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By Charles W. Huggins

Knoop hardness indentations were studied and measured with the electron microscope on TiB2, HfC, and A1B12 crystals. A detailed description of replicating the indentations using collodion and Faxfilm is made. A John Hopkins grating having 28,800 lines per inch was used to accurately determine the magnification used on the electron microscope. The primary objectives were to prepare carbon replicas of hardness indentations, to measure the indenations accurately, and to compare the results with those obtained with the light microscope. The resulting data showed excellent agreement between the measurements made on the replicas with the electron microscope and those made with the optical microscope. The replicas made from collodion showed slightly better agreement with the light optical values than did the replicas made from Faxfilm.

Jan 1, 1963

By N. Dahata

Earlier research has indicated that an addition of titanium master alloy to aluminum alloys, results in improved fillability, grain refinement and finer pores. B206 alloy differs from other alloys used in automotive industry, with lower titanium level. This paper examines the effect of alloy chemistry (copper and titanium levels) and grain refinement (A1-5`)oTi- 1%B grain refiner) on grain size, microstructure and microporosity in B206 aluminum alloy. In this study, characterization of grain size, microstructure and microporosity was carried out using light optical microscopy (LOM) and scanning electron microscopy (SEM). Results have shown that the addition of 0.05 wt % titanium resulted in grain refinement of B206 alloy. With an increase in titanium to 0.25 wt further grain refinement, much reduced pore size and uniform distribution of pores resulted. These results suggest that B206 with proper addition of titanium has a promise as an alloy for automotive casting.

Jan 1, 2007

By R. Kaibyshev, I. Zuiko

"The effect of thermomechanical processing (TMP) including cold working by tension or rolling before aging on mechanical properties and a dispersion of secondary phase particles of an AA2519 alloy (Al–5.64Cu–0.33Mn–0.23Mg–0.15Zr–0.11Ti–0.09V–0.08Fe–0.01Si (wt. %)) was examined. It was shown that the use of tension to impart pre-strain =10% in the alloy provides the best combination of properties in peak aging condition of the material. The AA2519T87 alloy processed by tension exhibits the yield stress, ultimate tensile strength and elongation to failure of 425.4±2.4, 475±2.4, 12.1±0.4, respectively. The one pass rolling leads to -5% decreases in yield stress and –20% decreases in ductility. Dislocations serve as heterogeneous nucleation sites for ?'-phase precipitation. The positive effect of tension is attributed to the formation of more homogeneous dislocation structure, uniform distribution of ?'-phase particles with higher aspect ratio. Precipitation of the O–phase plates on {111}a habit plane was detected. In addition it was shown that the low angle boundaries are heterogeneous nucleation sites for ?' and O particles.INTRODUCTION Precipitation-hardened alloys are a commercially important group of the materials because their mechanical properties can be modified by treating and changing the microstructure. Age-hardenable aluminum alloys belonging to the Al–Cu–Mg system are widely used due to their attractive combination of high specific strength, good fracture toughness and enhanced creep resistance attributed to the highly efficient strengthening by the ?'-phase (Palmer, StJohn, Nie, & Qian, 2017). An AA2519 alloy exhibiting superior mechanical properties among high-strength Al–Cu alloys (2XXX-serie) due to minor Mg additives. It is known that, in alloys with high Cu/Mg ratio (=5.6) the classic precipitation sequence (Palmer et al., 2017; Wang & Starink, 2005; Wang et al., 2010) of supersaturated solid solution (SSSS) decomposition occurs: SSSS ? GP zones (Al3Cu) ? ?? (Al3Cu) ? ?' (Al2Cu) ? ? (Al2Cu) (1)"

Jan 1, 2018

By J. R. Budden, P. A. Spencer, J. Barrett

The initially produced arsenic (III) is very toxic to the unconditioned culture but the mixed culture has the capacity to oxidise it to arsenic (V) in the presence of iron (III). It was possible to build up the resistance of the culture through progressive sub-culturing on arseno-pyrite until it could tolerate steady-state concentrations of 30 mM arsenic (III) and 200 mM arsenic (V). With some samples tested in the continuous systems the final arsenic concentrations reached 330 mM. It proved possible to use the laboratory batch data to establish the optimum operating conditions for continuous test systems with capacities of up to 32 m3. Data on the residence time, oxygen uptake rates and gold extraction from the bio-oxidised residues could then be confirmed by continuous testing without the need first to use empirical means to determine optimum conditions for continuous bio-oxidation. The data on residence time, oxygen uptake rate, solids density and neutralisation could be used to estimate the capital and operating costs of treating any given tonnage of the concentrate of interest. It was established that the arsenopyrite concentrates can be suitably bio-oxidised to cause the liberation of at least 90% of the gold content. The method is simple to operate and is flexible over a wide range of external conditions

Apr 1, 1991

By Y. S. Sun, Northeastern University, W. B. Li, P. Gao, Z. Y. Zhang, J. W. Yu

"The boron-bearing iron concentrate was extracted from ludwigite ore by the process of magnetic-gravity separation. In order to fully utilize the refractory ore and meet the boron consumption of China, a novel process for separation of boron from iron in boron-bearing iron concentrate was proposed in this paper. In particular, laboratory scale experiments of improving boron reactivity were performed. Fine boron-bearing iron concentrate briquettes were reduced by bituminous coal completely at 1125 °C for 150 min. The effect of sodium carbonate, which was used as an additive in the roasting process, was investigated. The addition of sodium carbonate decreased the boron reactivity and facilitated the volatilization of boron. The influence of diverse cooling methods of the reduced samples on the boron reactivity was studied. The results indicated that boron reactivity could reach up to 80.76% when the reduced samples were cooled by rapid water quenching. In addition, the magnetic material containing 92.71 % Fe with a recovery of 95.11 % and boron-rich non-magnetic material containing 14.51% B2O3 with a recovery 88.85% could be obtained by low-intensity magnetic separation. The magnetic material and boron-rich non-magnetic material were good raw materials for steel-making and borax production, respectively.INTRODUCTION Ludwigite ore is abundant in Liaoning province of China, with 28.43 Mt B2O3 accounting for 57% of the boron resources of the country (Liu et al., 2006). However, it has not yet been utilized on an industrial scale due to its complex mineralogy and fine mineral dissemination (Wang, Wang, Ding, Ma & Xue, 2012). At present, boron-bearing iron concentrate and boron concentrate can be obtained from ludwigite ore using magnetic-gravity separation. The boron concentrate contains B2O3 12%~16%, which can be used as a high-quality raw material for the boron chemical industry after activated roasting, but the B2O3 content in the iron concentrate reaches up to 4%~6%. In order to further separate boron and iron from boron-bearing iron concentrate, a blast furnace and a solid pre-reduction followed by electric arc furnace melting have been proposed (Liu, Cui & Zhang, 1998; Wang et al., 2012). However, both of these two current routes face the same crucial problem that molten boron-rich slag has to be cooled slowly to obtain the alkali-dissolution activity of boron, which affects the yield of boron resource."

Jan 1, 2016

By Stephanie Singarayer, Damodara Reddy Chinnasane, Mike Yao, Danielle Pelletier

Mining at Vale’s Creighton Mine has been active for nearly 120 years in Sudbury, Ontario, Canada. Being the deepest mine in the Sudbury region, mining induced seismicity is a common occurrence at Creighton Mine. Over the past five years, 26 large magnitude seismic events ranging from 2.5 Mn to 3.7 Mn (Nuttli) have occurred. Out of these large magnitude events, three 3.0+ Mn events occurred between April 2020 and January 2021. The majority of the 3.0+ Mn events are believed to be the fault-slip type that could be linked to the known major geological structures and/or long-term effect of mining over many years. The recent large magnitude events are believed to be triggered by high induced stresses while mining the first few stopes of a new lower horizon in the top-down centre out mining sequence.

Apr 26, 2022

By Alberto Tremea

The eddy current system is universally recognized as a most suitable method to point out discontinuities or modifications on the roll surface. The automation of the controls through the implementation of sophisticated equipments on the grinding machine has favoured its employment in the roll shop. A big effort is still going on to clarify the best way to promptly identify situations that could be really unsafe for the roll life. The results presented in this paper have been obtained through an intensive activity conducted in field by Innse Cilindri on work rolls of finishing stands of hot strip mills. The correct interpretation of the eddy current signals and a good calibration of the automatic system have allowed, in many cases, a substantial optimisation of regrinding practices.

Aug 16, 2017

By C. D. Rubert, W. J. Parton

A flotation plant was placed in operation in 1945 at the Tamaqua colliery of the Lehigh Navigation Coal Co. Inc., to recover fine anthracite which is discharged from the cleaning plant with the washery water.‡ In addition to the recovery plant, facilities were provided for the complete clarification of the washery water, recirculation of this clarified water for breaker use, and disposal of the refuse solids in a waste impounding dam. Fig I shows a view of the settling tanks and the flotation plant. Flow Diagram The flow diagram for the complete recovery project is given in Fig 2. All the waste water from the cleaning plant is collected in a sump A outside the breaker structure, from which a 7000 gpm pump B delivers it through a 16 in. line to a 75-ft diam hydroseparator C. The hydroseparator, acting as a classifier, is set to give a separation at approximately 200-mesh. The minus 200-mesh overflow is discharged by gravity into the 180-ft thickener D for final settling of the solids. The classifier underflow sludge is pumped to the flotation plant by a 6-in. quadruplex diaphragm pump E. A 10-ft diam hydroseparator F is used to make a second classification on the sludge solids at approximately 28-mesh. The underflow from this classifier containing the coarse particles is elevated by a 6-in. diaphragm pump G and is discharged on two 4- by 6-ft vibrating screens II. These screens are dressed with approximately 28-mesh cloth. Screen oversize product flows directly to the centrifuge that dewaters the cleaned froth. The screen underflow and the overflow from the 10-ft classifier flow to the flotation circuit. The flotation feed is conditioned in a 12 by 12-ft agitator tank J at a pulp density of I:2.33 (30 pct solids). Reagents are fed to the circuit by reagent feeder I. The conditioned pulp is then diluted to a pulp density of approximately I: 5 (18 pct solids) and is fed to two banks of four 100-cu ft froth flotation cells K for primary coal recovery and cleaning. Additional reagents from reagent distributor L are added to the feed weir-box of Nos. 2, 3, and 4 cells of each bank of flotation machines. Clean coal removed from these cells flows directly to the clean-coal sump. Dilute tailings from the primary cells is re-thickened in a 30-ft diam thickener M and is then retreated in a scavenger circuit for final recovery of coal. The scavenger circuit consists of a 6- by 6-ft agitator tank N and two banks of four 24-cu ft froth flotation cells 0. Coal froth from these cells flows to the dewatering equipment and the tailings flows to a vertical refuse pump which delivers it to the 180-ft diam waste thickener D. Dewatering of the coal products is accomplished in a 54- by 72-in Bird centrifugal filter P. The cake product is dropped onto a conveyor and is loaded

Jan 1, 1949

By D. F. Hewett

CONTENTS PAGE Introduction 1 Geologic features of eastern Oregon 2 Geology of the Sumpter quadrangle 2 Rocks older than the ore deposits 3 Rocks younger than the ore deposits 8 Lodes of the Sumpter quadrangle 8 Areal distribution 8 Geologic distribution 9 Major features of the veins 9 Mineralogy and texture of the veins 13 Ore deposits zonally disposed around the Bald Mountain batholith . . . . 13 Summary of mineralogy and texture 32 Zonal relations 33 Ore deposits zonally disposed around Greenhorn Mountain batholith . . . 36 Zonal relations 37 Relation of textural features to zonal arrangement of veins 37 Summary of zonal relations 38 Comparison with similar districts 39 Outlook for the district 40 INTRODUCTION IN an earlier report on the Sumpter quadrangle1 it was briefly stated that the quartz lodes of that region might be separated into several groups or belts on the basis of the kind and abundance of the minerals of which they are composed, and that these belts were disposed as areal zones around the principal intrusive mass of the region. When the opportunity to revisit the region was offered in 1929, as a result of a cooperative agreement between the State Mining Board of Oregon and the United States Geological Survey, it seemed advisable to pay particular attention to this feature of the lodes, in the hope that if the idea of zonal relations was confirmed it might serve as a guide in exploitation.

Jan 1, 1931

By B. Thomas Mansbach

INTRODUCTION The Overseas Private Investment Corporation ("OPIC") is a U.S. Government agency mandated to promote the economic development of the less developed countries ("LDCs") by assisting U.S. private investment in the Third World. Generally, investment decisions turn on the optimism or pessimism of the private sector's financial analysis of a project, with market price of product a major unknown in a very chancy set of projections. Discussions with American mineral companies, however, show that, more often than not, in developing country projects it is the political risks of investing in mineral exploration and extraction that pose the most serious deterrent to investment. In several of the projects described here, investments would not have been made if OPIC had not been involved providing support to the project sponsors and their funding sources. Clearly it is not OPIC's business to promote U.S. investment in a project which is not commercially viable, but OPIC's programs can neutralize the political uncertainties which act as disincentives to investment in otherwise commercially viable projects. That is to say, OPIC's programs are designed to reinforce market decisions and not distort them. Although OPIC is an independent agency of the U.S. Government, it is managed by a Board of Directors, the majority of whom come from the private sector. This, coupled with the statutory requirement that it be self-sustaining and operate with due regard for the principles of prudent risk management, requires that it operate on a business-like basis. Although established as a development agency, to the business public OPIC is both an insurance company and a lending institution, with two major programs which are available to U.S. investors in the minerals sector: its political risk insurance program and its finance program. Each has been specially tailored to the meet needs of the mining industry. The insurance program provides coverage against four basic types of political risk: Currency Inconvertibility, Expropriation, loss caused by War, Revolution and Insurrection and Interference with Operations as a result of an act of War, Revolution or Insurrection. Coverage against the risks of Civil Strife can be added to both War, Revolution and Insurrection coverage and Interference with Operations. Inconvertibility coverage provides protection against a deterioration in an investor's ability to convert local currency into U.S. dollars. This deterioration can be the result of either active or passive delays. Active delays consist of a change in exchange laws or regulations that leads to inconvertibility delays of 30 days or more. For example, if the exchange regulations at the time of contract execution allow an investor to transfer earnings equal to 18% of its registered capital per annum and the government of the host country later changes the law to allow conversion of only 12%, the insured would convert the 12% transferable under the new exchange regulations with the government foreign exchange authorities, delivering the remaining 6% to OPIC for conversion at 99% of the then prevailing rate of exchange. (OPIC does not cover devaluation risks.) Upon delivery of the local currency to OPIC, normally at the U.S. Embassy in the project country, the insured's account in the U.S. would be credited with dollars. Delays can also result from what is termed passive blockage, which includes administrative delays of more than 60 days (sometimes longer) caused by the bureaucratic tie-ups or pigeonholding of transfer requests, as well as delays suffered simply because the government of the host country does not have sufficient foreign exchange. The transfer procedure is the same as with active blockage - the local currency is delivered to OPIC in the project country and OPIC provides dollars in the United States at the then prevailing rate of exchange. The second coverage -- Expropriation -protects not only against the loss of the investment due to the well-known risks of expropriation, nationalization or confiscation by the host government, but also against

Jan 1, 1985

[In presenting this list of permissible explosives and blasting devices, the Bureau of Mines desires to call attention to pages 17 and 23, outlining the conditions in use under which, and only under which, the explosive or blasting device is permissible. In view of publications recounting trade practice favoring the use of a blasting device without stemming, particular emphasis is placed upon condition 4 on page 17 and condition 2 on page 23. An explosive or a blasting device enumerated in the permissible lists of thin Bureau is not permissible in use unless it is properly confined with clay or other incombustible stemming.]

Jan 1, 1941

In presenting this list of permissible explosives and blasting devices, the Bureau of Mines desires to call attention to pages 17 and 23, outlining the conditions in use under which, and only under which, the explosive or blasting device is permissible. In view of publications recounting trade practice favoring the use of a blasting device without stemming, particular emphasis is placed upon condition 4 on page 17 and condition 2 on page 23. An explosive or y blasting device enumerated in the permissible Lists of thin Bureau is not permissible in use unless it is properly confined with clay or other incombustible stemming.

Jan 1, 1941

The Southern 'B' lode orebody at the New Broken Hill Consolidated Limited (NBHC) mine, Broken Hill, is a continuation of the zinc-rich orebody that was first mined in NBHC in the 1940's. Preliminary diamond drilling in the early 1960's resulted in sufficient information to delineate the southern extension of the presently mined 'B' lode orebody, In 1966 the sinking of a 7.3 metre diameter circular shaft (No. 3 Airway) was commenced to improve the ventilation of the southern extremities of existing workings and to provide a base to further explore and develop the orebody extension. Development on four levels was started in the early 1970'.s to link the existing workings with the new shaft. Three possible mining methods - sublevel open stoping, loader cut and fill with ramp access and sublevel caving - were investigated and the decision was made to mine the orebody by transverse sublevel longhole stopes and pillars with trackless equipment and ramp access between the major working levels.

Jan 1, 1977

By Andrea Lisjak Bradley

Clay shales are currently being assessed as possible host rock formations for the deep geological disposal of radioactive waste. However, one main concern is that the favourable long-term isolation properties of the intact rock mass could be negatively affected by the formation of an excavation damaged zone (EDZ) around the underground openings. The goal of this thesis was to develop and validate a mechanically-based model of the deformation and failure process of a clay shale, namely Opalinus Clay (OPA), with particular focus on the influence of anisotropy on the short-term response of circular tunnels. To achieve this goal, a hybrid continuum-discontinuum numerical approach was developed in combination with new field measurements from the Mont Terri underground research laboratory. The response of OPA during the excavation of a full-scale emplacement (FE) test tunnel was characterized by geodetic monitoring of wall displacements, radial extensometers and longitudinal inclinometers. The deformation measurements indicated strong directionality induced by the combined effect of in-situ stress field and bedding planes striking parallel to the tunnel axis, with the most severe deformation occurring in the direction approximately perpendicular to the material layering. Computer simulations were conducted using a newly-extended combined finite-discrete element method (FEM/DEM), a numerical technique which allows the explicit simulation of brittle fracturing and associated seismicity. The numerical experimentation firstly focused on the laboratory-scale analysis of failure processes (e.g., acoustic activity) in brittle rocks, and on the role of strength and modulus anisotropy in the failure behaviour of OPA in tension and compression. The fracturing behaviour of unsupported circular excavations in laminated rock masses was then analyzed under different in-situ stress conditions. Lastly, the proposed modelling methodology was applied to the aforementioned FE tunnel to obtain unique insights into the EDZ formation process around emplacement tunnels for nuclear waste. The calibrated numerical model suggested delamination along bedding planes and subsequent extensional fracturing as key mechanisms of the damage process potentially leading to buckling and spalling phenomena. Overall, the research findings are already having a direct impact on the preliminary design process of an underground repository for nuclear waste in Switzerland.

Jan 1, 2015

By P. Turcotte, E. Karampinos, F. Mercier-Langevin

In some underground hard-rock mines, squeezing compressive ground conditions are influenced by the presence of rock foliation and high stress. In these cases, the orientation of the foliation with respect to the drift direction has a considerable impact on the magnitude of the resulting deformation. Irrespective of the reinforcement and support strategy, keeping drives developed sub-parallel to the rock foliation operational is difficult, and often requires excessive rehabilitation during the lifetime of the excavation. This study uses field observations and convergence measurements at the LaRonde and Lapa mines of Agnico Eagle Mines Ltd to provide guidelines of the anticipated squeezing levels at these operations.

Jan 1, 2015

By S Dunbar, S Harrison, J Cilliers

‘Those who cannot remember the past are condemned to repeat it.’George Santayana (16 December 1863 in Madrid, Spain to 26 September 1952 in Rome, Italy). Philosopher, essayist, poet and novelist.The minerals industry requires specific technical expertise in mining and mineral process engineering, geoscience, environmental science and social sciences to maintain and operate its current business and to develop future projects. A steady supply of new graduates is essential to replace not only retirees, but also those who left the industry during the recent downturn. The supply of trained graduates is however not instantaneous, and there is a four-year lag from entry into university to graduation. It is essential that this lag in human resource supply and a likely shortage of knowledgeable, qualified talent is taken into account when considering risks to the business of mining. The shortage of skilled professionals has in the past resulted in unsustainable salary expectations and is likely to pose financial and execution risk to new projects. This paper will review some recent statistics of students in training from around the world and explore what action is required to not only sustain the training courses that provide future ready talent to the mining industry, but also ensure that graduates from these courses are equipped to create change and be leaders in the industry. The future prosperity of the industry is dependent on delivering sustainable stakeholder returns through the cycle. This will be achieved by developing capable individuals that can respond to the complex, adaptive challenges facing the industry.*This is an abstract only. No full paper was prepared for this abstract.*CITATION:Plint, N, Cilliers, J, Dunbar, S and Harrison, S, 2018. Back to basics: resourcing the mining industry, in Proceedings 14th AusIMM Mill Operators' Conference 2018, pp 33–34 (The Australasian Institute of Mining and Metallurgy: Melbourne).

Aug 29, 2018

By Andrew P. Schissler

The Citronen Zinc-Lead Project is one of the world?s largest undeveloped zinc-lead resources, containing more than 13 billion pounds of zinc and lead metal. The project is located in northern Greenland, a self-governed region of the Kingdom of Denmark (Figure 1). Citronen is the northern-most mine in the world, operating at a latitude of 83o 3? N. In excess of 67,000 meters of diamond drilling have been completed to delineate the resource. As of January 2012, the measured, indicated, and inferred reserves for the Citronen project totaled 70.8 million tonnes, consisting of 5.7% zinc + lead (3.5% zinc cut-off) (Ironbark, 2012). For the underground mine plan, room-and-pillar and long holestoping mining methods were selected. The beneficial application of structural fill was considered for increased recovery, efficient tailings disposal, and ground control. Three types of fill were compared - paste fill, cemented rock fill, and iced tailings. An environmental and economic feasibility study concluded that iced tailings was the preferred alternative provided it met the ground control requirements. The purpose of this paper is to explain the investigatory steps that led to the possibility for the use of iced tailings as structural fi

Jan 1, 2012

By O. A. Knight

THE suppression of the austenite-martensite transformation that can be brought about by the addition of certain alloying elements, such as manganese or nickel, to plain carbon steel has been known for a long time, especially since Guillet's investigation at the beginning of this century. The extent to which the critical range is lowered depends upon the percentage and nature of the special element added. First the Ar1 point is lowered gradually, then at a certain percentage a sudden lowering to about 300° C. occurs. The addition of still larger percentages of the alloy may result in lowering the Ar1 point to room temperature or below, in which case the steel remains austenitic at room temperature, especially after rapid cooling. The effect of alloying elements of this general type on the lowering of the transformation temperature is well illustrated by Sauveur(1)§ in his Fig. 281a, reproduced here as Fig. 1. This type of curve is characteristic of both manganese and nickel though it requires about 2 1/2 times as much nickel as of manganese to produce the same result. The influence of nickel in retarding the transformation of austenite into the lower transition constituents is due to its lowering of the critical range of the steel, which is also well illustrated by Sauveur(1) (after Osmond) in his Fig. 284, reproduced here as Fig. 2. Scott(15) presents a diagram illustrating the effect of manganese on the Ac3 and Ar3 points which is strikingly similar to the diagram above referred to in Fig. 2 concerning the effect of nickel.

Jan 1, 1934

By Karl J. Dreher, Charles C. Hennig, Gregg A. Scott

INTRODUCTION Theodore Roosevelt Dam is a cyclopean-masonry, gravity-arch dam located on the Salt River northeast of Phoenix, Arizona. Construction of the dam began in 1903 and was completed in 1911. The dam is about 85 m high with a total reservoir capacity of about 1.7x109 m3. Raising the dam is now being considered to provide additional water storage and flood control. This paper describes preliminary analyses performed to assess foundation stability for increased loading resulting from raising the dam and reservoir water surface about 12 m. The foundation of Theodore Roosevelt Dam consists of variably metamorphosed limes tones, sands tones, mudstones, and shales. Bedding uniformly strikes nearly normal to the river (N 40º W) and dips upstream at 25 to 30º. The rock is cut by four prominent joint sets as indicated by the joint contour diagram shown in figure 1A. The diagram was developed from surf ace observations and vertical drill core oriented relative to the bedding. Sampling biases account for the differences in concentrations of various joint sets. However, field observations indicate that all sets are relatively prominent, planar, and continuous. SEEPAGE ANALYSES Consistent with practice at the time of construction, no foundation drainage was installed at Theodore Roosevelt Dam. Finite element seepage analyses were therefore performed to study the potential for large uplift pressures in the foundation. The dam has steep abutments and is curved in plan as shown in figure 1B. The effects of modeling the seepage two-dimensionally, radially symmetric about the dam's axis center, and three-dimensionally were therefore com-

Jan 1, 1982

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

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

Jan 1, 1969