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By Keith Leonard Sutherland

This paper is a study of the differential flotation of the sulphide minerals in the presence of salts of silver, lead and zinc. In practice, accidental activation due to these salts is more important than their use as reagents to replace copper sulphate. The general method of investigation has been based upon contact tests, the temperature of 35°C being chosen in conformity with earlier work. Potassium ethyl xanthate and potassium amyl xanthate were selected as collectors and pure sulphide minerals were used. The experimental procedure has been outlined in earlier papers and all solutions were kept carbonate-free.14 Contact, or spreading of an air bubble, at a mineral surface indicates the presence of an adsorbed collector film. Purity of Reagents The xanthates were purified in the usual manner.' Neither the cyanide nor the sodium hydroxide solutions contained sufficient carbonate to give a precipitate with barium chloride solution. The silver sulphate was prepared from pure silver nitrate by evaporation with concentrated sulphuric acid until there was no evidence of brown fumes, This solution was diluted and the difficultly soluble sulphate washed with water so that unchanged nitrate was dissolved. The resultant crystalline powder was pure white. The lead and zinc salts were prepared by dissolving especially pure lead and zinc in C.P. nitric and sulphuric acid solution and the crystals drained. The standard solutions were checked by titration. It was felt desirable to use the sulphate radical wherever possible, but since lead sulphate was insufficiently soluble for the purpose of the experiments, it was necessary to use some other lead salt. A.R. copper sulphate was used without further purification. Results The results are presented in the accompanying figures; the areas of noncontact (nonflotation) are shaded in Figs. 8, 9, 10 and 11; in the remainder they lie to the right of the curve. Zinc Sulphate The curves in Fig. I are to be compared with those for Fig. 2, for which zinc sulphate is absent. This comparison shows that the influence of the zinc ion is usually small. Its influence is more marked, however, for chalcopyrite in the absence of cyanide. The influence of zinc sulphate is also marked for copper-activated sphalerite, for which tests were made only in the "absence of cyanide. The results are of importance in the separation of pyrite from copper-activated sphalerite when zinc sulphate is added in the lead flotation section (p. 204 of ref. I). Sphalerite does not adsorb the collector (i.e., become floatable) under the conditions chosen.

Jan 1, 1943

"Located on the Big Hole River, three miles from Divide, Montana, and 21.75 miles from Butte.Built in 1899.DAM: Rock-filled wooden crib, 512 ft. long and 57.5 feet high.SPILLWAY: Equipped with flash-boards 189 ft. long, 8 ft. 10 inches high.PENSTOCKS: Two 8 ft. diameter of steel, each branching and supplying two wheels.WHEELS: Four double horizontal, double discharge turbines, made by The James Leffel & Co., 1,000 h-p., 180 r. p. m., direct connected to generators, operating at 60 ft. head. GENERATORS: Four G. E., revolving field, 750 k-w., 180 r. p. m., 800 volt, 3 phase, 60 cycle alternators.EXCITERS: Two water-wheel driven exciters.TRANSFORMERS: 12 250-k-w. G. E. air blast, primary 15,000 volts, Secondary 800 volts.OPERATION: The plant operates essentially as a peak load plant. Except in flood period, there is insufficient water to operate at full load continually. In December its average output is about 500 k-w."

Jan 1, 1913

By S. Marion Tucker

THE aggregate number of "papers" read within any one year before more or less bored and bewildered audiences is simply appalling. We have seventy to eighty engineering societies alone, not to speak of the many hundreds of societies of every other imaginable kind. And each meets at least once a year to tell what it has found out since the last meeting. All this is very fine and fortunate, at least in the case of the scientific and technological societies; for if even only one significant discovery, one new truth, one new idea comes out at the meeting, the session has been abundantly justified. To many of us, not scientists or technologists, the scientific and technological societies seem to release by far the most useful and important information. What they have to say is often of prime importance directly to human life and to industry, and is perhaps even more important indirectly in its final influence upon social and economic conditions, thus ultimately determining the course of what we like to call civilization. The paper read by that quiet, unpretentious man on the platform ma; mean the revolutionizing of a great existing industry, the creation of an entirely new industry, the gain of millions of dollars to some persons, the loss of millions to others. But, lamentably,

Jan 1, 1940

By A. H. Daane, B. J. Beaudry

The yttl-irtm-nickel system has been investigated by metallo-graphic, thermal ard X-ray methods. There are nine intermetal-lic compounds present: Y3Ni, Y3Ni,, YNi,, YNi,, Y,Ni,, YNi,, and Y,Nil, which rodergo peritectic decomposition and YNi and YNi, which melt congruently. There are eutectics at 34.8, 57.5 and 93.3 at pct Ni which melt at 805°, 950 and 1285 C, respectively. Crystallographic data are given for YNi, YNi,, YNi,, YNi5and Y,Ni,. The terminal solid solubility is low. In recent work by Fisher and Fullhart' in which yttrium crucibles to be used for containers of uranium-chromium eutectic were clad with a high nickel steel, a low melting phase formed where the yttrium was in contact with the steel. To investigate the cause of this phenomenon, Daane, et al. made a survey study of yttrium systems with chromium, manganese, iron, and nickel and found an 18 wt pct Ni (weight percent) alloy to melt at approximately 950°C. voge13 in a study of the systems of cerium, lanthanum, and praseodymium with nickel found six compounds of the same formula in each system, i.e., R3Ni, RNi, RNiz, RNi3, RNi4, and RNi5. Since there is a great similarity between yttrium and the rare earths, compound formation was likely to occur also in the yttrium-nickel system. voge13 observed that the ability of transition metals to form compounds with the rare earths diminishes in the order nickel, cobalt, and iron while no compounds are formed with manganese, chromium, and titanium. Available data on yttrium systems with these elements indicate similar behavior, except that a slightly greater tendency toward compound formation is apparent. Simple eutectics with limited solid solubility have been found in the yttrium-titanium4 and yttrium-chromium5 systems, but at least one compound is present in the yttrium-manganese system.' In the case of yttrium-iron, at least three compounds are present,5 while only two are present in the cerium-iron,' and no compounds are present in the lanthanum-iron5 system. On the basis of both the trend in the alloying behavior of yttrium and rare-earth metals with the first transition series metals and the large number of compounds in the cerium-nickel system, one might expect six or more compounds to form in the nickel-yttrium system. A consideration of Hume-Rothery's rules of alloying based on size factor, electronegati-vity, and valence predicted low terminal solid solubility and possible compound formation. The present study was undertaken to confirm these predictions of

Jan 1, 1961

By Keith Leonard Sutherland

THIS paper is a study of the differential flotation of the sulphide minerals in the presence of salts of silver, lead and zinc. In practice, accidental activation due to these salts is more important than their use as reagents to replace copper sulphate. The general method of investigation has been based upon contact tests, the temperature of 35°C. being chosen in conformity with earlier work. Potassium ethyl xanthate and potassium amyl xanthate were selected as collectors and pure sulphide minerals were used. The experimental procedure has been outlined in earlier papers and all solutions were kept carbonate -free.1,4 Contact, or spreading of an air bubble, at a mineral surface indicates the presence of an adsorbed collector film. PURITY OF REAGENTS The xanthates were purified in the usual manner.1 Neither the cyanide nor the sodium hydroxide solutions contained sufficient carbonate to give a precipitate with barium chloride solution. The silver sulphate was prepared from pure silver nitrate by evaporation with concentrated sulphuric acid until there was no evidence of brown fumes. This solution was diluted and the difficultly soluble sulphate washed with water so that unchanged nitrate was dissolved. The resultant crystalline powder was pure white. The lead and zinc salts were prepared by dissolving especially pure lead and zinc in C.P. nitric and sulphuric acid solution and the crystals drained. The standard solutions were checked by titration. It was felt desirable to use the sulphate radical wherever possible, but since lead sulphate was insufficiently soluble for the purpose of the experiments, it was necessary to use some other lead salt. A.R. copper sulphate was used without further purification. RESULTS The results are presented in the accompanying figures; the areas of noncontact (nonflotation) are shaded in Figs. 8, 9, 10 and 11; in the remainder they lie to the right of the curve. Zinc Sulphate The curves in Fig. I are to be compared with those for Fig. 2, for which zinc sulphate is absent. This comparison shows that the influence of the zinc ion is usually small. Its influence is more marked, however, for chalcopyrite in the absence of cyanide. The influence of zinc sulphate is also marked for copper-activated sphalerite, for which tests were made only in the absence of cyanide. The results are of importance in the separation of pyrite from copper-activated sphalerite when, zinc sulphate is added in the lead flotation section (p. 204 of ref. I). Sphalerite does not adsorb the collector (i.e., become floatable) under the conditions chosen.

Jan 1, 1942

By R. Adair, W. R. Hudspeth, W. T. McDaniel

D. C. Ralston (U. S. Bureau of Mines, Washington, D. C.)—Flake mica can be beneficiated by a wider variety of methods than almost any known mineral. However, most of these methods are not recorded. It is therefore a pleasure to find a written record of another application of a new method of beneficiation. The fact that the Humphries spiral gives a concentrate containing the mica flake mixed with the slime and small grit has forced a further separation by screening, in which the finest of the flake will pass through. Fine flake has its uses and if mixed with slimes or clay is recoverable reliably only by flotation. This loss must be charged against the spiral. On the other hand, the new muscovite mica paper recently brought out by General Electric Co., can be made only with grit free flake larger than 50 mesh. It is of interest to learn from the authors whether the washing of the flake on a 50 mesh screen can take the grit content below 1 pct, to meet this new demand. Must another degritting process be used on the flake, like electrostatic treatment of the dried material? H. D. Snedden (The Humphreys Investment Co., Denver)—When recovering mica in the spiral, gangue particles coarser than 16 mesh can be rejected more readily when operating at a high pulp density (35 pct solids) or a low volume rate (—15 gpm). A launder screen as used by Lehigh Coal Co. has proved very satisfactory to partially dewater the mica concentrate and to reject any gangue slimes it may contain. Under certain conditions mica cleaning in the spiral can be improved by reagentizing the spiral feed, the object being to insure wetting of the gangue minerals and to agglomerate or prevent wetting of the mica particles. R. B. Adair (authors' reply)—The grit content of the mica recovered on Humphreys Spirals varies with the fineness of the launder screen used to clean the mica product. Normal practice has been the use of 80 mesh screen, which will produce a mica product of acceptable grit content for most purposes. By using a 50 mesh screen, and increasing the screen area per ton of feed, it is felt by the authors that a mica of 99 pct plus purity could be obtained. This statement would hold only in the case of mica feed which was well de-laminated, and free from "clay balls," (semikaclinized feldspar), which tends to follow the mica through the process.

Jan 1, 1952

By H. T. Green, R. M. Brick

True stress-strain data on alloys of pure iron with up to 2.4 pct Al were obtained in the temperature range +100° to —185°C. Alumi-num was found to reduce yield and flow stresses of iron at low temperatures but to have little or no effect on ductility. The effects of temperature and composition on strain hardening are discussed. SEVERAL independent studies of the behavior of high purity iron binary alloys at low temperatures are now in progress in attempts to evaluate systematically the variables affecting the low temperature brittleness of ferritic steels. This paper reports the results of one such investigation in which the tensile properties of aluminum and aluminum plus silicon ferrites were measured from 100" to —192°C. True stress-natural strain data have been obtained in order to evaluate as many as possible of the parameters which describe the behavior of the materials involved. In comparable studies at the National Physical Laboratory in England, iron and iron alloys of high purity have been produced' and tested at subat-mospheric temperatures.' True stress-natural strain curves were obtained there also. The purest iron contained 0.0025 pct C and 0.001 pct O and N. Even this, as normalized at 950°C following hot rolling, showed little ductility at -196°C. The grain size was ASTM No. 3, and the room-temperature yield strength was 17,800 psi (which seems too high for pure iron). Some of the NPL irons contained considerably more oxygen and demonstrated intergran-ular fracture at —196°C. The authors2 carefully differentiated between intergranular fractures associated with excessive oxygen content and transcrys-talline cleavage with little ductility encountered at —196°C in the purer material. The cleavage stress was half again as great as that associated with inter-granular fracture. Test Material, Preparation, and Procedures Of a number of Fe-A1 alloys produced, eight were considered to be sufficiently pure for testing. Partial chemical analyses (Table I), low observed yield points, and high ductilities indicate these alloys to be comparatively pure for vacuum-melted irons of sizable ingots, 5 Ib or more. To produce the binary Fe-A1 alloys, electrolytic iron was melted in air, cast into slabs, and rolled to strips 0.010 in. thick. These strips, joined into a continuous ribbon and wound into 2 1/2 in. diameter spools, were subjected for four weeks to a moving atmosphere of purified dry hydrogen in a stainless-steel tube at 1050" to 1150°C. Charges of these spools were melted in beryllia crucibles under good vacuums (1 micron), and aluminum (99.97 pct Al) was added to the melts. Compositions of these alloys are recorded in Table I. The ingots were hot forged and then cold rolled at least 65 pct to 3/8 in. rods which were vacuum annealed to the desired grain size, approximately ASTM No. 4, prior to machining into tensile test bars. All tensile specimens had gage sections 1 in. long, with a fillet of 1.5 in. radius to the shoulder. Gage diameters were 0.250 in, except for a few rods where additional cold work required use of a 0.200 in. gage section. After machining, 0.002 in. was removed from the gage diameter using 240, 400, and 600-grit metallo-graphic papers. The final polish with 600 grit left the fine scratches running in the longitudinal direction. By this means, surface metal strained during machining was removed. A few specimens heat treated after machining were similarly reduced 0.004 in. to remove any material affected chemically by the atmosphere during heat treatments, as is discussed in a later section. Tensile tests of the eight alloys at constant temperatures from +100° to —185°C were performed in apparatus which has been described." The essentials include a double-walled insulated metal vessel which contained the liquid heat-transfer medium surrounding the test specimen. A constant temperature was maintained by means of a pyrometer which regulated the pressure of dry air driving liquid air through a copper coil. Temperature variation was less than ±2°C during a specific test. For axial straining, two lengths of case-hardened chain, terminating in simple shackles, loaded the specimen through threaded grips. The lower grip bar passed through a hole in the bottom of the test vessel to which it was joined by a thin-walled

Jan 1, 1955

By Lane Mitchell

A ceramic product or processed material is a solid composed of materials which have been subjected to heat above 875°F. The raw materials, which are blended together (or in some cases used singly), are selected and utilized for various reasons such as ease of fabrication, aid to processing, to yield desired properties after processing, lack or controllable degree of toxicity or hazard, availability, cost, and perhaps other considerations. Almost all solid inorganic, some organic, and some liquid and gaseous materials have the potential to be used individually in some ceramic product. There are several fundamental functions to be fulfilled in every ceramic product and a number of secondary functions are desirable in specified products. These functions are generally met by the most widely occurring minerals and rocks of the earth and their debris. This fact characterizes ceramics as a field utilizing the raw materials most available to man. Of course, specified products utilize synthetics, organics, and rare inorganics to produce desired results. Any solid nonmetallic product processed by subjection to temperature above a red heat may be called a ceramic product. Widely used construction materials and units, domestic utensils and units, industrial parts to facilitate manufacture, technical components, and aesthetic creations are very often of a ceramic nature because of the durability, inertness, hardness, ease of fabrication, cost, and availability of the ingredients. Often, organics or metals cannot meet desired specifications for some of these products. The rocks and minerals and mineral debris of the earth are largely siliceous. Oxygen and silicon comprise roughly 75% of the earth's crust with aluminum, iron, calcium, and the alkalies following in abundance. Silica ( SiO, ) and silicates can be melted to form glasses. Alumina (A1,0,), present in a mineral com- pound, gives greater durability, hardness, and strength, but lessens the glass-forming property. Iron, calcium, and the other alkalies flux silica and reduce melting points. Thus, sand, which is generally almost pure SiO,, and clay, which is generally hydrated alumina silicate, are the most widely used of all ceramic raw materials-principally because of the glass-forming propensities of silicates. In ceramic formulations, clay is generally a refractory filler or skeletal material, having in the raw state a plasticity derived from its colloidal grain size and its water-loving nature. On the other hand, silica sand is a glass former or nonplastic filler. Clay and silica sand in pure forms are quite refractory, i.e., not easily melted. Clay, although siliceous, is less of a glass former than pure silica and is more refractory. Natural contaminants, such as iron oxide or limestone, adulterate many clays and some sands. These contaminants act as fluxes and reduce the fusion points of the mineral or blends. Glass is made from silica sand by fluxing the sand with strong bases, usually soda ash and limestone. Red building bricks are hard and durable because the sand and clay have been partially fused with help of natural iron oxide serving as a flux. The iron oxide per- forms a dual function, serving as a pigment as well as a flux. In a blend of clay and sand and iron oxide, the sand is more susceptible to fusion than is the clay. Although silica sand and clay are the most widely used raw materials in most ceramic products, many other minerals, and some non- minerals are utilized in products where these materials can produce or aid in achieving desired results. Limestone and dolomite, feldspars, pigmentary minerals, refractory oxides or carbides, and special property producers can

Jan 1, 1975

By John Wulff

In a previous paper Burwell and Wulff1 have shown by electron diffraction studies that allotropic transformations can be induced in 18-8 stainless steel by polishing to a depth of about 5 X 10-5 cm. The development of a successful etching technique, which removes accountable amounts of metal from the surface without pitting and without changing the root-mean-square profile as measured with an Abbot pro-filometer, led to the application of the whole technique and material to an investigation of various mechanical methods of surface preparation, such as grinding, lapping, superfinishing and cold-rolling. Ideally suited to such a study is 18-8 of low carbon and nitrogen content. The material can be heat-treated to produce a coarse-grained single-phase structure. On cold deformation there occurs not only a reduction in grain size but, at regions of maximum stress, a change of face-centered material to body-centered material, provided the metal is worked below about 200°C. When worked between 200"about and 415°C., diffraction studies evidence a reduction in grain size without the appearance of any new body-centered ferrite. Ferrite, which can be referred also to strains induced by carbide precipitation, is evident when the material is worked at temperatures between 4150 and 800°C. Stainless steel is advantageous because the usual surface-finishing operations do not readily oxidize it to any appreciable depth. In order to produce detectable oxide films on the surface of austenitic 18-8 in a time equivalent to that required to produce, for example, a fine ground finish on 1/2 sq. in., the sample must be held in a furnace or oxygen stream above 600°C. By using longer heating times, it is possible to achieve measurable oxide films on samples , whose surface temperatures exceed only about 250°C. Experimental Procedure The apparatus, material, and technique described in the previous paper1 were employed in this investigation. Samples of 18-8, I by I cm. by 4 mm., were carefully annealed in the austenitic range to produce a coarse-grained structure. They were then quenched and pickled to remove scale, On a lapping machine of the Graton2 type, both sides of each sample were polished to a a of 1/6 a wave length of sodium D light. Thereafter they were electrolytically etched to remove at least 1 X 10-3 cm. of the surface, a depth that is well below that of any defermations induced by surface preparation. samples of this material, carefully mounted in steel holders, were then sent to various industrial organizations known for special finishing techniques. In the instrue ment shops at the Massachusetts Institute of Technology check samples were finished by the same methods, as far as they were available. Abbot profilometer3 readings Were made on all the samples, which were then carefully degreased in double distilled benzine and alcohol, dried in a hot-filtered air blast, and kept in a desiccator. SUC-

Jan 1, 1941

By John Wulff

In a previous paper Burwell and Wulff1 have shown by electron diffraction studies that allotropic transformations can be induced in 18-8 stainless steel by polishing to a depth of about 5 X 10-5 cm. The development of a successful etching technique, which removes accountable amounts of metal from the surface without pitting and without changing the root-mean-square profile as measured with an Abbot pro-filometer, led to the application of the whole technique and material to an investigation of various mechanical methods of surface preparation, such as grinding, lapping, superfinishing and cold-rolling. Ideally suited to such a study is 18-8 of low carbon and nitrogen content. The material can be heat-treated to produce a coarse-grained single-phase structure. On cold deformation there occurs not only a reduction in grain size but, at regions of maximum stress, a change of face-centered material to body-centered material, provided the metal is worked below about 200°C. When worked between 200"about and 415°C., diffraction studies evidence a reduction in grain size without the appearance of any new body-centered ferrite. Ferrite, which can be referred also to strains induced by carbide precipitation, is evident when the material is worked at temperatures between 4150 and 800°C. Stainless steel is advantageous because the usual surface-finishing operations do not readily oxidize it to any appreciable depth. In order to produce detectable oxide films on the surface of austenitic 18-8 in a time equivalent to that required to produce, for example, a fine ground finish on 1/2 sq. in., the sample must be held in a furnace or oxygen stream above 600°C. By using longer heating times, it is possible to achieve measurable oxide films on samples , whose surface temperatures exceed only about 250°C. Experimental Procedure The apparatus, material, and technique described in the previous paper1 were employed in this investigation. Samples of 18-8, I by I cm. by 4 mm., were carefully annealed in the austenitic range to produce a coarse-grained structure. They were then quenched and pickled to remove scale, On a lapping machine of the Graton2 type, both sides of each sample were polished to a a of 1/6 a wave length of sodium D light. Thereafter they were electrolytically etched to remove at least 1 X 10-3 cm. of the surface, a depth that is well below that of any defermations induced by surface preparation. samples of this material, carefully mounted in steel holders, were then sent to various industrial organizations known for special finishing techniques. In the instrue ment shops at the Massachusetts Institute of Technology check samples were finished by the same methods, as far as they were available. Abbot profilometer3 readings Were made on all the samples, which were then carefully degreased in double distilled benzine and alcohol, dried in a hot-filtered air blast, and kept in a desiccator. SUC-

Jan 1, 1941

By J. E. Schiller, S. E. Khalafalla

To improve technology for treating process water, US Bureau of Mines research has shown that magnesium oxide (MgO) has many advantages over lime or caustic soda for precipitating heavy metals. Sludge produced by MgO occupies only 0.2-0.3 times as much volume as the precipitate made wing a soluble base. While a settled, lime-formed precipitate is easily resuspended, the MgO-metal hydroxide sludge becomes cemented together on standing. Settling of the metal hydroxides from a dilute suspension is more complete than precipitates formed with other bases. Virtually any metal that can be precipitated by raising the pH can be treated using MgO. A three fold to fourfold stoichiometric excess of solid reagent is added. The mixture is reacted for five to 10 minutes. Polymer is added, and settling or filtration completes the process. Because of the greater cost of MgO compared with lime, large-scale practice of this technology will probably be limited to water containing 50 mg/L (3 gr per gal) or less of dissolved metals. For such dilute solutions, chemicals are not a large fraction of total treatment costs, so more desirable sludge properties might justify higher chemical expenses. While the MgO process is technically suitable for widespread application, the extent to which it is adopted will probably be determined by a trade-off between the greater cost of MgO compared with lime and the superior properties of the precipitates and their corresponding ultimate disposal costs.

Jan 1, 1985

By John Wulff

IN a previous paper Burwell and Wulff1 have shown by electron diffraction studies that allotropic transformations can be induced in 18-8 stainless steel by polishing to a depth of about 5 X 10-5 cm. The development of a successful etching technique, which removes accountable amounts of metal from the surface without pitting and without changing the root-mean-square profile as measured with an Abbot profilometer, led to the application of the whole technique and material to an investigation of various mechanical methods of surface preparation, such as grinding, lapping, superfinishing and cold-rolling. Ideally suited to such a study is 18-8 of low carbon and nitrogen content. The material can be heat-treated to produce a coarse-grained single-phase structure. On cold deformation there occurs not only a reduction in grain size but, at regions of maximum stress, a change of face-centered material to body-centered material, provided the metal is worked below about 200°C. When worked between 200° and 415°C., diffraction studies evidence a reduction in grain size without the appearance of any new body-centered ferrite. Ferrite, which can be referred also to strains induced by carbide precipitation, is evident when the material is worked at temperatures between 415° and 800°C. Stainless steel is advantageous because the usual surface-finishing operations do not readily oxidize it to any appreciable depth. In order to produce detectable oxide films on the surface of austenitic 18-8 in a time equivalent to that required to produce, for example, a fine ground finish on ½ sq. in., the sample must be held in a furnace or oxygen stream above 600°C. By using longer heating times, it is possible to achieve measurable oxide films on samples whose surface temperatures exceed only about 250°C. EXPERIMENTAL PROCEDURE The apparatus, material, and technique described in the previous paper1 were employed in this investigation. Samples of 18-8, 1 by 1 cm. by 4 mm., were carefully annealed in the austenitic range to produce a coarse-grained structure. They were then quenched and pickled to remove scale. On a lapping machine of the Graton2 type, both sides of each sample were polished to a flatness of 1/6 a wave length of sodium D light. Thereafter they were electrolytically etched to remove at least 1 X 10-3 cm. of the surface, a depth that is well below that of any deformations induced by surface preparation. Samples of this material, carefully mounted in steel holders, were then sent to various industrial organizations known for special finishing techniques. In the instrument shops at the Massachusetts Institute of Technology check samples were finished by the same methods, as far as they were available. Abbot profilometer3 readings were made on all the samples, which were then carefully degreased in double distilled benzine and alcohol, dried in a hot-filtered air blast, and kept in a desiccator. Suc-

Jan 1, 1941

By Herbert H. Kellogg

C. M. Decroly (University of Brussels, Belgium) — The importance of the fluorides in the process metallurgy of special metals has already been accepted and it will probably increase in the future. Free energy diagrams as such established by Professor Kellogg are therefore very useful. It is interesting to note that the absolute value of the standard free energy of formation of HF increases with temperature, whereas for almost all the other fluorides it decreases; consequently it should be theoretically possible to reduce all the fluorides of the metals which, at low temperature, have a greater affinity for fluorine than hydrogen by this last element, provided a sufficiently high temperature is used in order to have a good efficiency. However, with regard to the reduction of UFe by hydrogen, I doubt that it will be possible to obtain directly the metal at comparatively low temperatures. There are other uranium fluorides which are more stable than UF6 and it is very likely that such fluorides will be obtained first. For example, in considering the reaction: UF6gas + H2gas + UF1so1id + 2 HFgas it is found, using the thermodynamic data of Brewer et al, that ?H298 = —66 kcal and ?G°298, = —65.2 kcal. As a result, the reduction of UF6 to UF4solld should proceed spontaneously even at ordinary temperature. On the other hand, the standard free energy of formation of UF4solid at 298°K is AG°298 = -209 kcal per mol of F2. The reduction of UF4 by hydrogen will be practically difficult and, as it is known, the only practical way of reducing this compound is to use alkaline-earth metals such as calcium or magnesium. I should like to point out, further, that the fluorination of many metal oxides can be carried out very easily by using the ammonium difluoride method of preparation, which renders the use of fluoride gas unnecessary. The first compound formed is generally a double fluoride of the metal and ammonium. This compound can be decomposed by heating either in a vacuum or in an inert atmosphere, ammonium fluoride being volatilized leaving the metal fluoride in a very pure state. H. H. Kellogg (author's reply)—Professor Decroly is quite right in pointing out that the formation of lower halides of uranium may complicate the reduction of UF6 by H2. I was unable to find his reference to the free energy of formation of UF4 in the compilation of Brewer.13 however. The value of AG°298, = —209 kcal for formation of ½ UFa seems rather high, and I hope the source of this value may be made clear.

Jan 1, 1952

By H. J. Stehli

Probably the earliest sinter from lead ore was made in the product sinter boxes attached to some hand reverberatory roasters. The ore was drawn from the roaster bed when dead roasted, and then by laborious effort fritted together by rabbling at a high temperature in the sinter box. This was not a true sinter, but was a great improvement over the dusty dead-roasted fine ores. The Huntington-Heberlein pots were the first real advance in the art, and produced some real sinter. They required that the sulphides be preroasted to 5 or 6 per cent sulphur, and the long cycle of operating and deep bed of material used in the pots fostered the formation of densely fused material and fines. This necessitated crushing of the densely fused cake and returning to the next charge large amounts of fines screened out. The Huntington-Heberlein pots made comparatively high lead losses because the deep bed and high internal temperature together favored the volatilization of lead. Lime (CaO) was added to the charges, and this addition constituted the patented feature of the Huntington-Heberlein process. Its sole function we now know was to act as an isolator of the sulphide particles, and any other substance—for instance, iron oxide—of equal fineness performed the same function. The Savelsberg process used limestone instead of burned lime, and in this there was a definite advantage. The converting of CaCO3, to CaO is a highly endothermic reaction, so the lime acted not only as an isolator of sulphide particles but absorbed excess heat and to some extent prevented premature fusion of the sulphides. The Carmichael-Bradford process used gypsum instead of limestone, and had the disadvantage of adding more sulphur to a charge from which it was desired to eliminate sulphur. Here again the gypsum served only as an infusible isolator of sulphide particles. The first Dwight-Lloyd apparatus to sinter lead ores commercially was installed at Perth Amboy in 1907. The fact that lime in any form was necessary to sintering was quickly disproved by making excellent sinter from Bunker Hill and Sullivan table concentrates, silica sand and iron oxide only.

Jan 1, 1937

By N. A. McLeod

BALL wear in wet grinding mills has been the subject of considerable discussion in the last few years. Its importance to millmen is obvious in view of the fact that ball wear may cost from 2 to 4¢ per ton of ore for the more fortunate operators and many times this cost when a refractory ore must be reduced to a fine state of comminution. Consequently, any factual information that may be obtained on the nature of ball wear may be applied to introduce changes leading to lower ball consumption and therefore also to lower costs. In 1940, while employed with the Britannia Mining and Smelting Co., Britannia Beach, B.C., I had occasion to investigate factors that might affect ball consumption. We performed a number of tests, which will be briefly described. These tests originated as a result of changing from a 3 1/2-in. ball to a 2-in. ball of different type of manufacture and were motivated by the desire to obtain the best possible type of 2-in. ball. Our testing was helped by the fact that the company operated a one-ton electric furnace, so that it was quite easy to make steel changes. It should be emphasized at the beginning that these tests produced results that in their general application to milling should be interpreted qualitatively rather than quantitatively. As will be evident in the description of the method used in testing, the balls were subjected to an intermittent batch grinding treatment, which may have produced results in rate of steel wear that may not have an accurate correlation with steel consumption in full-scale mill operation. However, with this fixed and rather arbitrary method of testing, results were obtained that may be of some interest and may stimulate further work on this subject. Unfortunately, owing to pressure of war work, our tests, which we had intended to repeat on a continuous grinding operation, had to be discontinued. METHOD OF TESTING Tests were made in a small cylindrical mill, rotating at 72 r.p.m. Internal dimensions of the mill were 10 1/2-in. dia. by 9 in. The cylindrical inner surface was lined with rubber and the two ends were formed by steel plates. A charge of 2000 grams dry feed and 2000 c.c. of water was added every 2 hr., the mill being drained of pulp before the addition of each charge, by tilting and sluicing with water. The mill was run on afternoon and night shift for daily periods of about 15 hr. total grinding time, and each test lasted from 60 to 150 hr. This batch method of testing involved a higher average pulp temperature in the mill, which undoubtedly affected comparative results in some of the tests. HARDNESS OF BALL VS. WEAR In these tests, special "eutectoid" steel balls were used, some of which were chill-cast and quenched, some sand-cast and quenched, and some sand-cast and annealed to a dead soft condition. The results obtained, using as mill feed an ore containing considerable free quartz and

Jan 1, 1945

By J. Gross

G. H. Clevenger, Chairman of the Milling Methods Committee of the Institute, made the following introductory remarks: "Several years ago, a number of us felt that the time was ripe for a fundamental investigation of crushing and grinding. At the outset, it appeared that the first thing we needed was a yardstick whereby grinding efficiency could be measured. "The U. S. Bureau of Mines has been most generous in cooperating with the Milling Methods Committee in getting this work well under way. John Gross, who served the committee for a year as secretary, was placed in charge of the investigation and has been ably assisted by S. R. Zimmerley. "Messrs. Gross and Zimmerley will now present the Progress Report covering their work to date." PROGRESS REPORT J. Gross, Salt Lake City, Utah. -This has not been a simple problem, and when I tell you that we can give you a verbal report of what we have done during three years in five or ten minutes you will realize that we have necessarily done a great deal of work that does not appear in the final results. We have been in a virtually new field. Therefore, we have had to feel our way at each step so as to be fairly sure we were correct. The first thing that was realized in this problem was that unless we had some method of measuring what happened when we crushed an ore, we might as well quit and not go further. We realized that if we tried to measure the results of crushing or grinding by the ordinary sizing test we would not get anywhere. We could sieve down to say 200 mesh fairly accurately; we could even go one sieve size further with a little less accuracy, and then we were absolutely lost, unless we went into microscopic measurement. Even this latter method would not have been satisfactory. The question was: what were we going to measure? If we were going to measure size, we might measure one particular dimension of a particle and be off 200 per cent. or more. If we tried to measure surface, we would have something tangible; the surface of a particle, no matter how irregular, is something definite, far more definite than any linear dimension would be. Moreover, if we could measure surface, we would immediately have a method of checking the Rittinger law as to whether it was or was not correct. So the first thing that we sought was a method whereby we could measure surface on crushed particles or, we will say, on particles; it would not make any difference whether crushed or not. It then became a question of what kind of particles we were going to use in obtaining a method for surface measurement. We realized that it would be rather a com-

Jan 1, 1928

By E. H. Snow, B. E. Deal

Instability effects in semicanductor devices have long been attributed to the motion of charges on or within oxide layers on the surface. These effects are of critical importance in metal-insulator-semiconductor MIS) field-effect devices. For this reason, the capacitance-voltage or the conductance-voltage characteristic of these devices can be used as a sensitive detector to study charge transport and polarization effects in the oxide or insulator. A review is given of the results of such studies of thermally grown SiO2 as well as of other insulating films of importance in silicon technology. Three types of effects are distinguished. The first of these is the drift of mobile cations within the dielectric, examples being thermally grown SiO, which is often contaminated with sodium ions, and a variety of other glasses in which the mobile ions are a part of the glass composition. The second effect is a dipole-type polarization which occurs in phosphosilicate glass films obtained by reacting P2O5 with thermally grown SiO2. The third effect involves the transfer of charges between the dielectric and the silicon electrode. This occurs in silicon nitride and other deposited dielectrics. It is concluded that MIS studies have provided a powerful technique joy the study of charge transport and polarization effects in insulating films. The knowledge gained from these studies has led to an understanding of surface effects on conventional transistors and diodes as well as making possible stable MIS transistors. THE metal-insulator-semiconductor field-effect transistor is conceptually the oldest type of active semiconductor device.' The earliest attempts at making this device were frustrated because of high surface state densities at the interface between the semiconductor and the gate insulation.' However, by using a silicon substrate with thermally produced silicon dioxide as the gate insulation, this problem was solved and metal-silicon dioxide-silicon devices with good characteristics were made as early as 1960. 3 Yet it was still over 5 years before these devices became a commercial reality. This delay was largly due, not to surface states, but to stability problems associated with polarization effects within the insulating layer which caused the threshold voltage of the device to drift under temperature and bias treatments. The solution to these problems has not only made possible stable MIS devices, but it has added immensely to our understanding of failure mechanisms in conventional bipolar transistors and has added to the reliability of ali types of planar devices. In this review, we shall first describe the effects of various types of polarization phenomena on MIS device characteristics. Then, since thermally grown SiO, is by far the most important insulator used in these devices, we shall review historically the type of instabilities which have been observed in thermal oxides, the attempts at understanding and eliminating them, and the present status of the problem. We shall then turn our attention to the various deposited insulators which have been used, including lead glasses, phosphosilicate glass, vapor-deposited silicon oxide, and silicon nitride. Interestingly enough, many of these materials show polarization effects which are quite different from those generally observed in thermally grown SiO2. THE EFFECTS OF POLARIZATION PHENOMENA ON MIS CHARACTERISTICS The simplest MIS device and the one which has been most frequently used in the study of polarization effects is the MIS capacitor. Two modifications of this structure with single- and double-layer dielectrics are illustrated in Figs. l(a) and (b), respectively. The capacitance of this structure as a function of voltage applied to the metal gate electrode is plotted in Fig. 2 for the case of an n-type silicon substrate. When the silicon surface is accumulated (positive bias) the measured capacitance is just that of the insulating layer C. When the surface is inverted (negative bias), the capacitance is that of the insulator and a silicon depletion layer in series CoCs/(Co + Cs). Indicated on the horizontal axis of Fig. 2 is the voltage VT at which the silicon surface becomes strongly inverted. This voltage corresponds to the threshold or turn-on

Jan 1, 1969

By J. M. Camp

In conforniity with the design of the oficials of the United States Steel Corporation for the standardization of the methods employed in the sampling and analysis of all materials encountered in their various lines of manufacture, the Chemists' Committee presents this compilatioti of standard methods for the sampling and subsequent analysis of molten pig-iron. In selecting the methods, the Committee employed the same line of procedure as in former cases, viz., the careful consideration of all the methods employed in each laboratory of the Corporation, evolving therefrom the several methods herein described, the immediate adoption of which is desired. The services of Messrs. W. B. N. Hawk, William Brady, and C. H. Rich, a sub-committee appointed for the preparation of the present paper, are gratefully acknowledged. II. Introduction. A quite obvious cause of nonconformity of results of comparative analyses in the various laboratories of the Corporation has been an apparent lack of uniformity of method in the sampling and analysis of molten iron. This condition is particularly apparent with regard to the determination of the sulphur, numerous discrepancies in which would appear t.o indicate the absence of, and the necessity for, some uniform method of procedure. The estimation of the

Jan 1, 1913

By S. WHINERP

(Cleveland Meeting, October, 1912.) I AM indebted to L. E. Bryant, of Danville, Ky., President of the Virginia Mining Co., operating coal-mines in Scott county, Tenn., for the following information relating to the existence of the Clinton iron-ore under the NW. slope of the Cumberland Plateau in Kentucky and Tennessee. During the past 15 years quite an important oil-field has been developed in a region having Wayne county, Ky., as its center, and a large number of wells have been drilled in that and adjacent territory in the search for oil. Many of' these wells have been carried to considerable depths below the recognized oil-bearing horizon, and one of them was drilled by Mr. Bryant at Pine Knot, a station on the Cincinnati, New Orleans & Texas Pacific railroad, a few miles north of the point where that road crosses the Kentucky-Tennessee State-line. The elevation of the surface at the crossing is about 1,400 ft. above sea-level. The railroad is located on the dividing ridge between the Cumberland river and Big South Fork. At a depth of 1,720 ft. below the surface the drill reached and passed through a formation which the drillers called " red rock," but which Mr. Bryant classified as Clinton iron-ore, as its geological position corresponded to that formation. The ore at this point was 6 ft. thick and appeared to be of uniform quality throughout. An analysis of the drillings gave : Fe, 33; Mn, 0.25; Si02? 3 ; Al203, 2 ; CaO, 13; MgO, 7 ; P,05, 0.333 per cent. ; S, trace. This analysis seems to confirm the belief that the ore is Clinton, and that it is of a quality equal to the average of the deep or unbleached Clinton ores in Tennessee and Alabama. This discovery led Mr. Bryant to make further examinations and inquiries, and he found that the stratum called " red rock " by the drillers had been passed through and noted in the great majority of the wells carried down to the same geological hori-

Oct 1, 1912

By R. P. O’Shea

AS part of a program to investigate phase relationships in ternary systems containing semiconducting elements and compounds, an X-ray survey of alloys in the system Pb-Te-Bi was carried out which revealed that the pair PbTe-Bi probably formed a quasibinary system. This portion of the ternary was examined fully by thermal analysis, X-ray, and microscopic procedures. More than twenty-five alloys were made by melting together the proper combinations of the elements in quartz tubes at a temperature of 1000o C. The compositions which were high in PbTe content were prepared in evacuated, sealed, quartz tubes, allowed to freeze in vacuum, and then transferred to Crucibles for thermal analysis. The bismuth-rich alloys were made directly in the crucibles under a protective gas cover. The starting elements were obtained from the American Smelting and Refining Co. and had a purity greater than 99.99 pct. Cooling curves were made with about 50 g of alloy in graphite crucibles which were placed in a covered quartz container in which a protective atmosphere of helium or nitrogen was maintained. The thermocouple protection tube was made of mul-lite and served as a stirring rod when connected to a reciprocating stirring motor. Temperatures were

Jan 1, 1962