially with, the development of China, certain parts of Africa, and other regions which have hardly been touched as yet by modern industrialism. It is. therefore, not surprising that apprehension is felt that the known available iron-ore resources of the world are gradually being depleted. Signs of this feeling are the recent investigation, under the direction of the U. S. Geological Survey, of the iron-ore resources of the United States, and the estimate presented to the last International Geological Congress, at Stockholm, Sweden, of the iron-ore resources of the world. These investigations have emphasized the fact that the known high-grade ore-deposits are limited in extent, and will, at a not distant future, be exhausted, compelling the iron industry to depend for raw material on the enormous deposits of low-grade ores which are distributed over almost all the world. The discovery of new deposits of high-grade ore, in countries not yet thoroughly explored, will not materially change this prospect. Of course, the part which such new deposits will play in the future cannot be forecast. The difficulty and cost of transportation will probably exclude many of them from use at the present centers of the iron industry.

May 1, 1912

By J. B. Morgan

The mechanical behavior of MgCu2 from 20 o to 725°C has been determined by "brittle-ring" tensite-test techniques, axial compression, and bending experiments. Compressive ductility begins at 450°C (0.65 T/Tm) and slowly increases with increasing temperature white the tensile ductility is characterized by an abrupt brittle-ductile transition at 600°C (0.8T/Tm). The compressive strength increases eightfold from room temperature to 400°C with a "normal" decrease as the temperature is further increased. The tensile strength goes through a rather abrupt threefold increase above 600°C with a subsequent decrease at higher temperatures. The slip system is (111)[110] and the twinning system is (111)[112]. At high temperatures MgCu2 is quite rate-sensitive, and dynamic yield points are observed that are extremely orientation-dependent. The high-temperature creep behavior under constant load is characterized by an increasing strain-rate with time. The general characteristics of the mechanical behavior make it possible to classify MgCu2 with those materials in which initial mobile dislocation density and the dislocation velocity-stress dependence are significant in determining mechanical response. Mgcu2 is the C15 prototype of the cubic Laves phase. Its range of homogeneity extends from 32.8 to 35.5 at. pct Mg at 500°C and narrows at lower temperatures. The lattice parameter is reported to vary from 7.02 to 7.05A,1 and the compound is completely ordered to the melting point of 819°C. MgCu2 has a brassy metallic appearance, is extremely brittle, and many of its physical properties are intermediate between those of the constituent elements: the electrical resistivity is 3.5 x 10-6 ohm-cm, Young's modulus is 10x 106 psi, the shear modulus is 6 x l06 psi, and the thermal coefficient of expansion is 18.7 x 10-6 cm per cm per "C from 20" to 250°C. Usually, properties of intermetallic compounds as functions of temperature have been determined by hardness, compression, or impact behavior, and almost all of these experiments have been performed on polycrystalline materials. Tammann and Dahl,2 for instance, determined the onset of ductility in a series of binary intermetallics by ball-hardness measurements and found the onset to range between 0.71 and 0.96 T/T,. Lowrie's3 investigations included some tensile properties, and he found ductility beginning around 0.65 T/Tm for most materials examined. His work did include some data on polycrystalline, nonstoichiometric MgCu2, however. The present work is an attempt to extend the examination of the particular compound MgCu2 in single-crystal form in order to aid the formation of general concepts about mechanical be-

Jan 1, 1965

By Robert H. Richards

Tuns truly remarkable machine was built on a preliminary scale in May, 1895. The first full-sized table was built by Mr. A. R. Wilfley, and was used in his own mill in Kokomo in May, 1896. The first table sold for installation was placed' in the Puzzle mill, Breckinridge county, in August, 1896. The mill enthusiasts at first hailed it as the cure for all the ills that flesh is heir to in the milling line. A little later it was found to make losses which were serious, and on this account the table succeeded only to a limited extent in displacing the vanners of the gold-mills. Still later, mill-men in a number of districts throughout the country made special studies of the faults of the machine, and devised a number of ways of grouping supplementary machines to overcome as far as possible the losses, and at the same time retain the benefit of the extraordinarily large capacity accompanied by the production of clean concentrates for which the machine has become so justly famous. I hope to make an exhibit of some of these methods in an appendix to my book on ore-dressing which is now in preparation. These experimenters have not written up the subject, and if they possess all the facts they have not given them out for the benefit of the mining profession at large. The object of this paper is to obtain the facts and to pre¬sent them so clearly that their bearing can be seen by all. To this end two complete series-'of tests have been planned. One (the present paper), to study concentration of galena in presence of quartz; the other (to follow shortly), to study concentration of chalcopyrite in presence of quartz. Some authorities claim that the table does its best work when treating natural products; by this phrase I mean products which have been crushed to pass through a limiting

Jul 1, 1907

By J. B. Coher, M. B. Bever

COLD work destroys long-range order, as was first observed by Dehlinger and Graf.1 Dahl2 showed that the mechanical disordering caused by cold work produces changes in those properties that are affected by long-range order. The existence of order has a marked effect on tile manner in which an alloy deforms and therefore on its mechanical properties.L' The relation between order and deformation behavior however, is only beginning to be understood. Seemann and G1ander4 suggested that cold work reduces an ordered alloy to a kind of gruel of antiphase domains. According to Cottrell,5 superdis-locations and pairs of dislocations in a slip plane connected by a strip of anti-phase domain boundary provide deformation mechanisms which do not change the state of order. In general, however, slip may be expected to produce new domain boundaries and destroy order if dislocations move on intersecting planes or cut through existing domain boundaries. The yield strength of an ordered alloy may pass through a maximum with decreasing domain size.5"7 The reduction of domain size resulting from cold work may, therefore, lead to a maximum in strength properties. Flinn8 suggests that dislocations can climb by short-range diffusion during deformation and thus can generate domain boundaries not only on slip planes, but also on other planes which will be those with the lowest domain-boundary energy. It has long been known that the rate of strain hardening of an alloy in the ordered state is larger than in the disordered state.3'9 Also the slip bands in ordered CU3, AU10 and Ni3Mn" are finer than in the disordered alloys. The stress which causes initial yielding in Cu,Au passes through a maximum with decreasing domain size.6'12 A maximum has also been observed in the hardness of ordered Ni3Mn as a function of strain.' These observations suggest, but do not prove, that domain size reduction occurs during deformation. According to Fisher13 slip destroys short-range order and thus the strength of an alloy is related to the degree of short-range order present. Rudman and Averbach14 and Averbach et a1.,15 demonstrated that cold work reduces short-range order in copper-gold and gold-silver alloys. Destruction of long-range and short-range order by cold work implies slip on an appreciable fraction of planes. Yielding of an alloy in which short-range order exists or antiphase domain boundaries are present should be discontinuous because the first dislocations moving across the slip plane meet with the largest resistance.5 Such discontinuous yielding has been observed in CU3AU6,16 and Cuzn.l7 This phenomenon, however, can also be explained by mechanisms not involving order.b The published investigations of the effects of cold work on alloys with long-range or short-range order have not been covered thoroughly in reviews of order-disorder phenomena. These investigations, therefore, will be listed here. They have been concerned with strength properties> 2,3,6,8,9,12,16-21 electrical resistivity,2,4,18,19,21-26: thermoelectric power, magnetic properties,2,18,21,26 and X-ray strain'1,2,14,15,27,28 The slip systems and the appearance of the microstructure after deformation in ordered and disordered alloys have also been investigated. 6.10.ll,l7,23,29,30 The alloys used in these investigations were copper-gold. 1-4,6,9,10,14,16,18 23-26,28,29 copper-zinc. L7. 19. 20,30 nickel-manganese,2 11,21 iron-aluminum. iron-nickel,' copper palladium,4,18,22 gold-silver.4,18,22 and palladium-silver-copper.4 In the work reported here. the changes in properties of polycrystalline Cu3Au were investigated as functions of strain in wire drawing and rolling. Specimens were heat treated before deformation

Jan 1, 1961

By Maurice Lacasse, Pierre Legast

GENERAL OUTLINE For more than one hundred years, asbestos ore has been mined on Les Mines d’Amiante Bell's property at Thetford-Mines , Quebec, Canada. In 1878, the first tons of fibre were produced. The mine operated as an open pit until 1951 at a yearly production of about 330 000 mt of ore. Since 1951, the mine has operated underground using a block caving method. The mine produced 725 000 mt per year until 1978, when the rate of production was increased to 1 100 000 mt. The ore was produced entirely fm the first lift on 650 level until 1976. Then, a second lift on 950 level was put into operation to replace production facilities fm the first lift which is now exhausted. Annual fibre production is 72 500 mt with grades £ran 3 to 7. The total work force is 600 people. The host rock is a peridotite partially serpentinized. The asbestos fibre seams occur as stockwork deposit structurally controlled by talcose shear zone. The geological rock formations are heavily jointed and have a wide range of competence. Asbestos ore bodies have an heterogeneous nature which des difficult geological interpretation. THE GRIZZLY METHODS A full gravity method was used on the first level where the caved ore was drawn from finger raises onto grizzly bars spaced at 480 mn. Oversize blocks were reduced by secondary blasting. The ore fell by gravity in- to the ore pass below the grizzly chamber and was loaded into 5.7 mt haulage cars through a 1.2 m wide chute. Access to the undercut drift was fm the grizzly drift through finger raises. The undercut trough was drilled and blasted in a 1.2 m interval ring sequence into a slot situated at the end of each panel. The undercut stope was emptied through the finger raises. The undercut retreated from South to North at blast interval determined by the finger raises spacing. Fig. 1 represents the various steps involved with the grizzly method. Extraction drift dimensions were opened 1.8 m wide x 2.4 m high with anchor rock bolts and wire mesh where safety required them during excavation. Grizzly chambers were excavated at 2.4 x 2.4 x 4.6 m long on a 7.6 x 7.6 m grid spacing. Ore passes with dimensions of 1.5 x 1.5 m were developed from the haulage drift. On the extraction level, headings were drilled with jacklegs and cleaned by slusher into ore passes to the haulage chutes. The support used in the grizzly chambers was square concrete structure with 150 mn H beam reinforcement. The H beam was partially buried in the concrete and had one free face to allow for difference frequency of blast vibration between concrete and steel. The supported brow of the chamber had an opening 1.5 x 2.1 m. Ore passes were ring concreted 150 mn thick without any reinforcement. A 24 MPa compressive strength concrete was pumped and poured in pre-assembled forms. Based on the success of this method on the first level, the same layout was repeated on the second level. With the start of undercutting on the second lift, signs of deterioration were noticed in extraction drifts. At first, there was great concern as the operators were confident that standard repair techniques could cope with such a situation. An intensive program of support repair and a reduction of draw resulted. The following method of repairs were used: 1) Steel square sets of 150 mn H beam at 0.6 m intervals were installed. 2) This was reduced later to 0.3 m interval and eventually to a skin to skin steel structure. 3) Yieldable arches were introduced spaced at 0.9 m intervals, linked laterally with 150 m. H beam. 4) The yieldable arches spacing was then reduced to 0.46 m and eventually installed skin to skin. However, this support was not successful.

Jan 1, 1981

By R. Grierson, R. N. Parkins

The m.echanica1 properties, at high lzomologous temperatures, of the intermetallic compounds InzBi and Mg17A112 were measured as a .function of temperature, applied strain rate, previous thermal and mechanical history, and composition. Mgl,Al12 was investigated ilz compression, whereas Zn,Bi was investigated in tension. A decrease inflow stress with increasing strain was observed jor both alloys. The results obtained are discussed in terms of the dislocation-multiplication processes in these materials. MANY intermetallic compounds are reported to undergo a brittle-ductile transition at high homologous temperatures.' There is evidence in the literature that some of these compounds exhibit a large yield drop when plastically deformed.'j3 Both of these forms of behavior are shown by the covalent elements germanium and silicon4,5 and also by certain ionic compounds.8 The present work is a study of the deformation, at high homologous temperatures (>2/3 Tm), of two intermetallic compounds, In2Bi and Mg17Al12. InzBi has a disordered hexagonal structure7 (c/a = 0.598) and a solubility range of 32.3 — 33.2 at. pct Bi.8 It has a melting range from 72° to 89°C. Mg17Al12 has an ordered bcc (A12 type)7 structure and exists over the range 50 to 60 at. pct Mg8 with a melting range from 437° to 462°C. We have been unable to find any reference to previous investigations of the mechanical properties of BiIn,. Novikovg has reported that cast samples of Mg17A112 show ductility, when bend-tested, at temperatures above 380°C. EXPERIMENTAL Ingots of In2Bi and Mg17Al12 were melted under an argon atmosphere and cast, in situ, in a graphite crucible. The materials used were of 99.99 pct purity. The alloys prepared contained 66.9 at. pct In in the case of In2Bi and 58.4 at. pct Mg in the case of m17A112. The ingots were homogenized and then extruded. Two-in.-diam Mg17Al12 ingots were extruded at 375°C to give 3/8-in.-diam rod. The rate of formation of this rod was 0.25 in. per min. One-in.-diam InzBi ingots were extruded at 20°C, using a rate of 1 in. per min, to give 1/8-in.-diam rod. In both cases the extruded rod had a recrystal- lized, fine-grain, structure. (For Mg17Al12, d = 11.2 µ; for BiIn2, d = 22 µ.) Mechanical-property determinations were made in a hard-beam machine, in tension in the case of In2Bi and in compression with Mgl7Al12. The tensile tests were on specimens having a gage length of 1.1/2 in. and a diameter of 1/8 in. The compression tests on Ml7A112 were on specimens of 3/8 in. diam by 3/8 in. high and the ends were coated with poly-tetrafluorethylene to minimize friction. RESULTS In2Bi. Fig. 1 shows, particularly at the higher applied strain rates, that In2Bi exhibits a marked yield drop as the deformation increases to about 2 pct, after which the material shows neither hardening nor softening up to 15 pct strain. The magnitude of the yield drop, the stress in the region of flow under constant stress (the stress plateau), and the 0.5 pct proof stress were all dependent upon the applied strain rate according to an expression of the form

Jan 1, 1965

By E. S. Bumps, H. D. Kessler, M. Hansen

The titanium-rich end of the Ti-AI phase diagram has been determined to the compound TiAI3 (62.7 pct Al), thus joining the aluminum-rich portion previously investigated by others and completing the diagram. Micrographic analysis and X-ray diffraction were the chief methods used to determine the phase relationships. THE Ti-Al phase diagram has been investigated as part of a program on titanium phase diagrams for the Wright Air Development Center. Included in the available information concerning the phase relationships in titanium-rich Ti-A1 alloys is a brief statement by Brown' that: "aluminum raises the transformation temperature to 1000°C (183Z°F)." This observation is interesting in that it is the first example of a metallic alloying component raising the transformation temperature of titanium, and consequently widening the field of the a solid solution. Busch and Freyer' presented resistivity data which indicated the formation of titanium-rich solid solutions of 1 and 3 pct A1 alloys prepared by powder metallurgy methods. Duweza found that there is only one other intermediate phase other than the known compound TiA1, (62.7 pct Al). This phase, designated as y, is of variable composition; its crystal structure is of the AuCu type and is therefore based on the composition TiAl (36.02 pct Al). Earlier work on the constitution of the aluminum-rich alloys has been reviewed by Hansen, and need not be discussed here. The tetragonal crystal lattice of TiAl,, as found by Fink, Van Horn, and Budge," was confirmed by Brauer." Recently, Schubert7 has reported that TiA1, is homogeneous within a limited composition range; however, the solubility limits were not given. The Ti-A1 phase diagram as presented in. this paper was determined by micrographic analysis of alloys containing from 1 to 62 pct Al, annealed at and quenched from temperatures between 700" and 1400°C. The phases and phase ranges investigated extend to the compound TiA1, (62.7 pct Al) to join the aluminum-rich end of the system determined by other investigators, thus completing the diagram. Methods of Investigation Preparation of Alloys: Iodide titanium, 99.9+ pct pure, obtained from the New Jersey Zinc Co., and high-purity (99.99+ pct) aluminum sheet from the Aluminum Co. of America were used to make up alloy ingots weighing 10 to 20 g. Detailed descriptions of melting techniques have been presented previously for work on the Ti-Mo and Ti-Cb> nd Ti-Si" phase diagrams. Briefly, the melting practice consisted of arc melting an accurately weighed charge in a copper block crucible insert in a non-consumable tungsten electrode furnace, under helium at atmospheric pressure. All ingots were carefully weighed after melting to detect possible losses. Comparison of weight before and after melting showed no appreciable weight changes. Also, chemical analyses were in close agreement with nominal compositions, Table I. The diagram as presented is, therefore, based on nominal compositions. Alloys were prepared having the following nominal aluminum contents: 1 ... 36 (1 pct increments), 38, 40, 41, 42.5, 44, 45, 46, 47.5, 49 . . . 64 (1 pct increments), 67, 70, 80, and 90. Ingots with up to 14 pct A1 were cold-pressed various amounts in order to increase the rate of attaining equilibrium structures on heat treatment. The amount of cold deformation that could be applied decreased with increasing aluminum content, until alloys containing 12 pct A1 or more cracked after only a few percent deformation. Annealing Treatments: Samples annealed at temperatures of 700" to 1000°C were sealed in

Jan 1, 1953

By W. Chubb

By measuring the hardness of metals at temperatures just above and just below their allotropic change point, it has been established that crystal structure has a real effect upon the strength of metals. The DPH of cobalt, iron, titanium, uranium, and zirconium have been measured at temperatures up to 1000°C. It was found that the body-centered-cubic crystal structure is always the softer structure when it is involved in an allotropic transformation. The close-packed and more complex structures are inherently harder, and may be expected, therefore, to be better base materials for high strength alloys. IT has been observed that for metals with nearly the same melting point (i.e., tin and lead, magnesium and aluminum) the metal with the more complex crystal structure has a higher tensile strength and hardness. It might be asked whether this effect is really caused by the difference in crystal structure; and, if so, just what is the contribution of crystal structure to the strength of these metals. A qualitative answer to these questions can be obtained by measuring the change in hardness produced by the change in structure in metals exhibiting allotropic forms. The evidence for changes in mechanical properties during allotropic transformations is rather meager. In 1909, Rosenhain and Humfrey' observed that "ß" iron showed much less deformation at the transformation temperature than a iron. By means of a torsion test, Lee found that iron bars were "critically plastic" at the a-7 transformation temperature. Sauerwald and Knehans have shown that the dynamic hardness of iron increases between 900" and 1000°C. In 1930, Albert Sauveur' presented data on the hardness, tensile strength, and torsional strength of pui-e iron up to 1000°C. He concluded, "At 900°C, the a iron transforms into y iron, and this is accompanied by increased strength and stiffness and decreased ductility." The same year, Schischokin" obtained data on the hardness of thallium at temperatures above and below its transformation temperature. His data are replotted on semilogarithmic coordinates as Fig. 1. The fact that his data fall on straight lines in this type of plot is believed to attest to the purity of his metal and the accuracy of his results. In 1941, Nadai and Manjoine" obtained tensile data on pure iron with an indicated increase in strength at about 900°C. These experiments make it quite evident that changes in mechanical properties occur when a metal transforms from one crystal structure to another; but, except for Schischokin's data on thallium, none of the measurements seem accurate enough to determine the relative magnitude of the mechanical property change. Materials The metals that have been examined for changes in hardness during transformation include l—as- deposited commercial electrolytic cobalt about 99.7 pct pure, 2—Armco ingot iron, 3—are-melted iodide titanium of a purity in excess of 99.8 pct, 4—uranium of a purity in excess of 99.5 pct, 5—are-melted iodide zirconium of a purity in excess of 99.8 pct, 6—annealed, 0.08 pct C, rimmed steel, and 7—commercially pure RC55 titanium. While the purity of the first five of these materials leaves something to be desired, it will be noted that the observed hardness discontinuities occurred at the accepted transformation temperatures. (These temperatures are indicated by vertical arrows in Figs. 1 and 3 through 7.) The last two materials are commercial alloys introduced to show the effect of minor alloying elements upon the hot hardness curve. Apparatus Hardnesses at elevated temperatures were determined by means of a vacuum hot hardness machine. A diagram showing the basic features of this machine appears as Fig. 2. This machine is essentially a deadweight hardness .machine in a furnace within a vacuum chamber. The sapphire-tipped indentor

Jan 1, 1956

By M. L. Hammond, G. M. Bowers

Silicon dioxide films have been prepared on silicon wafers by the oxidation of SiH, near 400°C. Results previously reported by Goldsmith and Kern7 have been qualitatively corrobovated using a system of different geometry, and significantly greater deposition rates have been achieved. The deposition rate is independent of thickness and nearly independent of the O2/SiH, ratio over a wide range; however, the rate is strongly temperature-dependent. The structure of the deposit depends upon the cleanliness of the substrate, and the electrical field strength of the deposited oxide depends upon the nature of the electrodes. MULTILEVEL interconnects in integrated circuits using aluminum metallization require an insulator that can be deposited at low temperature. Because the A1-Si eutectic is only 577°C, the maximum deposition temperature must be below about 500°C to prevent reaction of the aluminum with the silicon and with other materials in the integrated circuit. Many methods of depositing insulating films of SiO, and other dielectrics have been reported'-6 but the technique described by Goldsmith and Kern7 offers the simplest method of preparing SiO, films. The technique involves the reaction of SiH, and 0, to form SiO, films in the 300" to 500°C temperature range. Previous work using this gas system has been reported8 and the initial development work at Philco Microelectronics was done at the East Coast R&D Laboratories. 9 This paper corroborates some of the results of Goldsmith and Kern,7 shows that much higher deposition rates can be obtained than previously reported, and presents some observations on the structure of deposited SiO, films. EXPERIMENTAL CONDITIONS Fig. 1 is a schematic drawing of the apparatus used in this study. It differs from that of Goldsmith and Kern in that 1) the gases are mixed before they enter the reaction chamber, 2) there is no fritted glass diffuser, and 3) the wafers are stationary during deposition. The control thermocouple was in a well located 0.06-in. from the substrate, and three gas supplies were used: 1 pct SiH4 in N 2, O 2, and N 2. Water vapor must be excluded from the plumbing to prevent the formation of colloidal SiO, and the SiH4 must be diluted with an inert gas because SiH4-0, mixtures are extremely flammable above about 4 pct SiH The wafer temperature was determined by attaching a thermocouple to a test wafer and the temperature was maintained to +5 C. The conditions used in this investigation are listed in Table I. The temperature range was chosen for compatibility with the A1-Si system. The volume ratio of 0, to SiH4 is the actual volume of 0, delivered to that of SiH4, taking into account the initial dilution of the SiH4. This ratio, which was used by Goldsmith and Kern,7 is a useful indicator of the experimental conditions. The active/inactive ratio is the ratio of the volume of active gases, SiH4 and O2, delivered to the volume of dilution gas. The active/inactive ratio is an important parameter to specify for deposition rate determinations since it determines the amounts of reactants that arrive at the sample per unit time. Fairly high dilution ratios were necessary to achieve uniform deposits of SiO,. Most of the process characterizations were performed on the polished (111) face of 3 to 5 ohm-cm, n-type silicon wafers which were 0.009 in. thick; but the data approximately apply to deposition of SiO, on thin films of aluminum. It is difficult to obtain accurate deposition rate data over aluminum films because of coarsening the aluminum surface during exposure to 300" to 400°C. The deposited SiO, film fol-

Jan 1, 1969