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By D. Cronin, A. Plumtree, A. Hosseini

"Crack in corrosion (CIC) linepipe defects are hybrid defects not directly addressed by existing assessment methods. To investigate the collapse pressure of these defects, CIC defects were formed in 508 mm (20 in) diameter, 5.7 mm thick API X52 linepipe. These defects were 200mm long and varied in depth from 3.0 to 3.8 mm. The respective failure pressures decreased from 14.3 MPa for the plain pipe to 7.9 and 6.2 MPa respectively. A standard FAD method was applied to evaluate these defects as equivalent length and depth cracks, predicting the rupture pressure conservatively by 18% on average. However, when assessed as equivalent cracks with a reduced wall thickness corresponding to the corrosion depth, the predicted collapse pressures were more accurate, approximately 14% conservative on average.INTRODUCTIONPipelines are a safe and efficient method for transporting high volumes of oil and gas. However, aging pipelines may experience defects, such as cracks or corrosion. Present approaches include detection, assessment and repair of defects before they may become critical to the integrity of the line. There are different codes and standards for assessing pipeline defects, depending on the type of defect, with API 579 (API, 2000) being the most common code for the assessment of cracks in oil and gas pipelines . Corrosion is commonly assessed using RSTRENG (Kiefner & Vieth, 1989). Other methods such as the Finite Element method and the CPS method (Cronin & Pick, 2002) may be used for crack and corrosion, respectively.At present, there is no specific method or procedure for assessing crack in corrosion (CIC) defects, and as a consequence there is a need to provide an assessment and evaluation of the integrity of these defects in order to determine the requirements for defect repair or hydro line testing. Hence, the goal of this study was to provide guidance for the assessment of CIC defects for linepipe.CRACK IN CORROSION DEFECTS (CIC)Significant amounts of corrosion and cracking are not generally found together (Hosseini, 2010). However, a new hybrid defect including cracking within corrosion (CIC) has been identified in operating pipelines. In this case, cracking coincident with corrosion (schematic shown in Figure 1) provides the motivation for the current study."

Jan 1, 2012

By G. C. Bateman

THE Workmen's Compensation Act of Ontario was passed in 1915 and Miners' Phthisis was added to the list of compensable industrial diseases in 1916. Under this provision of the Act only about two cases were compensated per year. In 1924, The Department of Public Health made a survey of miners in the four principal camps-Sudbury, Porcupine, Kirkland Lake and Cobalt--and the survey indicated that an alarming proportion of the men exposed to dust had silicosis in one or other of its several stages. A number of conferences were held between representatives of the Department of Mines, the Department of Public Health, the Compensation Board and the mine operators. The operators were advised that in the earliest stages of silicosis there was no physical disability and if men in that stage were removed from underground there would be little danger of permanent disability. They were further advised that if active steps were taken at once to compensate men that had some real disability and remove from the mines men in the early stages of silicosis, the first cost would be the greatest and thereafter their liability should decrease. As a result of this advice, and having at that time no reason to doubt the findings of the survey, the operators agreed to do all that was asked of them and cooperate with the Government in the steps believed necessary to meet the situation, and to provide compensation for the men affected. Amendments In 1926 Arrangements were made for the necessary amendments to the Mines Act and the Workmen's Compensation Act and these amendments were passed in 1926. The Amendment to the Mines Act provided that all underground employees must be the holders of certificates certifying that they were free from tuberculosis of the respiratory organs and further provided that the certificates must be renewed annually. The Government, however, at that time refused to adopt a form of certificate for applicants certifying as to their physical fitness for underground work. The Amendments to the Compensation Act defined both silicosis and

Jan 1, 1937

By B. P. Watson, D. Hoffmann, D. P. Roberts

Potholes on the Merensky and UG2 reefs in the Bushveld Complex occur as near-circular to elliptical depressions or slumps on the reef horizon, normally presenting as severe disruptions which prevent economic extraction. Within the pothole, the reef and other strata may either be attenuated, absent, or highly deformed, this being the result of the overlying hangingwall strata having slumped down. The hypotheses for pothole formation involve several mechanisms, including downward erosion, upward fluid movement, or synmagmatic deformation. When potholes are exposed in mine workings, significant fracturing is often observed. This fracturing is particularly evident in anorthosite rock types. Stress measurements were conducted in a pothole on the Merensky Reef to determine if the fracturing was due to high stress conditions. The paper describes the measurement results and numerical modelling that was done to determine the influence of depth and mining on the stress condition at the site. The results show that high stresses do exist in at least some potholes, and that current formation theories do not adequately explain the measured stresses. In support of understanding the high local stress associated with the pothole, the study explored several rock engineering modelling processes to validate the conditions of the study site and enclosing excavations. A better understanding of the stress conditions in potholes with additional data could lead to more appropriate support design and avoidance of potential rockbursts in these structures.

Jan 1, 2021

By WenFeng Li

Comparing to the coal seams in Eastern China, the coal seams in Western China usually have better geological conditions. Therefore, changes in the conventional gateroads layout are required for the Western longwalls. A case study based on a Western coal mine (LiMin) was presented to discuss the feasibility of an innovative gateroads layout. Based on the geological conditions, a 5m wide pillar between the adjacent two longwall panels, 09112 and 09113, was proposed in order to increase the recovery rate. More importantly, the entry supporting strategy of panel 09113 headgate needed to be determined and verified carefully since only 5m wide pillar was left to separate the entry from the panel 09112 gob. Three strategies with different supporting intensities in the panel 09113 headgate were evaluated by numerical modeling. The model outputs indicated that roof and rib boltings plus single hydraulic props were essential to maintain the gateroads stable. Field observation showed that under the proposed entry supporting strategy, the total roof-tofloor and rib-to-rib convergences were only 360mm and 460mm, respectively, during the service life of the panel 09113 headgate, which indicated that the innovative gateroad layout proposed in this paper is suitable for longwalls with similar geological conditions in Western China.

Jan 1, 2013

By Arthur C. Simmons

The area that produces Pennsylvania grade, which includes New York, Pennsylvania, West Virginia and a part of Ohio, increased its production in 1942 about 1,580,000 bbl. over that attained in 1941. Such an increase is substantial for this area, and measured in terms of increased output of lubricants, for which the crude is particularly suitable, it represents a needed arid worth-while addition to the lubricant resources of the United States. The year 1942 was a difficult operating period for most of the petroleum-producing areas in the United States, but the Appalachian region, owing principally to its location, type of operations, and crude value, suffered less from war influences than other areas. The state of Pennsylvania produced 17,823,870 bbl. of crude oil, which is approximately 63 per cent of the total production of Pennsylvania grade in the entire area. Production Bradford Field The Bradford field, which produces almost wholly by water-flooding methods, increased its production nearly 4000 bbl. per day over 1941 despite a very slight reduction in total number of wells completed. Well completions in the Bradford field (in both New York and Pennsylvania) includc both producing oil wells and water-intake wells. About half of the well completions are producing oil wells and the remaining half are water-intake or injection wells. About 10 per cent of the total well completions of the Bradford field were in Cattaraugus County, New York. No segregation of well completions is available, so that precise statistics cannot be given for New York and Pennsylvania.

Jan 1, 1943

By Arthur C. Simmons

The area that produces Pennsylvania grade, which includes New York, Pennsylvania, West Virginia and a part of Ohio, increased its production in 1942 about 1,580,000 bbl. over that attained in 1941. Such an increase is substantial for this area, and measured in terms of increased output of lubricants, for which the crude is particularly suitable, it represents a needed arid worth-while addition to the lubricant resources of the United States. The year 1942 was a difficult operating period for most of the petroleum-producing areas in the United States, but the Appalachian region, owing principally to its location, type of operations, and crude value, suffered less from war influences than other areas. The state of Pennsylvania produced 17,823,870 bbl. of crude oil, which is approximately 63 per cent of the total production of Pennsylvania grade in the entire area. Production Bradford Field The Bradford field, which produces almost wholly by water-flooding methods, increased its production nearly 4000 bbl. per day over 1941 despite a very slight reduction in total number of wells completed. Well completions in the Bradford field (in both New York and Pennsylvania) includc both producing oil wells and water-intake wells. About half of the well completions are producing oil wells and the remaining half are water-intake or injection wells. About 10 per cent of the total well completions of the Bradford field were in Cattaraugus County, New York. No segregation of well completions is available, so that precise statistics cannot be given for New York and Pennsylvania.

Jan 1, 1943

By M. Tanaka, S. Kita, Y. Jinnouchi, Y. Sawada

This paper generalizes the results of the recent theoretical and experimental investigations on the air-pulsated jigs in Japan. The pulsating mechanism is analyzed as a special vibratory system, and the jigging mechanism as a mass system subjected to the law of hindered settling. The results of investigations on the following items are reviewed: dynamics of the pulsating mechanism; pulsation in a practical TACUB jig development of a new type of air valve; uniform pulsation in a large Baum jig; motion and mobility of bed particles; separating speed in hindered conditions; and standard deviation in practical jigs.

Jan 1, 1985

By R. Patel, D. R. Taylor, P. M. Varley

In-situ measurements of ground stress were made from surface boreholes, using overcoring and hydrofracturing techniques, to obtain data for the detailed design of the underground works at Pergau. Unexpectedly low stresses were measured and appeared to correlate with apparent hydrofracturing observed during permeability testing. The low values of the minor principal stress had a major impact on design, particularly of the lining for the pressure tunnel and shaft. Additional hydrofracture tests were made underground during construction of the low- and high-pressure headrace tunnels and the pressure shaft, to define the vertical reduction in the minor principal stress with overburden. These data were then used to locate and design the steel and reinforced concrete linings

Jun 19, 1905

By G. Paul

The mechanism of nodular crystallisation of graphite in the production of spheroidal cast Iron is not fully understood. The work reported In this paper confirms that in cast iron melts having a high Interfacial tension against the environmental atmosphere, the graphite tends to crystallise in nodules during solidification. The Influence of Interfacial tension between melt and solid graphite is similar.

By Masakazu Takano, Koji Suzuki, Naotoshi Shinkawa

"Cement deep mixing (CDM) method successfully applied to a marine construction project in northern Vietnam is reported. The method is classified as wet method, in which cement slurry is injected into the ground. Thickness of clayey deposit subjected to improvement is from 20 m to 28 m, and the total volume of CDM improvement exceeds 460,000 m3. This is the first massive application of CDM method in the region. Three CDM barges, each equipped with four mixing shafts, were brought to the site in order to finish CDM work within a period of seven months. Cement content used in the work was 180 kg/m3 and water-cement ratio of slurry was 100%. Unconfined compression strength of stabilized soil was 1,200 kPa to 1,600 kPa in average with coefficient of variation from 0.3 to 0.4. Statistics analysis of the strength with these values gave percentage of lower strength less than 10%. Trial use of needle penetration test performed to study strength profile of a CDM column is also reported.INTRODUCTIONThe site of Lack Huyen Port Infrastructure Construction Project is located in the sea adjacent to Cat Hai Island, offshore Hai Phong city which is around 100 km east of Hanoi, the capital of Vietnam. Left side of Fig. 1 shows the location of the site. The project contains development of container terminal, dredging of waterway, construction of sand protection dyke to prevent waterway from being buried, and bridge construction to connect the island to the mainland.Joint venture of Penta Ocean Construction and Toa Corporation was awarded Package 6 of the project, in which reclamation of container terminal area, retaining wall construction and terminal road construction were included. Plan of the site is presented in right side of Fig. 1. The site work has been started in June 2013 and is scheduled to finish within 4 years."

Jan 1, 2015

By Willie M. NeSmith

Conventional augered, cast-in-place (ACIP) piles were introduced into the New York City area as a result of the damage to existing structures caused by pile driving operations. ACIP piles are often specified where deep foundations are to be installed adjacent to transit facilities, sensitive underground utilities or in close proximity to existing structures. However, loss-of-ground issues associated with the installation of ACIP piles have prevented the wide-scale use of these systems. Beginning in 2002, Berkel & Company Contractors, Inc. began using its augered, cast-in-place displacement (ACIPD) system in the New York City area. Like conventional ACIP piles, this system produces almost no vibration. Also, as almost no material is brought to the surface, there is no opportunity for loss of ground. This paper presents a description of Berkel's displacement pile system and a brief discussion of six projects in the New York City area that have been executed with this system over the past two years.

Jan 1, 2004

By P. J. Petit

Financial evaluation is necessary to investigate the viability of implementing and/or utilising new technology in mining projects. It establishes a techno-economic base for decision-making and justifies capital expenditure. This paper aims to present a monetary appraisal of the electric rock drilling system in a typical feasibility project, whose purpose is to increase the production rate. The in situ environment is a platinum orebody, and the stoping operations occur in UG2 reef. The results are a function of production requirements, technical parameters and financial outlay of the drills. The costs involved in implementing and operating electric rock drills are assessed to the current method of drilling, namely the compressed air operation. A comparison of the electric and pneumatic rock drills in terms of financial outlays for drilling and service requirements, peripheral equipping and training is discussed. Other factors that affect the business case are technical advantages, safety and risk management and the environmental objective of the company.

Jan 1, 2006

By L. Yan, N. Damiano, J. Bickson, E. Bauer, D. Yantek, B. Whisner, M. Reyes, J. Srednicki

Built-in-place (BIP) refuge alternatives (RAs) are designed to provide a secure space for miners who cannot escape during a mine emergency. Heat and humidity buildup within RAs may expose miners to physiological hazards such as heat stress. To minimize the risk of heat stress, Title 30 Code of Federal Regulations (CFR), or 30 CFR, mandates a maximum allowable apparent temperature (AT) for an occupied RA of 35°C (95°F) [1]. The National Institute for Occupational Safety and Health (NIOSH) has conducted extensive research on the thermal environment of occupied RAs intended for use in underground coal mines. NIOSH research has demonstrated that a fully occupied BIP RA can exceed the AT limit by >5.6°C (10°F) in mines with elevated mine strata and air temperatures. In this circumstance, an RA cooling system could provide a solution. This paper provides an overview of test methodology and findings as well as guidance on improving the performance of a cryogenic air system prototype by optimizing the flow rate, increasing the tank storage capacity, and improving the efficiency of the heat exchanger of the cryogenic system. This may enable BIP RAs to meet the 35°C (95°F) AT limit in mines with elevated temperatures. The information in this paper is useful for RA manufacturers and mines that may choose to implement a cryogenic air system as a heat mitigation strategy. INTRODUCTION The apparent temperature inside an occupied RA could be significantly affected by the surrounding environment’s thermal conditions, such as mine air temperature and mine strata temperature. Apparent temperature (AT) is a temperature-humidity metric for the perceived temperature caused by the combined effects of air temperature, relative humidity (RH), and air velocity. It is used to assess the perception of indoor temperatures. Depending on factors such as geographic location and season, mine air temperature, relative humidity, and mine strata, temperatures can vary significantly [2]. RAs located in cold mines may pass the 96-hour 35°C (95°F) AT limit test that poses a challenge for RAs located in hot mines. One solution in these cases is that the occupancy of the RA could be derated (i.e., the RA occupancy could be reduced) to ensure the AT limit is not reached. However, this would require mines to purchase additional RAs to accommodate all personnel in the mine. For mines with high temperatures (above 26.7°C or 80°F), the occupancy might have to be reduced so much that the necessary number of additional RAs would be impractical. In these cases, RA cooling systems could provide a solution.

Jan 1, 2019

By D. V. Carter, Dan C. Williams, John R. Coombs

Exploration was active in East and East Central Texas during 1944. Ten oil fields were discovered during the year, of which four show promise of development. The discovery wells of the Sand Flat and Tyler, South fields were drilled to a depth greater than 10,000 ft., and the latter field now produces from the Pettit at a depth of 9890 ft. The Sand Flat well was plugged back to the Paluxy. The other two fields are Glen Rose producers near 8000 ft. The Pickton field produces from the Bacon Lime and Winnsboro from the Rodessa section. The Eylau field, Bowie County, was significant as the first Smackover production in Texas. Magnolia drilled a test in the Concord field, which topped salt. The most extensive and significant development in the district was the Carthage gas-condensate field. It expanded from the 8000 acres of last year to an estimated 190,000 acres, or about 300 sq. miles, and is not defined as yet. The first oil production in the Carthage area was made from the Travis Peak in 1944 in the Rogers Lacy's Cameron Lumber Company well No. I, on the northwestern side of the field. The New Hope field, Franklin County, scored the largest number of completions during 1944 with 24, bringing its total number of wells to 27. Two more pays were opened and produced as dual completions with the older horizons. The Manziel field, Wood County, had 19 new wells added during the year, for a total of 29, while the Pittsburgh field, Camp County, reached a total of 23 wells by completing 14 new ones. Material shortages and drilling restrictions dropped the total number of producing wells completed in the district from 171 during 1943 to 141 for 1944. Abandonments increased from 531 during 1943 to 609 for 1944. Of this number, 479 were in the East Texas field. Subsidy payments had very little effect in the district and it was mostly a few of the old fault-line fields that had any wells to fall within the requirements for subsidy payments. The prices of crude oil remained constant in the district except for increases as a result of subsidy payments. Production and Probation Wartime demands called for increased allowables for many fields, consequently the condensate and oil production for 1944 increased to 190,016,180, which is up 6.9 per cent over 1943. The East Texas field, of course, remained the principal producer of the district, accounting for 134,768'499 bbl. during the year, or 71 per cent of the district total production of condensate and oil. The field topped its own 1943 production by 4.8 per cent and became the first field in the world to produce 2 billion barrels of oil. The Hawkins field remained the second largest oil producer in the district, with 13,317,088 bbl. for the year, a drop of 6.8 per cent from 1943, while Van field was third with 11,635,708 bbl. The

Jan 1, 1945

By Nicholas S. Lynn

Introduction Borne out of the need for reductions in capital expenditure and increased production, several new and innovative carbon systems have been developed for small precious metal heap leach operations throughout the United States. Perhaps the most important aspect of these systems is the carbon column. Though diverse in design, these columns can be categorized into three basic types. The first is known as the gravity flow type or Cortez type. As the name indicates, solution flows via gravity, throughout 4 to 6 columns which are arranged in a normally stepped con- figuration which is conventionally upflow in design. The second type, known as the vertical column, is an arrangement whereby flow is established through pressurization in an upward manner, throughout 4 to 6 columns in a vertically stacked configuration. This arrangement is typically intended for use with small portable heap leach operations and employs a semi-continuous mode thus preventing gravity from occurring. The third type and newest development in carbon columns is an arrangement whereby the solution flows throughout 4 to 6 columns placed in a side by side configuration and pressurized by a single feed pump (Figure 1). A unique aspect to the third type, is that the adsorb and desorb cycles are accomplished in the same column, due to a fixed carbon charge. An in-depth analysis is warranted due to numerous advantages of this arrangement, and is therefore the subject of this paper. Advantages and Variations One advantage to the third type of carbon column is the fact that initial capital expenditures and operating man- power requirements are reduced. Another advantage is that the system can be made fully portable up to a 0.0315 m3/s (500 gpm) capacity. Systems of this nature are operational at several sites. Above this flow rate, the system's portability is one which can be maintained, but disadvantages (i.e. larger diameter carbon column and greater weights) far outweigh the advantages. There are several variations in each of these systems which allow for unique operation. For example, carbon columns made highly portable, can be moved from unitized heap leach operations to central stripping facilities. Although this method has been used in Colorado, transportation of these units has been known to be quite cumbersome. If distances exceed 5 km (3.2 miles) then special front-end loaders are required. This limits heap locations to within 5 km (3.2 miles) of the central processing facility. Another example transports the carbon charge from the heap leach locations to a centralized processing facility; this method is quite effective. For the past 5 years one mine has employed this technique of transporting carbon in 907 kg (1 ton lots), in DOT containers, towed by company pick-ups. This operation uses a vertical column with a 907 kg (1 ton) carbon charge. A third example uses static carbon columns with fixed carbon charges. Carbon Adsorption System The carbon adsorption system (Figure 1) is fed by a single preg solution feed pump. This feed pump pushes the preg solution through all four to six fixed charged carbon columns, which are on line. The sequencing of the carbon columns is achieved using valves. Expansion of the carbon charge is dependent upon the carbon selected. The carbon typically used is a 6 x 12 mesh size, with a nominal flow rate of 0.00135 - 0.00138 m 3/s (22-25 gpm) per square foot of carbon, based on a 40% bed expansion. With 8 x 16 mesh size,

Jan 1, 1987

By Leszek Blacha

Since several years aog there is noted an increasing importance of the metallurgical vacuum technologies. This refers mainly to the extra furnace steel treatment processes, melting of steel and special alloys in the induction and arc vacuum furnaces, as well as refining processes of nonferrous metals. In the presented work, there is discussed a phenomenon of evaporation of volatile components of metal bath under reduced pressure with description of kinetics of this process. In this article are presented are the evaluation of the mass transfer coefficients in the melt and gaseous phase. Based on results of our own research on removal rate of impurities from liquid copper (bismuth, lead) in vacuum refining process, it is determined the thickness of hypothetical boundary layer in the gas phase. This allowed to formulate a general kinetic equation defining the evaporation rate of gaseous components from metal bath. The values of mass transfer coefficients determined from this equation were compared with experimental results by other authors working on the evaporation effect of melt components of metal alloys.

Jan 1, 2006

By D Larson, M Finger

Chemical explosives may become a key element in many of the in situ energy and mineral recovery methods under development. This paper discusses the potential role of explosives in deep rock mining for resource recovery. Several energy and mineral recovery programs described are an outgrowth of the Plowshare Program and Explosives R&D conducted as part of the AEC/ERDA mission at Lawrence Livermore Laboratory. Several important aspects of the use of explosives in deep rock mining are reviewed. First, the status of knowledge of deep rock fracturing to create permeability underground is discussed. Completely contained blasting has not been a widely applied tool used in the mining industry. We conclude that data available on deep rock fracture is minimal and that the mechanisms that control the processes must be understood before technical and economic feasibility can be established. We also discuss the unusual problems in the selection of an explosive or blasting agent for deep rock applications including emphasis on the functioning at depth and safety aspects. Finally, a brief review of similar activities within the U.S. is given.

Jan 1, 1976

By E. M. Wise

THE properties required of gold alloys for jewelry are not well standardized, due in part to problems peculiar to certain branches of the jewelry industry, in part to the individual preference of the fabricator and to his willingness to cope with certain difficulties in manufacture, which arise with the use of certain alloys. GENERAL REQUIREMENTS In general, the properties desired may be classed as follows: 1. Color should conform to the dictates of good taste and smart style. 2. Corrosion resistance and tarnish resistance should be good. This is to a considerable extent determined by the carat. Resistance to such corrosive agents as mercuric chloride as well as certain depilatories is unreasonable to expect and difficult to meet. 3. Strength and hardness must be adequate to maintain the delicate contours of finely modeled jewelry. 4. Wear resistance must be great enough to resist abnormal wear, such as is encountered by a wedding ring in a lifetime of wear. 5. Ductility must be sufficient to permit the fabrication of drawn shells, tubes and difficult shapes. Material having a yield point of not less than 60,000 lb. per sq. in., an ultimate strength of 100,000 lb. per sq. in., and an elongation of 40 per cent. is desirable. 6. Melting point should be between 800° and 1200° C.

Jan 1, 1928

By Robert Goodrich

THERE is a small area about Murray where bedded gold quartz veins occur in Prichard slate. The ore taken from the upper levels, during the early days, was free milling and was treated by stamp milling and amalgamation. There was likewise a considerable placer working. The report is current that tungsten (scheelite) was encountered, which interfered with the amalgamation in the stamp mills and which, in placering, collected in the riffles in the sluice boxes and. clogged them. Consequently, in the quartz mines, the scheelite, when encountered, was rejected, being thrown into the waste, sometimes inside the mine and at other times outside on the clump. The free surface ores became worked out and as the ore in depth became pyritic and rebellious to amalgamation the mines closed down. Last spring tungsten ore brought a high price, near $80 per unit, 60 per cent. W03 and up. This so stimulated the output of tungsten ore that old clumps were explored and waste stored in the mines was gone over. Tungsten was likewise mined from virgin ground. So the district produced quite heavily for a time. The condition now is different. The price is not so high, about $20 per unit W03, which makes profits questionable when mining in new ground. The accumulations from early clay mining have been exhausted and the output has greatly declined. The Golden Chest mine was the heaviest producer of tungsten. The months of June and July were spent at this mine studying the problem. Since the mine had produced both gold and tungsten, we looked forward to the problem of recovering both from what might be called a gold-tungsten ore. A study of the Golden Chest vein showed this not to be so there. While gold ore and tungsten ore come from the same vein, the tungsten ore is confined to a more or less disturbed or distorted portion

Jan 8, 1917

By C. G. Dunn

This note describes a method for revealing micro-structures in tantalum through an {hkl} effect which was found during a study involving amorphous and crystalline tantalum oxides. Three steps are involved. First, an amorphous film of Ta2O5 is formed anodically1 on the surfaces of the tantalum. The amount needed depents on the thickness of the substrate tantalum; 1600Å of oxide, however, is generally satisfactory in the 1/2 -mil (12 µ) to 3-mil thickness range. The film at this point is uniform in color. Second, the anodized specimen is heated to 800°C in. vacuo during a period of a few minutes and held at temperature for 5 min. During such a treatment some oxygen leaves the oxide through dissolution into the substrate tantalum (e.g., at 10-8 Torr oxide films thinner than about 800 completely disappear on 5-mil strip). Considerable crystallization of the amorphous oxide also occurs adjacent to the metal/oxide interface but not throughout the oxide thickness. The thickness of oxide needed as a residue is not too critical; values between 500 and 1000Å (optical estimate') may be most useful. (The presence of a residual oxide layer after the heat treatment usually is not apparent; in fact, in most instances the surfaces have a metallic appearance. This can be the case also for thicker residual films needed in the detection of a crystalline oxide phase by surface X-ray diffraction—e.g., if the initial oxide film is 3000Å thick, enough crystalline oxide is formed for X-ray detection.) The third step eliminates the metallic appearance at the surface and reveals (or produces) a varied colored film of tantalum oxide. Two methods can be used and both will be illustrated. If the specimen is dipped in 48 pct HF for a few seconds, the tantalum is found to be covered with a multicolored oxide. Moreover the colors correlate with the grain structure of the substrate tantalum through an orientation dependence of the type illustrated in Fig. 1, where results of an orientation analysis by the Laue X-ray method have been plotted. Other film conditions would have provided a different set of colors for the same orientations. Any such correlation, however, provides a basis for a qualitative assessment of the distribution of orientations in a large sample. The cold-rolled structure of tantalum foil produced by a recrystallization anneal and a cold-rolling reduction of 95 pct is not easily obtained by usual metal-lographic methods.' The structure, however, is easily revealed by the present technique, Fig. 2. The alternative third step is to reanodize the specimen. The optical nature of the final anodic film depends on the presence of the crystalline oxide phase; color variations indicate optical thickness variations in the film. As the reanodization voltage is increased from zero, straw and light brown colors appear (as usual), followed now by variations in color from grain to grain depending on {hkl} orientation. Suitable end points, which are determined by voltage and time, are easily established. Fig. 3, for example, shows the grain structure developed in 5-mil tantalum strip during a 30-min re-crystallization and grap-growth anneal at 1800°C. An anodic film of 1600Å thickness was added prior to the special 800°C anneal. Reanodization was done at constant current density (near 0.2 ma per sq cm) in an aqueous solution of H3PO4 (0.01 pct) and was terminated after the initial brown colors were replaced by a deep blue at approximately 30 v. Although good grain contrast can be obtained with bright field illumination, even greater contrast for black and white micrographs may be obtained with polarized light, as in Fig. 3.

Jan 1, 1967