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By Ralph B. Stevens

INTRODUCTION Underground fires continue to be one of the most serious hazards to life and property in the mining industry. Although underground mines are analogous to high-rise buildings where persons are isolated from immediate escape or rescue, application of technology to locate and control fire hazards while still in their controllable state is slow to be implemented in underground mines. Even in large surface structures such as hotels, often only fire protection systems which meet minimal laws are implemented due to the high cost of adding extensive extinguishing systems, isolation barriers, alternate ventilation, escape routes and alarm systems. Incomplete and ineffective protection occasionally is evidenced where costs would not seem to be a factor, such as the $211 million MGM Grand Hotel fire November 21, 19801. Paramount in increasing fire safety and decreasing the threat of serious fire is early warning followed by proper decision analysis to perform the correct action. However, very complex fire situations can be produced in structures such as high-rise buildings and underground mines simply because of the distances between the numerous fire-potential locations and fire safe areas. Other complexities arise when normal activities occur that emit products of combustion signaling a fire condition to a sensitive fire/smoke sensor. For example, the operation of diesel equipment or the performance of regular blasting can produce combustion products that reach the sensitive alarm points of many sensors2. Smoke detectors for surface installations provide fire warning when occupants are at a distant location or when sleeping, thus greatly reducing injuries and property damage. However, when installed in the harsh environments of underground mines, fire and smoke detection equipment soon becomes inoperative, unreliable, or requires excessive maintenance. The U.S. Bureau of Mines has performed many studies and tests to improve fire and smoke protection for underground mine workers3. This paper describes several USBM safety programs which included in-mine testing with mine fire and smoke sensors, telemetry and instrumentation to develop recommendations for improving mine fire safety. It is hoped that the technology developed during these programs can be added to other programs to provide the mining industry with the necessary fire safety facts. By recognizing fire potentials and being provided with cost-effective, proven components that will perform reliably under the poor environmental conditions of mining, mine operators can provide protection for their working life and property equal to that which they provide for themselves and their families at home. The basis of this report is two USBM programs for fire protection in metal and nonmetal mines4,5 and one coal program6. The data was collected beginning in May 1974 and continuing through the present with underground tests of a South African fire system installed at Magma Mine in Superior, Arizona, and a computer-assisted, experimental system at Peabody Coal Mine in Pawnee, Illinois. The conduct of each program was as follows: • Define the problem and its magnitude in the industry • Develop concepts to solve or diminish the problem • Review available hardware or systems approaches to fit the concepts • Install and demonstrate the performance of a prototype system through fire tests in an operating mine. MINE FIRE FACTS Whether in coal or metal and nonmetal mines, the potential severity of fire hazard is directly related to location. As shown in Figure 1, fire in intake air at zones A, B, C or D can cause contamined air to route throughout the mine quickly if not detected, isolated or rerouted. Causes and location of former metal and nonmetal fires are represented in Table 1; the cause and location of fatalities and injuries is shown in Table 2. Coal-related fires and their impact on deaths and injuries are graphed in Figure 2; their locations are described in Table 37. Significantly the table shows that the hazard to personnel was three times greater for fires occurring in shaft or slope areas, and the percentage of deaths and injuries was four times that of other areas. Number of Persons Affected A 129-mine sample indicated that from 8 to 479 employees per shift work in underground metal and nonmetal mines, and that deeper mines have larger populations, as shown in Figure 3. Coal mining relates similar employment, and a 16-state sample of 670 mines employing at least 25 persons shows the distribution in Figure 4. Drift mines accounted for 58 percent of the sample but employ only 45 percent of the underground workers.

Jan 1, 1982

By Sheldon P. Wirnpfen

AN extensive study of German underground manufacturing experience is being undertaken by the Air Materiel Command. Headquarters officials consider completely underground facilities one of the most effective means of protecting aircraft production against air attacks of the strength and type employed in World War II. Advantages accruing to underground manufacturing installations other than protection are, perhaps, a smaller maintenance problem and the possibility of using gravity flow on some production lines. Offsetting these advantages are the high cost of construction, problems of ventilation, and poor acoustics. Excavation costs might well be less than the cost of enclosing the same area on the surface, as new and better methods of rock drilling and transportation are developed. Certainly the amount of building materials used would be far less than in constructing a surface plant of the same dimensions. A fewer number of skilled workers would be required to perform the labor of excavation. Underground construction would

Jan 1, 1947

By D. W. Fuerstenau

Locked-cycle grinding experiments on mineral mixtures provide a means to study circuit performance in simulated continuous grinding systems. Such experiments with calcite/quartz mixtures revealed that approximately twenty-five 2-minute cycles are required before the composition of the circuit product and the recycle material attain steady state. The circulating load, after steadily increasing during the first 15 cycles, continued to fluctuate over a narrow range. Previous batch ball mill grinding of mineral mixtures has shown that breakage rate functions of minerals are time- independent but composition-dependent. In the closed-circuit grinding of ores with constituents having different grindabilities, the grinding rate parameters for the components also would therefore change during the transient period. With fluctuations in feed composition occurring randomly every half to one hour in processing plants, it is quite likely that the grinding circuit can be in unsteady state perpetually. The significance of these observations is discussed in this paper in the con- text of the models used in control schemes for the grinding circuits

Jan 1, 1984

By G. S. Cole, G. F. Bolling

Fluid flow strongly influences ingl structure and the columnar -to-equaaxed transition. Artificial flow patterns siwzilar to the nuturul ones act to induce this transition, while dampening forces act to suppress this transition. It is shown here how simple mechanical forces can be applied to a systerrz in order to induce or slipPvess relative fluid flow and the change both the structure transition and the exact structures obtained. The example used is the effect of slow rotations and oscillations 012 a cooling- ingot (of laboratory scale). The details of rotution and oscillation for various cooling rates, lenlperal~ire gradients, and sizes of ingot are related to other solidzfication variables. THE grain structure of a casting can be changed by altering the fluid motion during solidification. Just how important these changes are depends directly upon the degree to which the fluid motion can be controlled. An early step in understanding the nature and influences of fluid motion was taken by studying natural thermal convection; when a static mechanical device was used to suppress natural flow the result was opposite to that obtained when an electromagnetic device was used to augnlent flow in a pattern similar to the natural one. ''2 Suppression allowed more columnar growth to occur, but "augmented natural convection" brought about an earlier columnar-to-equiaxed transition (CET). Since the solidification of a free ingot must have characteristics somewhere between those displayed during suppression and augmentation, we know that natural convection must influence the CET. Further, since heat transfer in the liquid is always some time-dependent combination of convection and conduction, it can easily be guessed that the temperature gradient in the liquid is the vital factor affecting the CET.1,2 It is obvious that the structure arising from the unadulterated solidification of an ingot, without external influence, is rarely if ever the best possible one. Although the pattern of the natural fluid flow may be considered efficient, the magnitude of the flow and the heat transfer decrease freely from the outset. For a

Jan 1, 1968

By A. M. Kivari

OPERATIONS at the cement plant of the Permanente Corporation, in the hills about 45 miles south of San Francisco and 12 miles west of San Jose, are interesting to the members because of the adoption of modern hydrometallurgical methods for handling and beneficiating raw materials. Closed-circuit grinding, classification, hydro-separation, flotation, agitation, and thickening are familiar terms at this cement plant. These methods make it possible to process refractory limestone into suitable materials for the manufacture of modern cements. Construction of the plant, having originally a design capacity of 7000 bbl. of cement per day, was started in June 1939, and the first clinker was ground on the following Christmas Day. At present the capacity is about 12,000 bbl. of finished cement per 24 hr., most of the production being low-heat cement.† About 3130 tons of limestone, 620 tons 0f clay and 100 tons of gypsum are required daily for this output. Occasionally iron oxide is added to the clay to obtain the desired composition. This, together with the gypsum, is purchased from outside sources. Up to the present time, the corporation has produced low-heat, normal, moderate heat, moderate-sulphate-resisting, high-early-strength, oil-well, modified-oil-well, and plastic cements. Most of the present production is for Shasta Dam, near Redding, Calif., the total demand being 5,800,000 bbl, of cement. Following are some of the cement requirements of the Shasta Dam specifications: [PERCENT Chemical composition: Loss in ignition2.25 Insoluble residue0.75 SO32.25 MgO5.00 Uncombined lime in clinker (CaO)1 .25 Percentage of iron oxide to alumina ratio1.5 Compound composition: Tricalcium silicate (3CaO.Si02)Not more than 3,5 Dicalcium silicate (2CaO.Si02)Not less than 40 and not more than 65 Tricalcium aluminate (3CaO.Al2O7)Not more than 7 Tetracalcium aluminoferrite (4CaO.A12O3.Fe203) Not more than 0 Fineness:] The average specific surface in the bin sampled shall be not less than 1800 sq. cm. per gram and no individual sample less than 1600 sq. centimeters. Compressive strength: The average compressive strength-in pounds per square inch of three mortar cubes composed of one part cement and 2.75 parts fine testing sand, by weight, shall be equal to or greater than the following:

Jan 1, 1941

By A. M. Kivari

OPERATIONS at the cement plant of the Permanente Corporation, in the hills about 45 miles south of San Francisco and 12 miles west of San Jose, are interesting to the members because of the adoption of modern hydrometallurgical methods for handling and beneficiating raw materials. Closed-circuit grinding, classification, hydroseparation, flotation, agitation, and thickening are familiar terms at this cement plant. These methods make it possible to process refractory limestone into suitable materials for the manufacture of modern cements. Construction of the plant, having originally a design capacity of 7000 bbl. of cement per day, was started in June 1939, and the first clinker was ground on the following Christmas Day. At present the capacity is about 12,000 bbl. of finished cement per 24 hr., most of the production being low-heat cement. [t] About 3130 tons of limestone, 620 tons of clay and 100 tons of gypsum are required daily for this output. Occasionally iron oxide is added to the clay to obtain the desired composition. This, together with the gypsum, is purchased from outside sources. Up to the present time, the corporation has produced low-heat, normal, moderate-heat, moderate-sulphate-resisting, high-early-strength, oil-well, modified-oil-well, and plastic cements. Most of the present production is for Shasta Dam, near Redding, Calif., the total demand being 5.800,000 bbl. of cement. Following are some of the cement require¬ments of the Shasta Dam specifications: [PER CEN'I Chemical composition: Loss in ignition2.25 Insoluble residue0.75 S032.25 M905.00 Uncombined lime in clinker (CaO)T.25 Percentage of iron oxide to alumina ratio1.5 Compound composition: Tricalcium silicate (3CaO.Si02)Not more than 35 Dicalcium silicate (2CaO.Si02)Not less than 40 and not more than 6,5 Tricalcium aluminate (3CaO.Al203)Not more than 7 Tetracalcium aluminoferrite (4CaO.A1203.Fe203) Not more than 20 Fineness:] The average specific surface in the bin sampled shall be not less than 1800 sq. cm. per gram and no individual sample less than 1600 sq. centimeters. Compressive strength: The average compressive strength in pounds per square inch of three mortar cubes composed of one part cement and 2.75 parts fine testing sand, by weight, shall be equal to or greater than the following: [ ]

Jan 1, 1941

By A. M. Kivari

Operations at the cement plant of the Permanente Corporation, in the hills about 45 miles south of San Francisco and 12 miles west of San Jose, are interesting to the members because of the adoption of modern hydrometallurgical methods for handling and beneficiating raw materials. Closed-circuit grinding, classification, hy-droseparation, flotation, agitation, and thickening are familiar terms at this cement plant. These methods make it possible to process refractory limestone into suitable materials for the mallufacture of modern cements. Construction of the plant, having originally a design capacity of 7000 bbl. of cement per day, was started in June 1939, and the first clinker was ground on the following Christmas Day. At present the capacity is about 12,000 bbl. of finished cement per 24 hr., most of the production being low-heat cement. † About 3I30 tons of limestone, 620 tons of clay and I00 tons of gypsum are required daily for this output. Occasionally iron oxide is added to the clay to obtain the desired composition. This, together with the gypsum, is purchased from outside sources. up to the present time, the ccrporation has produced low-heat, normal, moderate-heat, moderate-sulphate-resisting, high-early-strength, oil-well, modihed-oil-well, and plastic cements. Most of the present production is for Shasta Dam, near Red- ding, Calif., the total demand being 5,800,000 bbl. of cement. Following are some of the cement require ments of the Shasta Dam specifications: Per Cent Chemical composition: Loss in ignition.......... 2.25 Insoluble residue......... 0.75 SO3.................... 2.25 MgO................... 5.'' Uncombined lime in clinker (CaO)......... I.25 Percentage of iron oxide to alumina ratio....... I.5 Compound composition: Tricalcium silicate (3CaO.SiO2)........... Not more than 35 Dicalcium silicate (zCaO.SiO2)........... Not less than 40 and not more than 65 Tricalcium aluminate (3CaO.Al2O3).......... Not more than 7 Tetracalcium aluminofcr- rite (4CaO.Al²O³.Fe²O³) Not more than 20 Fineness: The average specific surface in the bin sampled shall be not less than 1800 sq. cm. per gram and no individual sample less than 1600 sq. centimeters. Compressive strength: The average compressive strength in pounds per square inch of three mortar cubes composed of one part cement and 2.75 parts fine testing sand, by weight, shall be equal to or greater than the following:

Jan 1, 1942

By A. M. Kivari

Operations at the cement plant of the Permanente Corporation, in the hills about 45 miles south of San Francisco and 12 miles west of San Jose, are interesting to the members because of the adoption of modern hydrometallurgical methods for handling and beneficiating raw materials. Closed-circuit grinding, classification, hy-droseparation, flotation, agitation, and thickening are familiar terms at this cement plant. These methods make it possible to process refractory limestone into suitable materials for the mallufacture of modern cements. Construction of the plant, having originally a design capacity of 7000 bbl. of cement per day, was started in June 1939, and the first clinker was ground on the following Christmas Day. At present the capacity is about 12,000 bbl. of finished cement per 24 hr., most of the production being low-heat cement. † About 3I30 tons of limestone, 620 tons of clay and I00 tons of gypsum are required daily for this output. Occasionally iron oxide is added to the clay to obtain the desired composition. This, together with the gypsum, is purchased from outside sources. up to the present time, the ccrporation has produced low-heat, normal, moderate-heat, moderate-sulphate-resisting, high-early-strength, oil-well, modihed-oil-well, and plastic cements. Most of the present production is for Shasta Dam, near Red- ding, Calif., the total demand being 5,800,000 bbl. of cement. Following are some of the cement require ments of the Shasta Dam specifications: Per Cent Chemical composition: Loss in ignition.......... 2.25 Insoluble residue......... 0.75 SO3.................... 2.25 MgO................... 5.'' Uncombined lime in clinker (CaO)......... I.25 Percentage of iron oxide to alumina ratio....... I.5 Compound composition: Tricalcium silicate (3CaO.SiO2)........... Not more than 35 Dicalcium silicate (zCaO.SiO2)........... Not less than 40 and not more than 65 Tricalcium aluminate (3CaO.Al2O3).......... Not more than 7 Tetracalcium aluminofcr- rite (4CaO.Al²O³.Fe²O³) Not more than 20 Fineness: The average specific surface in the bin sampled shall be not less than 1800 sq. cm. per gram and no individual sample less than 1600 sq. centimeters. Compressive strength: The average compressive strength in pounds per square inch of three mortar cubes composed of one part cement and 2.75 parts fine testing sand, by weight, shall be equal to or greater than the following:

Jan 1, 1942

By Vernon A. Mrak

The Powder River Basin of northeast Wyoming was the first area in the state to receive attention during the early days of uranium exploration. Although the uranium occurrences are many and widespread, most of the known ore deposits are quite small and difficult to mine. As a result of this, detailed regional exploration in the Powder River Basin has been neglected. The uranium ore deposits occur in that part of the Wasatch Formation that is of earliest Eocene age, and they are scattered over an area of about 400 square miles. All uranium ore deposits are associated with red beds or altered sandstones within the Wasatch Formation. Uranium ore was first shipped from the region in 1953. Total production through June of 1965 is 506,257 tons of uranium ore containing 1,922,527 pounds of U3O8. The average grade of ore is about 0.19 per cent U3O8. The major producing area of the Powder River Basin is the Monument Hill district where about 91 per cent of the basin's total uranium ore has been mined. The source of uranium is presumed to have been the Oligocene, Miocene, and perhaps Pliocene tuffaceous rocks that once overlay the area. Joints, fractures, and permeable beds or zones were the passageways for the migration of uraniferous waters from the overlying beds to the Eocene host rocks.

Jan 1, 1968

By Robert B. Johnson

The refraction seismic method has been used as an indirect means of exploring for fluorspar in southern Illinois by the Illinois State Geological Survey. Use of the method has been restricted to those areas where mineralization is associated with faults, a restriction necessitated by the operating principles of the refraction method. The seismic data enable the interpreter to locate fault zones in the subsurface and, under ideal circumstances, to make estimates of dip direction and magnitude and vertical displacement provided the local stratigraphic units are known and are geophysically recognizable. In this instance, refraction seismic exploration has been successful in the surface mapping of well-developed faults, both simple and complex with which fluorspar may or may not be associated. However, less clear results have been obtained where faulting has been less severe and where there are numerous accompanying mineralized joints.

Jan 1, 1964

By Daniel J. Martin, James L. Martin

The dendritic pattern of steels shown by deep etching is used extensively as a guide in the inspection and control of the great majority of steels used in ordnance construction and for many applications in industry. The value of macroexamination lies in the fact that it enables a qualified observer to make deductions concerning the general quality of relatively large pieces of metal. Not the least of these general characteristics is the nature and extent of the dendritic segregation in the steel, either in the cast condition or after mechanical or thermal treatments. Previous Work Detailed methods for macroetching were outlined by Yatsevitchl and have been standardized by the American Society for Testing Materials. A comprehensive study of the occurrence, origin, and the chemical and crystalline nature of the dendritic structure was given by Keshiam2 The marked persistence of dendritic segregation in nickel steels is fully recognized and has been discussed by Sauveur and Reed3 and by others. Very little, however, has been written on the effect of the various elements on the macrostructure of steels, and the purpose of this report is to submit evidence concerning the influence of chromium, nickel and molybdenum on the macrostructure of some 4 by 4-in. ingots cast and treated under closely controlled conditions. Methods and Results The ingots to be described were made in a 60-lb. high-frequency induction furnace at the Watertown Arsenal. Heats were made from a single lot of materials; were molten for the same length of time; tapped at approximately the same temperature into a standard mold preheated in each case to 150º ± 10º C.; and stripped and buried in ashes after 10 min. in the mold. Transverse disks were taken from the same location in

Jan 1, 1939

By James L. Martin, Daniel J. Martin

The dendritic pattern of steels shown by deep etching is used extensively as a guide in the inspection and control of the great majority of steels used in ordnance construction and for many applications in industry. The value of macroexamination lies in the fact that it enables a qualified observer to make deductions concerning the general quality of relatively large pieces of metal. Not the least of these general characteristics is the nature and extent of the dendritic segregation in the steel, either in the cast condition or after mechanical or thermal treatments. Previous Work Detailed methods for macroetching were outlined by Yatsevitchl and have been standardized by the American Society for Testing Materials. A comprehensive study of the occurrence, origin, and the chemical and crystalline nature of the dendritic structure was given by Keshiam2 The marked persistence of dendritic segregation in nickel steels is fully recognized and has been discussed by Sauveur and Reed3 and by others. Very little, however, has been written on the effect of the various elements on the macrostructure of steels, and the purpose of this report is to submit evidence concerning the influence of chromium, nickel and molybdenum on the macrostructure of some 4 by 4-in. ingots cast and treated under closely controlled conditions. Methods and Results The ingots to be described were made in a 60-lb. high-frequency induction furnace at the Watertown Arsenal. Heats were made from a single lot of materials; were molten for the same length of time; tapped at approximately the same temperature into a standard mold preheated in each case to 150º ± 10º C.; and stripped and buried in ashes after 10 min. in the mold. Transverse disks were taken from the same location in

Jan 1, 1939

By J. C. Bradley

The relation of annealing temperature to conductivity of copper wire has been determined. Conductivity hard was 98.26 per cent. After a 10-min. heat,ing at 200" C. it was 98.69. By annealing 10 min. at 300" C. a large increase, to 100.93, occurred. Maximum conductivity, 101.15, was attained after a 500" C. anneal; thereafter it decreased to 100.53 after a 950" C. anneal. If copper is gassed the decrease is much more than this. Material and Method The work was done on high grade electrolytic copper, 99.942 per cent, copper plus silver, silver 0.0008 per cent. It was hot-rolled to 1/4 in., then cold drawn to 0.080 in. The wire was cut into 25 5-ft. lengths and numbered 1 to 25 as cut. Four samples were tested hard. The others were wound into 5-in. diameter coils. For the 100" C. heating a coil was put into water, the water brought to . boiling, and the wire kept at this temperature for 10 min. For the higher temperatures the coils were placed in envelopes of sheet copper, a little water added, and the envelopes sealed by folding over the edges twice, and hammering them together. This kept the air out very well. The envelope and wire were brought to the desired temperature; this was maintained for 10 min., then the whole was water-quenched. Results Data from the tests are shown in the table and plot (see Fig. 1); conductivity is referred to the International Annealed Copper Standard at 20" C. Conductivity hard is considerably less than conductivity soft.1 The increase is sharp when the wire anneals. The maximum, 101.15 per cent, in the particular material used, comes at 500º C.; thereafter the conductivity falls to 100.53 per cent. after 950" C. annealing, a drop of 0.62 per cent.

Jan 1, 1927

By R. O. Williams

It is shown that Ni3Al precipitates homogeneously from nickel-rich alwminum alloys as plates on the (100) planes. Prior to actual precipitation a process occurs which is believed to be one of increasing short-range order. After precipitating the Ni3Al plates enlarge through competitive growth. Discontinuous precipitation can occur simultaneously with the above processes. Recent ideas of the origin of precipitation strengthening appear adequate to explain the hardness changes. REMARKABLY little appears to be known about the precipitation process in Ni-Al alloys in spite of their technical importance. This investigation originated to supply additional information about precipitation in general, this system in particular. Information on the structures and kinetics have been obtained through the use of hardness, X-rays, microscopy, calorimetry, and resistivity on high-purity alloys. PROCEDURES Six alloys, Table I, were prepared by melting carbonyl nickel and high-purity aluminum in alumina crucibles in vacuum and casting into 1-in. graphite molds. All rods were homogenized at least once at 1300°C for 24 hr prior to swaging and this was repeated on the first three alloys after 75 pct reduction. Alloy 4 could be reduced only 10 pct at 1000°C (probably in two-phase field) prior to fracture but 1/4-in. samples quenched from 1100°C were readily reduced cold. Alloy 5 was reduced 15 pct cold but failed on the next pass while alloy 6 of essentially the same aluminum content failed inter-granularly without apparent flow up to 1000°C. The alloys were heated in hydrogen at the elevated temperatures and formed thin, coherent aluminum oxide coatings which provided excellent oxidation resistance at lower temperatures. However, freshly prepared surfaces showed considerably less resistance at 500"to 700°C in air and apparently resulted in internal oxidation. As a consequence, low-temperature agings were carried out in evacuated tubes. RESULTS The isothermal hardening behavior of these alloys at 500"and 565C is given in Figs. 1 and 2. These results were obtained from samples cold worked 75 pct, recrystallized at 1000°C (1100°C for the 7.8 pct Al) and quenched in water. This recrystallization was used to give smaller grain sizes so as to obtain more uniform hardness values and the points represent an average of five readings. The electrical resistivity was measured on 1/16-in. wires quenched from 1000°C during aging at 495°C to give Fig. 3. The energy release and its rate are given in Fig. 4 for the 6.9 pct Al alloy during aging around 500°C. Inasmuch as this was a single run, its accuracy is not known but certainly the general shape and magnitudes are correct. The method used to obtain these results is described elsewhere.' Data for the aging at 600°, 700°, and 800°C of these alloys cold worked 50 pct are given in Fig. 5. Supplementary information from microscopy and X-ray diffraction have been included to indicate recrystallization, discontinuous precipitation and the appearance of superlattice lines from the Ni3Al. The hardness of these alloys as annealed, aged, cold worked, and cold worked and aged is given vs composition in Fig. 6. Those samples which were isothermally aged, Figs. 1 and 2, were reaged at 532°C and at successively higher temperatures for the indicated times to give the data of Fig. 7. These results as well as certain others, support the idea that the level of hardness reached for temperatures above 600°C are equilibrium values more or less independent of path. This being the case, the breaks in the curves would be the complete solution of the Ni,Al. The electrical resistivity versus temperatures for some of these alloys, both aged and unaged, is given in Fig. 8 along with those data from heating slowly (10 deg per day) to high temperatures. Interesting points include the lowering of the Curie temperature (the change in slope), the lack of any indications of a solubility limit and the large temperature coefficient for the Ni3Al. A slight break for Ni3Al around 100C shows up but this is not a Curie temperature as Ni3Al is not ferromagnetic down to -190°C. Metallographically both the nickel-rich solid solution and the Ni3Al appear very much like pure nickel. Profuse twin boundaries are present both

Jan 1, 1960

By Douglas J. Harvey

The surface tension of lead-tellurium alloys (in the range 0 to 6.70 at. pct Te) ad lead-arsenic alloys (in the range 0 to 10.53 at. pct As) has been examined by the maximum bubble pressure method. The surface tension of high purity lead can be expressed over a range of temperatures (M.P. to 750°C) by the relationship = 512 — 0.133t. Arsenic and lellurium were both found to be surface active in lead. The surface excess concentration at 700°C was .found to be constant at 0.74 x 10-10 moles per sq cm for tellurium. The surface excess of arsenic at 700°C varied between 0.26 x 10-10 moles per sq cm at 0.16 at. pct to 1.5 x 10-10 moles per sq cm at 8.3 at. pet. The surface tension of lead has been investigated sporadically over the last 90 years. The first recorded study was made by Quincke1 who used a rather crude application of the drop-weight method. Hogness2 obtained the first reliable value for the surface tension of lead by measuring the pressure necessary to force the liquid metal from the end of a small capillary of known radius. Hogness gives the empirical formula: ?(surface tension)= 444 - 0.077 (l-327) which describes the relationship between surface tension and temperature ("C); This work was followed by that of Bircumshaw3 who applied the two-capillar maximum bubble pressure method of Sugden.4 The values published by Bircumshaw are in good agreement with those found by Hogness. Matuyama5 examined the surface tension of lead by the drop weight method. However, the values found are somewhat higher than those previously reported. More recent investigations by Greenaway6 and by Melford and oar' have resulted in data which are not in close agreement, but which are well within the expected range at most temperature levels. The study of the surface tension of lead alloys began with Drath and sauerwald8 who examined the lead-bismuth system. They found that the surface tension values of the alloys in this system deviated only slightly from the ideal mixture rule. Matuyarna5 examined the lead-antimony system. Bircumshaw the lead-tin, and the lead-indium system was studied by Hoar and Me1ford.10 The results of these investi- gations are summarized in Fig. 1. It may be seen that the data vary only slightly from the ideal mixture rule. As none of the metals studied and reported in the literature has a very interesting effect on the surface tension of lead,*the next logical step might be to examine the effect of metals of low solubility or nonmetals having some liquid solubility. Baes, and Kellogg11 have pointed out that the elements most likely to be surface active in liquid metals are ones of limited solubility in the liquid state and possessing weak intermolecular bonding forces in the solid state. Therefore, Group V, VI and VII nonmetals are most likely to be surface active. It was decided to examine the effect of a borderline metal, arsenic, and a nonmetal tellurium. Arsenic forms a eutectic with lead having a melting point of 290°C and a composition of 6.9 at. pct As.13 Pure arsenic sublimes when heated above 610°C. Even though alloying with lead lowers the vapor pressure, fumes containing arsenic are evolved at a very noticeable rate when lead-arsenic alloys are heated above 650°C. Tellurium raises the liquidus temperature of lead sharply to 904°C,14 the melting point of PbTe (lead-telluride). The solid solubility of tellurium in lead was determined by Greenwood and worner15 to be 0.0007 at. pct at room temperature. EXPERIMENTAL METHOD Surface Tension Measurement—The two capillary maximum bubble pressure method for measuring surface tension developed by Sugden,4 and used later

Jan 1, 1962

By I. A. Lesk

The various materials utilized in the construction of integrated circuits, and the resultant materials interfaces, are discussed with emphasis on a materials system that is compatible with all types of integrated circuits and minimizes the number of different interfaces. Problems with interfaces may originate in the silicon, on its surface, and between other materials within the integrated-circuit package independent of the silicon. ThE difference between integrated-circuit theory and practice may generally be spelled out in terms of the difficulties in fabricating a desired structure. There are, of course, problems in forming the requisite materials, of the necessary composition and geometry, where needed. A distinct class of problem, however, is associated with interfaces— generally between different materials, but occasionally between regions of the same material. We require that each interfacial system perform its proper electrical, mechanical, and thermal function, and do so in an unchanging manner with time under the most severe operating conditions. In a practical sense, we deal in nonideal systems, such that it is generally not possible to form an interface exactly the way it was intended, even if we allow for a knowledge of the practical limitations of the fabrication system. Another way of looking at this situation is to realize that, when we form a group of interfaces under apparently the same experimental conditions, there are often differences of important consequence between them. Very high-magnification pictures, such as are obtained by an electron microscope, reveal fine structure that often differs over the area of a given sample, as well as from sample to sample. Low-magnification pictures look better, but don't eliminate the problem. The trend towards integrated circuits, and away from circuits fabricated utilizing separate components, is very strong in many areas of electronics. A typical silicon monolithic integrated circuit, still in place in the wafer on which it was fabricated, is shown in Fig. 1. The increased reliability which is being experienced through the use of integrated circuits can, to a large extent, be credited to the reduced complexity of the interface system that is present in the electronic system. A glance at Fig. 1, however, with all of its epitaxial and diffused p-n junctions, and interconnect system, shows that interfaces have been far from eliminated. Fig. 2, depicting a schematic cross-sectional view of a (partial) typical integrated circuit, illustrates in detail the numerous interfaces that occur in this type of structure. Besides the individual circuit elements, there are interfaces for isolation, and, Fig. 3, even a crossover requires a series of interfaces. What has been accomplished, however, irrespective of whether or not the total number of interfaces in the circuit is increased or decreased, is that the variety of interfaces is very much reduced. This is because there are fewer materials involved. Since the expense incurred in an R & D program to improve reliability is pretty much directly proportional to the variety of interfaces involved, it is economically advisable to work with integrated circuits for highest reliability. That is not to say that circuits built using standard components could not be made as reliable as integrated circuits, but that the expense involved because of the more complex over-all interface system would be much greater. Although electronic performance utilizing integrated circuits with all silicon elements (i.e., transistors, diodes, resistors, capacitors) is adequate for many applications, there are numerous instances where thin-film passive elements must

Jan 1, 1965

By G. St. J. Perrott

ONE of the important hazards in coal mining is the danger of ignition of explosive mixtures of methane and air or coal dust and air, or both, by the explosives used in blasting the coal. It has long been recognized that certain explosives are more dangerous than others in this respect. In America and abroad, government testing stations have been established for officially passing on the suitability of explosives for use in coal mines. In this country the Federal government is given no power to enforce the use of the approved explosives but merely publishes from time to time, through the Bureau of Mines, those explosives which have passed the tests necessary to place them on the list for use in coal mines. In spite of this lack of police power, the increase in the use of permissible explosives since the promulgation of the first list in 1909 has been rapid. In 1912, only 8 per cent. of the explosives used in coal mines were permissible; in 1925, this figure had increased to 25 per cent. While the past record of permissible explosives has been most gratifying, it is very desirable that we pave the way for further improvement in explosives and blasting methods by learning more about the mechanism of ignition of gas and coal dust by explosives. To this end a considerable amount of investigative work already has been carried out and a large amount yet remains to be done. It is the purpose of this paper to discuss briefly the effect of the characteristics of explosives and method of loading in the borehole on the liability of a blown-out shot to ignite explosive mixtures of gas or dust. For an account of the methods by which an explosive is tested for permissibility for use in coal mines, the reader is referred to Schedule 17-A of the U. S. Bureau of Mines.

Jan 10, 1926

By C. Wert, P. Bunn

Determination of the solid solubility of gases in metals is usually done by one of two methods. The first is an additive method, in which measurement is made at temperature of the maximum amount of gas absorbed by an initially degassed piece of the metal. Gas additions are made until the dissolved gas first comes into equilibrium with a compound. This method is most useful at relatively high temperatures where the amount of gas absorbed is relatively large and where equilibration of the dissolved gas with the gas atmosphere can be achieved in a relatively short time. The second is a precipitation method. A supersaturated solution of the gas in the metal is held at temperature until equilibrium is established between the gas atoms in solution and a compound. The quantity of dissolved gas is then determined by some physical measurement which is sensitive only to the gas in solution. This method is generally useful in low temperatures. This paper describes measurement of solubility of nitrogen in tantalum whereby measurements at low temperatures using internal-friction methods are plotted together with existing measurements at high temperatures. The solubility is thereby known from less than 0.5 at. pet at 350°C to near 13 pet at 2300°C. Several measurements have been reported of the solubility of nitrogen in tantalum. These are collected in Fig. 1. Three single determinations by Ke,1 Andrews,2 and Brauer and zapp3 are plotted along with a series of measurements by Vaughn, Stewart and schwartz4 and Gebhardt, Seghezzi, and Fromm.5 Although not much doubt exists about the solubility being in excess of 10 at. pet above 2000°C, the solubility indicated at low temperatures depends on whose data are selected as being most reliable. The variation is enormous, being at least an order of magnitude at 500°C. Accordingly, a measurement was begun to examine this discrepancy. The method of measurement finally selected was that of internal friction. A solid solution of nitrogen in tantalum was prepared by heating a tantalum wire in a dilute at-

Jan 1, 1964

By G. P. Airey, R. F. Mehl, T. A. Hughes

The coarsening of cementite particles in a ferrite matrix has been studied in a series of steels with 0.15 pct C only and 0.15 pct C plus 1 pct Ni, Mn, and Cr, respectively. Two initial states were employed: quenched nartensite, and quenched and cold-rolled martensite. A series of tempering temperatures between 500' and 700" and tempering times of up to 190 hr were used. The structures were studied by replica and transmission electron microscopy. Particle size distribution curves were determined. From the average size value coarsening curves were obtained. These were plotted in accordance with the Wagner analysis assuming diffusion control. A discussion of the significance of the results is given. L HE reactions occuring upon the tempering of martensite have long engaged the attention of metallurgists. The latter stages, when cementite particles coarsen in a ferrite matrix, have been studied both qualitatively and quantitatively. Studies of such coarsening processes have recently been spurred by the publication of the Lifshitz-Wagner theory1, and the extension of this to the a Fe-Fe3C system by Oriani3 and by Li, Blakely, and einold. Following Wagner the coarsening process is often designated as "Ostwald Ripening". The only quantitative data on the rate of coarsening, except for the work of Hyam and uttin,' in the a Fe-Fe3C system are those of Bannyh, Modin, and odin' for a commercial eutectoid steel and those of Heckel and ereorio" using a pure eutectoid steel. The data of Bannyh, Modin, and Modin have been employed by 0riani3 to derive the a Fe-FeE interface energy. The reaction is one of the most important ones in steel and is worthy of detailed study. This is the purpose of the present study. Laboratory heats were prepared; these were steels with approximately 0.15 pct C, selected so that the num ber of carbide particles would be relatively small and thus so that the overlapping diffusion fluxes would be minimized, presumably a desirable circumstance.'-3 In addition to Fe-C alloys, comparable heats containing 1 pct of Ni, Mn, and Cr, respectively, were included with a view of appraising the effect of alloying elements. This report includes an account of the micro-structures observed, primarily with the electron microscope, and of kinetic data and their interpretation. MATERIALS AND TREATMENT The alloys were prepared from electrolytic iron ("Plastiron") and high-purity graphite; these were melted in a zirconia crucible using a vacuum furnace. The alloy steels were made by adding electrolytic nickel, electrolytic manganese, and "vacuum grade" chromium, respectively, under a partial pressure of argon. Each melt was poured into a mold within the vacuum furnace and cooled in the mold. The ingots were 2 in. in diam. and 8 to 10 in. long. The analysis of the alloys is given in Table I. These ingots were hot-rolled to strip 0.1 in. thick, then cold-rolled to 0.05 in. and each alloy split into two batches. One batch was austenitized at 1200 for 1 min, quenched in cold brine, then cold-rolled to 0.02 in.; samples given this treatment are hereinafter designated as "worked". The other batch was cold-rolled to 0.025 in., austenitized at 1200" for 1 min, and quenched in cold brine; such samples are hereinafter designated as "quenched". These two batches were then tempered, as below. The purpose of the treatment given the first batch was to provide an initial structure of cold-worked martensite, with the expectation that the additional defect structure created by cold work would encourage a higher rate of nucleation of cementite on tempering and hence a more uniform distribution of cementite particles. Individual specimens were sealed in evacuated quartz or Pyrex tubes, then tempered in a muffle furnace. The temperature control was better than 3'C at 700. Tempering treatments wer: performed at 400°, 500°, 550°, 600°, 65o°, and 700C for time periods between 15 min and 190 hr. PREPARATION OF SPECIMENS Specimens for optical and replicalelectron microscopy were mounted, polished conventionally, and etched with 2 pct nital. For electron microscopy, single-stage "formvar" replicas were made, dry-stripped and rotary-shadowed with chromium at an angle of 30 deg. Carbide extraction replicas were prepared from electropolished specimens usirig the method described by Smith and uttin.' Thin foils for electron transmission microscopy were prepared by chemical thinning in an H202-HF bath prior to electropolishing in a chromium trioxide-acetic acid solution. The most

Jan 1, 1969

By Milton E. Wadsworth, John N. Ong, W. Martin Fassell

The temperature and oxygen concentration dependence on the reaction of sphalerite in oxygen at pressures from 6 to 640 mm Hg have been investigated in the temperature range 700° to 870°C. Sphalerite has been found to oxidize linearly over this entire temperature and pressure range. At higher rates, considerable self-heating was observed. The dependence of the oxidation rate on the oxygen concentration may be expressed by: Rate = k' where k' is the specific rate constant and 0 = K1[O2]/(1 + KI[O2]), where K1 is the equilibrium rate constant for the adsorption of oxygen on sphalerite. Values of the activation energy and the enthalpy of adsorption were found to be 60.3 and —59.6 kcal per mol, respectively. Data have been presented that indicate conditions under which either a sulphatizing or an oxidizing roast may be obtained. ROASTING processes have been employed in the metallurgy of a great number of basic metals in use today. Until recently, however, little attempt has been made to deduce the fundamental mechanism by which oxidation takes place. Structural changes upon oxidation have been investigated1 = and thorough work has been performed with regard to the reaction products and the thermodynamics of the oxidation reactions. The objective of this investigation was to determine the rate of oxidation of sphalerite and to apply the absolute reaction rate theory in the theoretilcal interpretation of the experimental results." "O Description of Apparatus The apparatus contains the following features: 1—a furnace with gas system, 2—an autographic weighing system, and 3—a temperature control system. Furnace With Gas System—The furnace was mounted by a yoke on each end and was free to travel up and down on steel guide rods, permitting the introduction and removal of samples from the apparatus with minimum difficulty. The furnace was heated by three sections of Kanthal wire wound externally on a zirconia tube and insulated with Fiber-frax. Pure gases or mixtures of gases were introduced into the lower end of the furnace through two flowmeters, a mixing chamber, and a gas-tight sparger, Fig. 1. The gaseous products of the reaction and the unused gases were prevented from escaping to the atmosphere by maintaining a small negative pressure on the system. This procedure permitted air from the outside to enter through the small an-nulus around the quartz suspension fiber and prevented the escape of the internal gases. Autographic Weighing System—The autographic weighing system consisted of an adapted gold balance, a photoelectric circuit, and a weight recorder, Fig. 2. The sample was suspended from one end of the balance beam by means of a platinum chain outside the furnace and a long thin quartz fiber on the inside of the furnace. On the other end of the balance beam, the necessary weights were added to counterbalance the sample. In addition, a calibrated chain was added to the balance which was linked directly to the weight recording unit. Control was effected by means of a photoelectric circuit." A parallel beam of light from a strong source was directed onto a small front-surfaced aluminum mirror mounted in the middle of the balance beam and then to a front-surfaced mirror mounted on the ceiling of the room. The beam was then reflected onto a front-surfaced right prism at a distance of 9 ft from the balance

Jan 1, 1957