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By E. I. Larsen, E. F. Swazy, F. R. Hensel

Experience has indicated that hard bronzes are not suitable for bearing applications where high bearing loads and speeds are involved. It is the general practice to utilize softer materials for these purposes, such as copper, lead, silver, babbitt, lead-base alloys, and more recently aluminum-base alloys, preferably supported by a steel backing. It was the objective of the present investigation to study a new material produced by powder metallurgical methods susceptible to precipitation-hardening. Test MAteriaIs Preliminary tests were made with compacts containing copper, nickel and silicon in quantities sufficient to form 3 to 5 per cent nickel silicide. It mas found that this type of alloy was susceptible to the formation of a soft surface shell when sintered in tank hydrogen. The depth of the shell depended On the length of sintering time and sintering temperature, and varied in thickness from a few thousandths to as much as One eighth inch. This soft shell resulted from the preferential oxidation of silicon, thereby reducing the efficiency of age-hardening by the nickel silicide compound. The body of the sintered compacts below the soft shell could be precipitation-hardened to a hardness of 70 to 85 Rockwell B, by quenching from goo°C. and age-hardening at 450°C. A series of tests was made with various addition agents, in order to decrease the rate of preferential oxidation, and it was found that phosphorus was most beneficial in this respect. After considerable experimentation, the following nominal com-position was accepted as standard: 2.4 per cent nickel; 0.8 silicon; 0.3 phosphorus; balance copper. The physical propertties and certain bearing properties of this alloy are described in the present paper Preparation of Compacts Several methods of incorporating the hardening ingredient (nickel silicide) were studied. Compacts formed from copper, nickel and silicon powders were found to be inferior to those fabricated from prealloyed nickel silicide master alloys, because of the rapid oxidation of pure silicon during sintering. The use of a prealloyed nickel silicide hardener containing 25 per cent silicon and 75 per cent nickel could be further improved by preparing a master alloy, incorporating nickel, silicon, phosphorus and copper, having the following nominal composition~ 25 per cent nickel; 7 silicon; 3 phosphorus 64 copper. This alloy is brittle in the cast condition and can be readily powdered. Sintering Procedure The blended powders were pressed at '5 to 40 tons per sq' in., the pressure depending on the size and shape of the compacts. Sintering was carried out in hydrogen or cracked ammonia atmospheres at

Jan 1, 1946

By E. I. Larsen, E. F. Swazy, F. R. Hensel

Experience has indicated that hard bronzes are not suitable for bearing applications where high bearing loads and speeds are involved. It is the general practice to utilize softer materials for these purposes, such as copper, lead, silver, babbitt, lead-base alloys, and more recently aluminum-base alloys, preferably supported by a steel backing. It was the objective of the present investigation to study a new material produced by powder metallurgical methods susceptible to precipitation-hardening. Test MAteriaIs Preliminary tests were made with compacts containing copper, nickel and silicon in quantities sufficient to form 3 to 5 per cent nickel silicide. It mas found that this type of alloy was susceptible to the formation of a soft surface shell when sintered in tank hydrogen. The depth of the shell depended On the length of sintering time and sintering temperature, and varied in thickness from a few thousandths to as much as One eighth inch. This soft shell resulted from the preferential oxidation of silicon, thereby reducing the efficiency of age-hardening by the nickel silicide compound. The body of the sintered compacts below the soft shell could be precipitation-hardened to a hardness of 70 to 85 Rockwell B, by quenching from goo°C. and age-hardening at 450°C. A series of tests was made with various addition agents, in order to decrease the rate of preferential oxidation, and it was found that phosphorus was most beneficial in this respect. After considerable experimentation, the following nominal com-position was accepted as standard: 2.4 per cent nickel; 0.8 silicon; 0.3 phosphorus; balance copper. The physical propertties and certain bearing properties of this alloy are described in the present paper Preparation of Compacts Several methods of incorporating the hardening ingredient (nickel silicide) were studied. Compacts formed from copper, nickel and silicon powders were found to be inferior to those fabricated from prealloyed nickel silicide master alloys, because of the rapid oxidation of pure silicon during sintering. The use of a prealloyed nickel silicide hardener containing 25 per cent silicon and 75 per cent nickel could be further improved by preparing a master alloy, incorporating nickel, silicon, phosphorus and copper, having the following nominal composition~ 25 per cent nickel; 7 silicon; 3 phosphorus 64 copper. This alloy is brittle in the cast condition and can be readily powdered. Sintering Procedure The blended powders were pressed at '5 to 40 tons per sq' in., the pressure depending on the size and shape of the compacts. Sintering was carried out in hydrogen or cracked ammonia atmospheres at

Jan 1, 1946

By George B. Langford

ON THE QUESTION of postwar controls there are today three schools of though ; some advocate state control of everything the socialists ; second are those who advocate the removal of all governmental control over industry - the freedom of enterprise ideal ; and third are those who advocate a middle course - sufficient control to stabilize economic and industrial life, and to prevent violent fluctuations such as we saw in the interwar years. I advocate this third course. I firmly believe un free enterprise, but not in freedom of enterprise, or laissez faire, and there is a great and significant difference between these two.

Jan 1, 1944

By T. D. Tiemann

The chemical and mineralogical composition of Caribbean bauxite ores are described. Extraction of alumina by several processes from both Haiti and Jamaica bauxites is discussed and data presented. IMMENSE deposits of bauxite occur in the Caribbean islands of Hispaniola and Jamaica in the high plateau lands and have been excellently described by 0. C. Schmedeman.' The bauxite occurs as deposits in catchments or etched depressions in Tertiary limestone believed to have been deposited in the Eocene and Oligocene periods.' In appearance both the Haiti and Jamaica bauxites resemble a relatively high iron clay and have indeed been mistaken for such.' They are very soft and friable and disperse readily on vigorous agitation in water. The color range in general is light brown to red. Chemically, the outstanding characteristic of the bauxites is the low silica and high ferric oxide content. The extremely low silica makes them particularly valuable for the production of alumina in the Bayer plant since silica is responsible for the loss of both alumina and soda chemically combined as XNa,OYSiO2,ZAl2O2. The ferric oxide, only traces of ferrous iron are present, offers no interference in the production of high grade alumina. Typical oxide analyses of three types of ore are given in Table I2 and a list of the elements occurring in spectrographic quantities in Table 11." The size of the individual particles in the ore makes successful petrographic examination extremely difficult. The ores contain some relatively coarse grains of heavy minerals such as ilmenite, magnetite, and rutile, but other than occasional crystals of a few microns, the greater portion of the minerals are submicroscopic in size and approach colloidal dimensions. The mineralogic composition of the ores has been investigated by X-ray and differential thermal analysis.' These investigations indicate that the predominant mineral phases present are gibbsite (A1203.3H2O), boehmite (Al2O3.H2O), hematite (Fe2O3), and goethite (Fe2O3-H2O). There is no evidence of the occurrence of diaspore (Al2O3.H2O) in either the Haiti or Jamaica ores, but some type of "amorphous" alumina may be present in some of the bauxites of Jamaica." The temperature stability regions in the alumina-water system have been investigated and are given in recent literature. In the temperature range where the hydrated forms are stable, as determined by hydrothermal bomb methods," ibbsite is the stable phase to 155°C (311°F), boehmite from 155°C (311°F) to 280°C (536oF), and diaspore from 280°C (536°F) to 450°C (842°F). Although quite similar in many characteristics, the Haiti and Jamaica ore show a divergence in mineralogic composition that is reflected in the extractability of the alumina described in later paragraphs. Two principal differences occur in mineralogic composition. The iron-bearing mineral in the Haiti ores is predominantly hematite, while in the Jamaica ores goethite is predominant.4 Directly related to the extraction of alumina are the two minerals, gibbsite and boehmite. Boehmite is relatively high in the Haiti ores and in some of the less soluble Jamaica ores, while gibbsite predominates in the ores in Jamaica amenable to the American Bayer process of extraction. Pedersen and Related Processes In general, all processes for the extraction of alumina involving sintering or fusion of bauxite ores with limestone, soda ash, or a combination of limestone and soda ash followed by leaching, are based on the formation of alumina compounds that. yield alumina soluble in the subsequent leach. The principal idealized reactions in respect to alumina and silica for the three types of processes are as follows: Soda Ash Sinter: A12O3 + Na2CO3 = Na2O-Al2O, + CO2 SiO2 + Na2CO3 = Na2O . SiO2 + CO2 A12O2 + SiO2 + Na2CO3 = Na2O.Al2O8. SiO2 + CO2 Leach (with excess water): H2O + Na2O-A12O3 = 2 NaOH + A12O3 (insolution) H2O + Na2O-SiO2 = 2 NaOH + SiO2 (in solution) Soda Ash— Limestone Sinter: Na2CO2 + A12O3 = Na2O.A1203 + CO2 2CaCO3 + SiO2 = 2CaO . SiO2 + 2CO2 Leach (with excess water): Na2O' A1208 + H2O = 2NaOH + A13O3 (in solution) These latter reactions are the basis of the sinter process currently used for the recovery of soda and

Jan 1, 1952

AARONS, J. BOYD, Major. AGNEW, FRANK VANS. ALLEN, HERMAN H., Private, D Co., 8th -Reserve Engineers. BAINS, THOMAS M., Major, Engineer Officers' Reserve Corps. BANKS, H. R., Lieutenant, Canadian Engineers, B. E. F. BARBOUR, PERCY E., Deputy Supt. (Captain), New York State Troopers; Captain, 22d Regiment, N. Y. N. G. BARLING, H. B., Ist Lieutenant', Engineer Officers' Reserve Corps. BIGELOW, BRAXTON. BLOOMFIELD, E. C., Lieutenant. , BORROW, F. K. BROCK, R. W., Major, 19th Reserve Battalion of Canadians. BROOKS, ALFRED H., Captain, Engineer Officers' Reserve Corps. BROWNE, DE COURCY, 1st Lieutenant, Ordnance Dept., Fortress Monroe, Va.

Jan 9, 1917

Charles Catlett, Staunton, Virginia (communication to the Secretary*): I have had occasion to examine a few of the irondeposits in the immediate section of which Mr. Watson speaks, but have not had an opportunity to visit any of the well-known manganese-deposits. I find the former can be very safely read in light of the information which it is possible to get from the same measnres farther. north, where they are less completely decomposed. In the same way all of his conclusions in regard to the geology of the manganese-deposits bear out their occurrence in Virginia, when we allow for the far more complete decomposition in the section he has so carefully studied. Judging from the same measures farther north, I think he will be safe in agreeing even further with Penrose as to the origin of these ores. Some years ago I carried on prospecting work in these measures in Virginia, in which the iron-ore and manganese-ore were followed down to undecomposed material, and in which their occurrence along a definite line of stratification, and apparently a part of the original bedding, was plainly shown. This is unusual, however, even in the section of which I speak. At Crimora, Virginia, the decomposition is quite complete; at the same time the results of some hydraulic work, which has been done there, disclosed, at the time of my last visit, the manganese interbedded in the residual clay along a definite and distinct plane parallel to the bedding of the underlying quartzite, and which, as is shown at other points, corresponds with the plane of the original material. In view of the phosphorus reported by Mr. Watson as existing in the Cartersville ores, and the not uncommonly prohibitive amount in southern ores, I am interested to know whether

Jan 1, 1904

By ALEXANDER S. CORSUN

THE main orebody in the Hecla mine, Burke, Ida- ho, occurs along a nearly vertical shear zone in the Burke quartzite, with a substantial gouge and lamprophyre dike occurring in an irregular manner throughout the lode. The veins range from 3 to 40 ft. wide and dip from 70 deg. to 90 deg. There is 110 definite line of demarcation between the lode and the wall rock. Stringers of ore are often found in the wall rock for irregular distances. Horizontal but irregular quartz stringers are also found running into the walls and positions of the wall have a tendency to break to the quartz stringers and the accompanying gouge, which causes indefinite, uneven and extremely heavy side and top pressures.

Jan 1, 1930

By Charles Will Wright

ALTHOUGH the United States has long led all other countries in both the production and consumption of mineral products, the trend seems definitely toward an increasing dependence upon foreign sources of supply. This is not to take the position that we are either a have or a have-not nation. For years we shall continue to secure a large proportion of our needed minerals: from our own mines, but we must face the fact that this century has seen "a more thorough and intense development of the mineral resources of the United States and a greater depletion of its irreplaceable mineral reserves than has occurred in most other countries. An audit of our mineral production given in the attached charts discloses the extent of our deficiencies. Because of these facts, low-cost foreign sources offer a promising field for the investment of a portion of our mining capital and an opportunity to obtain for the United States a greater supply of strategic metals and minerals. How. ever, to reach this end, the industrialist investing in the foreign field must have the full co-operation and strong backing of the Federal Government and the involved Federal agencies.

Jan 1, 1947

By C. H. Herty Jr, C. H.

FEW subjects have attracted the attention of metallurgists more than oxygen in steel. From the days of Mushet and Ledebui interest in this subject has been increasing, and as additional knowledge has become available, the problem has naturally grown more complex. Instead of using the simple term "oxygen" we now distinguish between iron oxide, silicates of various kinds, oxysulfides, oxygen as gas and oxygen in solid solution in steel. There are five general methods for determining oxides in steel: hydrogen reduction; vacuum fusion; various wet-extraction methods, including electrolytic methods; methods depending on volatilization of the iron away from the oxides; and metallographic methods. For oxygen in solid steel each of these methods has both advantages and disadvantages. The hydrogen-reduction method is of no use on steels above about 0.20 per cent. carbon; 1 furthermore, it gives only FeO and possibly some MnO. The vacuum-fusion method2 is expensive and gives total oxygen, with the exception of some A1203, and does not differentiate between the various oxides in which the oxygen exists. Most of the wet-extraction methods3 give only the more insoluble oxides SiO2 and A1203, though the iodine method gives MnO to an uncertain degree (information that may be more misleading then no information

Jan 1, 1957

By Paul M. Tyler

HISTORICAL concepts of the economics of the glass-sand industry are changing rapidly. The greatly expanded demand for glass containers combined with higher freight rates on raw materials and manufactured products have induced a migration of glass factories toward densely populated centers and the creation of new standards of place value for sub- standard sand deposits. This migration has been facilitated by the construction of pipelines to bring cheaper natural gas and liquid fuel to large cities and may be further speeded by the adoption of modern mineral dressing methods to permit economical utilization of local raw materials. Our national resources of naturally high-grade 1 silica sand are abundant, but most of the best de- posits are situated so far from large centers of population that it now costs $3.00 to $5.00 a ton to carry the sand from the mine to the optimum site for a 1 factory making beverage bottles, scientific and electrical glassware, and miscellaneous blown and pressed ware for local markets. It follows that on the basis of freight savings alone it may be economical to use material from inferior deposits closer to the factory even though the f.o.b. cost of mining and treatment may be much high

Jan 1, 1950

SUCCESSFUL development of a new process for heat hardening of pellets made from taconite concentrates was announced by Arthur G. McKee & CO., steel plant engineering and construction firm of Cleveland, and Allis-Chalmers Mfg. Co. An order for the design, engineering, and materials for a plant incorporating the process, has been received by the McKee Co. from the Reserve Mining Co. for its new E. W. Davis Works at Silver Bay, Minn. It is estimated that this plant will cost around $19 million and when in full operation, will turn out 12,000 tons of pellets per day.

Jan 10, 1954

Discussion of the paper of R. H: Sweetser,. presented at the Cleveland meeting, October, 1912, and printed in Bulletin No. 71, November, 1912 pp. 1327 to 1334. See also Bulletin 11 No. 72, December, 1912, pp. 1561, 1562. J. J. HOWARD, Dover, N. J. (communication to the Secretary*) :-No doubt there are as many different methods of starting a blast-furnace as there are men who assume that responsibility. Having blown-in a furnace a few years ago in a manner similar to that outlined by Mr. Sweetser, things went along so well at the start that I had time for a little reflection on what was going on inside the furnace. I saw the wood turned to charcoal practically, and it occurred to me, why should I use wood when I could put in the charcoal in the. first place, and thus save a lot of time, and also eliminate the dangerous gas from the wood, which is the cause of most of the accidents in starting up a furnace. I had a furnace out for repairs and decided to use no cord-wood in blowing in. I put in about a carload of charcoal and used no wood except some shavings and oily waste at each of the tuyeres. The furnace had 16 tuyeres and was 100 by 22 by 14.5 ft. Hot rods were put in each tuyere' and the blast started immediately at 11 a.m. Within 5 mill. the air was all driven out of the stack and the gas lighted of its own. accord at the top of the furnace. It was allowed to burn for 5 min. longer and then the bell was closed and the gas taken to the last stove and the last boiler on the gas-main. It was all clone so quietly that it was hard to realize that the gas was down. The tuyeres were as bright as if the furnace had been in blast for a long time. I have learned since that others have used the same method, but they had not passed the good advice along.

Jan 5, 1913

By Robert W. Hunt

When I had the honor of presenting to the Institute at the Buffalo meeting in October, 1888 (Trans., xvii., 226), my paper on " Steel Rails and Specifications for their Manufacture," I expressed my hesitancy in submitting my ideal rail-sections. Since then, continued residence in Chicago, perhaps, or greater intercourse with railroad officials, has either given me more courage or has taught me that so little is really known on the subject that one is safe in expressing one's views, let them be ever so erroneous. As a further personal excuse, I may remind you that " fools rush in," etc. At all events, I would now call attention to certain rail-sections which I believe to be good. I do not say they are the best, but I feel sure they have more merit than the majority of the adopted heavier-sectioned rails. In determining the proper form for a rail, the subject should be considered from two points; first, and most important, the duty required ; second, and of almost equal importance, the influence of existing details of manufacture upon the character of the finished product. It is perfectly proper that all the strains to which the rail will be subjected should be considered and calculated. But its ability to resist them will depend quite as much upon the character of the metal as upon the form of its section. That which would be the realization of the ideal with good steel would be disappointment with poorer metal. Therefore, the railroad engineer should always have in mind and pay due respect to what the metal worker may give him—the may being the factór of danger to be covered by his factor of safety, and possessing greater importance than any formula laid down by never so eminent authorities. It is well-known how positive is my conviction that high heat during manufacture and good rails cannot go together; hence, if we insist upon the avoidance of this evil by rail-makers, we must give them sections which can be made at low temperatures with commercial as well as technical success. The market-price for rails controls the practice of makers, and,

Jan 1, 1889

By Albert A. Mathews

OUTCROPS of gypsum rock near the present site of the city of Gland Rapids, Mich., were known to fur traders early in the nineteenth century. However, the deposits seemed without value and were not worked for some time. So far as cat1 be learned, Michigan gyp- sum was first used by a plasterer who settled in Grand Rapids in 1834 as a member of its fourteenth white family. In building a house for one of the early traders, be used some otnamental stucco mouldings manufactured from the local gypsum deposits for decorations in the gables and around some circular windows. The gypsum was broken out with a hammer, ground in an Indian corn mill, and burlled in a caulclron kettle,. After two attempts, the ornaments were successfully set, and remained on the house until it was destroyed by fire in 1850.

Jan 1, 1936

By E. A. von Hahn, T. R. lngraham

The rates of cementation of pd11 on electropolislzed copper cylinders were studied in aqueous perchloric acid solutions at pdII concentrations from 0.02 to 0.1 mM. The cylinders were rotated at various high speeds to reduce the diffusion layer to a minimum thickness. In 0.1 M HClO4 solutions, the cemented palladium is dense, adherent, and shiny. The rate data indicate that there are two stages in the deposition. In the initial stage, the rate of cementation is first order with respect to the pd11 concentration. The second stage is much slower. The first stage is consistent with rate control by the diffusion of pd11 ions to the copper surface, and/or chemical reaction at the surface, and the second stage is consistent with rate control by the diffusion of copper ions from the cop-per surface through the deposit of cemented palladium, out to the main body of solution. In 0.001 M HClO4 solution, only the first stage is evident and the rate is more rapid than at higher acidities. This rate enhancement is attributed to PdOH+ ions that predominate at low acidity and aye more reactive than unhydrolyzed pdII. The deposit is porous and loose. All of the cemented deposits are Pd-Cu alloys rather than pure palladium. Activation energies are 9.5 kcal per mole in 0.1 M HClO4 and 7.4 kcal per mole in 0.001 M HClO4. CEMENTATION or displacement reactions occur between aqueous solutions of metal salts and immersed metals according to the general equation: where M1 is electrochemically the more noble metal. Although these reactions find considerable application in metals recovery processes (e.g., the cementation of copper192 or gold3), in electrorefining processes (e.g., solution purification before electrolysis4,5), and in plating and metal finishing processes,6 few studies have been made of the kinetics of such reactions.7-9 The rates of cementation reactions will depend on one or more of the following factors: a) chemical reactions at the metal-solution interface; b) ionic transport to or away from the interface;'-' and c) the character and adherence of the cemented deposit on the substrate metal,6a,10 because the deposit will inhibit the rate of transport of dissolving ions (M2m+) into the solution. In this investigation, the kinetics of the early stages of cementation were studied to obtain an understanding of the reaction mechanism under conditions in which the deposit was sufficiently thin that its inhibiting effect could be disregarded. To achieve this, very dilute solutions in Mn+ were used. Cementation rates are often fast in the initial stages and transport-contr01led.9 To find conditions under which transport control would shift to chemical control, very high stirring velocities were used to minimize the diffusion-layer thickness. Of the many possible cementation reaction systems, the palladous perchlorate-copper system was chosen for this investigation because it was believed to involve simple ion-for-ion exchange. In addition, there are no interfering side reactions, such as the reduction of hydrogen ions, and anion effects are usually absent in perchlorate solutions. EXPERIMENTAL Materials. Reagent-grade chemicals and redistilled water were used in all experiments. Palladous perchlorate stock solutions (0.02 M) were prepared by dissolving 99.5 pct Pd sponge (Johnson Matthey and Mallory Ltd.) in concentrated nitric acid, adding concentrated perchloric acid, evaporating twice slowly (to prevent PdO precipitation) to a small volume, and diluting in a volumetric flask. To prevent gradual hydrolysis of PdII, the stock solutions were made 0.4 M in HC104. Tests for pdIV (Ref. 11) and C1- were negative. Copper strips were cut accurately from 0.025-in. electrolytic tough pitch sheet, Sample 1 (Mines Branch stock or Canadian Copper Refineries Ltd., Montreal), or from oxygen-free, high-conductivity sheet, Sample 2 (American Metal Climax O.F.H.C. brand, sold by Utility Brass and Copper Corp., Brooklyn). The strips were annealed for 1 hr at 335°C in a stream of purified nitrogen (Union Carbide, Linde Division) which had

Jan 1, 1967

EVERY dry thing that burns easily and multiplies or maintains fire by its own intrinsic nature can be put into an incendiary composition and various effects are produced. Some of these things are mineral combinations, like sulphur or its oil; some others, [163v] hot, dry, and subtle substances, like saltpeter; and some are. unctuous things, like fats and oils of any kind; while some serve because of dryness, like pith and wood. Some of these things are natural and some artificial But now I set aside the search for these differences in their composition. This is what I have found among all the ancient and modern things that I have been able to seek, and first, back in the time of Alexander the Great. Marcus Graecus, who was perhaps the inventor or a great experimenter and practicer of such things, writes of many of them. I have chosen some among these, and one* is this: In order to make it, he took Grecian pitch, alchitran, live sulphur, tartar, sarcocolla, niter, and petroleum oil, one part of each, and, in addition, a double amount of quicklime. He mixed it all with oil of egg yolks. Having put it in a well-covered and closed vessel of glass or glazed earthenware under warm manure, he left it for a month. Then, having liquefied it over a slow fire, always keeping the vessel well closed, he finally put this liquor in hollow sticks, in little pots, or in vessels expressly made, all with a little fuse fitted in the middle. If I should have to do this, I would say that a little gunpowder should be put in, which should give beginning to the fire so that it would ignite more easily. I have also found that another fire is made. For this sulphur is taken, or oil of sulphur if it is possible to obtain, petroleum oil or some rock oil, juniper oil, very well-refined saltpeter, and for one part of each of these five parts of asphalt; in addition, take goose or duck fat, pure black pitch, varnish, pulverized dove's dung, and enough aqua vitae to cover all the aforesaid things.. Then it is put in a glass vessel under warm manure for

Jan 1, 1942

By Raynor Linzey, Karl M. Busen

The formation of thin films of silicon oxide by anodic oxidation of silicon and the subsequent removal of these films by an etch is a process often used for the evaluation of concentration distributions Profiles) in silicon layers by the differential sheet conductance method. The accuracy of the resulting profile is very strongly influenced by the uniformity of the thickness of the reacted silicon. Normally, it would be expected that for a constant number of coulombs passed the thickness would be the same from oxidation to oxidation. Investigations show that in certain electrolytes, for a given number of coulombs passed through an n-type silicon sample, the thickness of the reacted silicon increased with increasing resistivity. Even for the same resistivity the thickness varied sometimes by a factor of 1.5. When an electrolyte was used which consisted of 10 pct water by volume in ethylene glycol with 4.0 g KNO per 1000 ml of solution, anodiza-tion at 5 ma per sq cm led to satisfying results. Short-time anodizations gave oxide layers of a higher apparent density than those experienced from thermally gown silicon oxides. THE functioning and the electrical characteristics of semiconductor devices are based upon the incorporation of "impurities" into a single-crystalline body of suitable material and on the concentration distribution (profile) of this impurity. The incorporation can be achieved by well-known processes as, for example, by diffusion, epitaxial growth, alloying, or ion implantation. Often the profile resulting from these processes is not known. A powerful tool to learn about a concentration distribution is given by the method of differential sheet conductance which employs successive four-probe measurements on a layer subjected to stepwise removal of thin sublayers. Differential sheet conductance vs position (or penetration depth) of a sublayer is plotted and a smooth curve is drawn through the data. From this curve the profile is then calculated. When the semiconductor material is silicon, the sublayers are removed suitably by anodic oxidation of the silicon and subsequent dissolving of the formed silicon oxide by an etch. The accuracy of the resulting profile is very strongly influenced by the uniformity of the sublayer thickness. Normally, it would be expected that, for a constant number of coulombs passed, the thickness would be constant from oxidation to oxidation. Investigations showed that for sublayers several hundred angstroms thick the reproducibility can be rather poor. Therefore, efforts were made to obtain a reliable technique for uniform removal. The present paper describes such a technique and certain phenomena which were encountered during the investigations. APPARATUS AND TECHNIQUE The first report on the investigation of concentration distributions, where for differential sheet conductance measurements thin silicon sublayers were removed from a diffused layer by anodic oxidation, was given by Tannenbaum. The author reports the removal of sublayers which for the most part were 400 thick. More advanced device designs now require much narrower layers. When it was tried in these laboratories to determine profiles within such layers, difficulties were encountered with respect to sublayers which by necessity had to be thinner than the ones reported by Tannenbaum. The apparatus used for the investigations is sketched in Fig. 1. Two cylindrical containers connected by a wide tube are filled with an electrolyte. The left container receives the cathode whereas the right container is closed at the bottom end by a sample support consisting of a Teflon base and a copper pedestal. The silicon sample (1 by 1 cm) is mounted to the pedestal embedded flush in the Teflon base using silver paint (Degussa) for electrical contact. Pyseal is applied to the edges of the sample to protect the copper pedestal from the electrolyte. The base is mounted to the container using a water-tight silicon rubber gasket. Fig. 2 gives a view of the sample support. The copper pedestal is connected to the positive side of a power supply operating at a constant current output (Kepco Model ABC 425M). The electrolyte which has been reported by Duffek et al. consisted of either 2 or 10 pct water by volume in ethylene glycol and 4.0 g KNO3 in 1000-ml solution. The electrolyte is best prepared

Jan 1, 1967

All the Affiliated Student Societies report that the present college year promises to be a most successful one. The officers for this year, so far as reported, are as follows: TUFTS COLLEGE CHEMICAL SOCIETY President, CHESTER B. PIERCE Vice-president, JOHN H. SCHMUCK Secretary-treasurer, DANIEL A. PRESCOTT President, R. G. SATTERLEY Third vice-president, H. E. BLAKE First vice-president, LESTER VOCKE Secretary,-J. E. FLANIGAN Second vice-president, `V. J. KLINE Treasurer, PROF. JAMES FISHER, JR About 75 per cent. of the students are ex-service men, and most of them saw service in France.

Jan 12, 1919

By G. S. Tint, M. Herman, V. V. Damiano

Dislocation arrays and substructures were studied in cadmium doped zinc crystals using a newly devised etching technique. Cadmium precipitates delineating the dislocations were revealed by etching a surface closely parallel to the (0001) slip plane. Cinephotomicrography of the continuous etching process revealed the three-dimensional aspects of dislocations in the bulk crystal. Dislocation etch patterns were studied in both deformed and annealed crystals after suitable aging at room temperature. The effect of annealing was evidenced by a rearrangement of the dislocations into low-angle boundaries and hexagonal networks. ETCH pit techniques have been used extensively to study dislocations in both deformed and annealed bulk metal crystals. Ideally one hopes to obtain a one-to-one correspondence between the etch pits and the points of emergence of the dislocations at the surface. One then attempts to deduce the way in which dislocations are arranged in the bulk crystal from the arrangement of etch pits on the surface. It is clear that one can obtain only limited information of the dislocation configurations inside the crystal from etch pit studies of single surfaces. Considerably more information is obtained if one is able to follow the course of the dislocations through the crystal using progressive etching technique. Techniques of this sort were used by Gilmanl to study dislocations on the slip planes of NaCl crystals and by Damiano and Tint2 to study dislocation arrangement in zinc crystals grown from the melt. The present paper makes use of a technique first described by Tint and Damiano3 to observe and continuously record the dislocation structures which appear while a crystal surface was being progressively etched. Studies were made on cleaved (0001) surfaces to reveal the dislocations along their length on the surface closely parallel to the slip plane. The technique for revealing segments of dislocations along their length by etching is well known. Wilsdorf and Kuhlmann-wilsdorf4 revealed disloca- tions along their length in aluminum containing a few percent copper, when precipitates segregated along the dislocations. The technique was used by Low and Guard5 to study dislocation configurations on the slip plane in Fe-Si alloys containing carbon. In the present work the technique was applied to zinc containing cadmium since it was shown by Gil-man6 that a cadmium-rich phase could be made to precipitate from supersaturated solutions along dislocations in zinc. Segments of dislocations delineated by the precipitates were revealed by etching a surface prepared by cleaving the crystal. The three-dimensional nature of dislocations and substructures was thus studied from the cinephotomicro-graphic record of the continuous etching process. EXPERIMENTAL Single crystals of zinc containing the order of 0.1 pct Cd were prepared by slowly lowering a graphite crucible containing the melt through a temperature gradient of 15°C per cm at a rate of 1.5 X 10-3 cm per sec. "As grown" crystals were aged for periods of 1 month at room temperature, then cleaved in liquid nitrogen, and etched according to the procedure used by Gilman.' The etchant containing 32 g of CrO3, 6 g of hydrated Na2SO3 in 100 ml of water behaved as a chemical polish for zinc and etch pits were produced at the site of precipitates or inclusions. After the precipitates or inclusions were removed from the surface, the etch pits left behind were eventually polished smooth. This behavior enabled one to continuously observe the surface while the specimen was immersed in the etchant. Best results were obtained when the specimen surface was vertical and the reaction products of polishing were continuously removed by gravitational convection. Some crystals were heavily deformed in excess of 25 pct strain, others were lightly deformed the order of a few pct by compression such that the deformation occurred essentially by basal glide. Some crystals were etched immediately after deformation, others were allowed to age at room temperature for several weeks prior to etching. Heavily deformed crystals were annealed at various temperatures and etched on the cleavage plane immediately after annealing, others were allowed to age at room temperature for several weeks prior to etching. The etched structures of deformed and annealed structures were studied. Similar experiments were conducted on 99.9999 pct pure zone refined Tadanac zinc crystals which

Jan 1, 1963

By AUDLEY H. STOW

I. INTRODUCTION. THE general drift of the discussion as to the relative merits of pressure- and exhaust-fans has resulted, if we may judge from the prevailing practice, largely in favor of the latter. The subject has been hitherto treated, however, with special reference to highly gaseous mines, the effect of the form of ventilation upon dust-explosions having been too little considered. Even in mines containing practically no gas, dust-explosions may occur; and if, as I believe, pressure-fans are to be preferred for their effect upon dust, it may be worth while to reopen the debate, and to challenge the advisability of exhaust-ventilation under certain conditions. There are several forms of colliery-ventilation, which may be described as follows: Plain or simple pressure-ventilation, in which the fan acts as a pressure-fan, and the movement of coal is unobstructed at the surface by doors or equivalent devices in drifts or shafts, the traveling and haulage thus being in the return-current. Plain exhaust-ventilation, in which the fan acts as an exhaust-fan, the movement of coal being likewise unobstructed at the surface, and the traveling and haulage being in the intake. Obstructed pressure-ventilation, in which the movement of coal is obstructed at the surface, in order that the traveling and haulage may be in the intake. Obstructed exhaust-ventilation, in which the movement of coal is obstructed at the surface, in order that the traveling and haulage may be in the return. The apparent advantages in running a fan "pressure" during working-hours, and " exhaust" between shifts, seem to justify the recognition of this combination as a standard form of ven-

Feb 1, 1909