11 resultados para Scanning Electron-microscope

em Iowa Publications Online (IPO) - State Library, State of Iowa (Iowa), United States


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The major objective of this research project was to investigate the chemistry and morphology of portland cement concrete pavements in Iowa. The integrity of the various pavements was evaluated qualitatively, based on the presence or absence of microcracks, the presence or absence of sulfate minerals, and the presence or absence of alkali-silica gel(s). Major equipment delays and subsequent equipment replacements resulted in significant delays over the course of this research project. However, all these details were resolved and the equipment is currently in place and fully operational. The equipment that was purchased for this project included: (I) a LECO VP 50, 12-inch diameter, variable speed grinder/polisher: (2) a Hitachi S-2460N variable pressure scanning electron microscope; and (3) a OXFORD Instruments Link ISIS microanalysis system with a GEM (high-purity germanium) X-ray detector. This study has indicated that many of the concrete pavements contained evidence of multiple deterioration mechanisms: and hence, the identification of a single reason for the distress that was observed in any given pavement typically had to be based on opinion rather than empirical evidence.

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The major objective of this research project was to investigate the chemistry and morphology of portland cement concrete pavements in Iowa. The integrity of the various pavements was evaluated qualitatively, based on the presence or absence of microcracks, the presence or absence of sulfate minerals, and the presence or absence of alkali-silica gel(s). Major equipment delays and subsequent equipment replacements resulted in significant delays over the course of this research project. However, all these details were resolved and the equipment is currently in place and fully operational. The equipment that was purchased for this project included: ( I ) a LECO VP 50, 12-inch diameter, variable speed grinder/polisher: (2) a Hitachi S-2460N variable pressure scanning electron microscope; and (3) a OXFORD Instruments Link ISIS microanalysis system with a GEM (high-purity germanium) X-ray detector. This study has indicated that many of the concrete pavements contained evidence of multiple deterioration mechanisms: and hence, the identification of a single reason for the distress that was observed in any given pavement typically had to be based on opinion rather than empirical evidence.

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Concretes with service lives of less than 15 years and those with lives greater than 40 years were studied with petrographic microscope, scanning electron microscope, and electron microprobe to determine why these two groups of concrete exhibit such different degrees of durability under highway conditions. Coarse aggregate used in both types of concrete were from dolomite rock, but investigation revealed that dolomite aggregate in the two groups of concretes were much different in several respects. The poorly-performing aggregate is fine-grained, has numerous euhedral and subhedral dolomite rhombohedra, and has relatively high porosity. Aggregate from durable concrete is coarse-grained, with tightly interlocked crystal fabric, anhedral dolomite boundaries, and low porosity. Aggregate in short service life concrete was found to have undergone pervasive chemical reactions with the cement which produced reaction rims on the boundaries of coarse aggregate particles and in the cement region adjacent to aggregate boundaries. Textural and porosity differences are believed to be chiefly responsible for different service lives of the two groups of concrete. The basic reaction that has occurred in the short service life concretes between coarse aggregate and cement is an alkali-dolomite reaction. In the reaction dolomite from the aggregate reacts with hydroxide ions from the cement to free magnesium ions and carbonate ions, and the magnesium ions precipitate as brucite, Mg(OH)2. Simultaneously with this reaction, a second reaction occurs in which product carbonate ions react with portlandite from the cement to form calcite and hydroxide ions. Crystal growth pressures of newly formed brucite and calcite together with other processes, e.g. hydration state changes of magnesium chloride hydrates, lead to expansion of the concretes with resultant rapid deterioration. According to this model, magnesium from any source, either from reacting dolomite or from magnesium road deicers, has a major role in highway concrete deterioration. Consequently, magnesium deicers should be used with caution, and long-term testing of the effects of magnesium deicers on highway concrete should be implemented to determine their effects on durability.

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The objectives of this research were the collection and evaluation of the data pertaining to the importance of concrete mixing time on air content and distribution, consolidation and workability for pavement construction. American Society for Testing and Materials (ASTM) standard C 94 was used to determine the significance of the mixing time on the consistency of the mix being delivered and placed on grade. Measurements of unit weight, slump, air content, retained coarse aggregate and compressive strength were used to compare the consistency of the mix in the hauling unit at the point of mixing and at the point placement. An analysis of variance was performed on the data collected from the field tests. Results were used to establish the relationship between selected mixing time and the portland cement concrete properties tested. The results were also used to define the effect of testing location (center and side of truck, and on the grade) on the concrete properties. Compressive strength test concepts were used to analyze the hardened concrete pavement strength. Cores were obtained at various locations on each project on or between vibrator locations to evaluate the variance in each sample, between locations, and mixing times. A low-vacuum scanning electron microscope (SEM) was used to study air void parameters in the concrete cores. Combining the data from these analysis thickness measurements and ride in Iowa will provide a foundation for the formulation of a performance based matrix. Analysis of the air voids in the hardened concrete provides a description of the dispersion of the cemtitious materials (specifically flyash) and air void characteristics in the pavement. Air void characteristics measured included size, shape and distribution.

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The freeze-thaw resistance of concretes was studied. Nine concrete mixes, made with five cements and cement-Class C fly ash combinations, were exposed to freeze-thaw cycling following 110 to 222 days of moist curing. Prior to the freeze-thaw cycling, the specimens were examined by a low-vacuum scanning electron microscope (SEM) for their microstructure. The influence of a wet/dry treatment was also studied. Infilling of ettringite in entrained air voids was observed in the concretes tested. The extent of the infilling depends on the period of moist curing as well as the wet/dry treatment. The concretes with 15% Class C fly ash replacement show more infilling in their air voids. It was found that the influence of the infilling on the freeze-thaw durability relates to the air spacing factor. The greater the spacing factor, the more expansion under the freeze-thaw cycling. The infilling seems to decrease effective air content and to increase effective spacing factor. The infilling also implies that the filled air voids are water-accessible. These might lead to concrete more vulnerable to the freeze-thaw attack. By combining the above results with field observations, one may conclude that the freeze-thaw damage is a factor related to premature deterioration of portland cement concrete pavements in Iowa.

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Portland Cement Concrete (PCC) pavement has served the State of Iowa well for many years. The oldest Iowa pavement was placed in LeMars in 1904. Beginning in 1931, many miles of PCC pavement were built to "get out of the mud". Many of these early pavements provided good performance without deterioration for more than 50 years. In the late 1950s, Iowa was faced with severe PCC pavement deterioration called D cracking. Research identified the cause of this deterioration as crushed limestone containing a bad pore system. Selective quarrying and ledge control has alleviated this problem. In 1990, cracking deterioration was identified on a three-year-old pavement on US 20 in central Iowa. The coarse aggregate was a crushed limestone with an excellent history of performance in PCC pavement. Examination of cores showed very few cracks through the coarse aggregate particles. The cracks were predominately confined to the matrix. The deterioration was identified as alkali-silica reactivity (ASR) by a consultant. To investigate the cause of the deterioration, the Iowa DOT and Iowa State University jointly purchased a high resolution, low vacuum Hitachi Scanning Electron Microscope (SEM) with an energy dispersion detector. Subsequent evaluation identified no concentration of silica gel (silicon-Si), but did identify substantial amounts of sulfur-S and aluminum-AL (assumed to be ettringite) in the air voids. Some of these voids have cracks radiating from them leading us to conclude that the ettringite filled voids were a center of pressure causing the crack. The ettringite in the voids, after being subjected to sodium chloride (NaCl), initially swells and then dissolves. This low vacuum SEM research of PCC pavement deterioration supports the following conclusions: (1) A low vacuum SEM and an energy dispersion detector are very important for proper evaluation of PCC pavement deterioration; (2) There are instances today where PCC pavement deterioration is mistakenly identified as ASR; (3) Ettringite initially expands when subjected to NaCl; and the ettringite filled voids are a center-of-pressure that cracks the PCC; and (4) The deterioration of some current premature PCC pavement distress locations is caused by factors related to the formation of excessive ettringite.

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Examination of field portland cement concrete cores, from Iowa pavements with premature deterioration, reveals extensive infilling of calcium sulfate aluminum (CSA) compound in their air voids. A previous study (Phase I) has shown some evidence of the correlation between freeze-thaw durability of concretes and ettringite infilling. To further verify the previous observation, a more extensive experimental program was conducted in this Phase 2 study. A total of 101 concrete mixes were examined. Seven cements, six fly ashes, two water reducers and three coarse aggregates were used in the concrete mixes. Specimens were under moist curing for up to 223 days before being subjected to the freeze-thaw cycling. An environmental treatment consisting of three consecutive wet [70 deg F (21 deg C) in distilled water]/dry [120 deg F (49 deg C) in oven] cycles was applied to some specimens. Immediately prior to the freeze-thaw cycling, most specimens were examined by a low-vacuum scanning electron microscope (SEM) for their microstructure. The results obtained further demonstrate the correlation between concrete freeze-thaw response and CSA compound infilling in the air voids. The extent of the infilling depends on the period of moist curing as well as the wet/dry treatment. The extent of the infilling also relates to materials used. Concrete mixes with extensive infilling are more vulnerable to the freeze-thaw attack. Based on the obtained results, material criteria on cements and fly ashes for mainline paving were proposed for minimizing potential infilling of CSA compound in concrete.

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The major objective of this work was to evaluate the potential of image analysis for characterizing air voids in Portland cement Concrete (PCC), voids and constituents of Asphalt Concrete (AC) and aggregate gradation in AC. Images for analysis were obtained from a scanning electron microscope (SEM). Sample preparation techniques are presented that enhance signal differences so that backscattered electron (BSE) imaging, which is sensitive to atomic number changes, can be effectively employed. Work with PCC and AC pavement core samples has shown that the low vacuum scanning electron microscope (LVSEM) is better suited towards rapid analyses. The conventional high vacuum SEM can also be used for AC and PCC analyses but some distortion within the sample matrix will occur. Images with improved resolution can be obtained from scanning electron microscope (SEM) backscatter electron (BSE) micrographs. In a BSE image, voids filled with barium sulfate/resin yield excellent contrast in both PCC and AC. There is a good correlation between percent of air by image analysis and linear traverse.

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A two-stage mixing process for concrete involves mixing a slurry of cementitious materials and water, then adding the slurry to coarse and fine aggregate to form concrete. Some research has indicated that this process might facilitate dispersion of cementitious materials and improve cement hydration, the characteristics of the interfacial transition zone (ITZ) between aggregate and paste, and concrete homogeneity. The goal of the study was to find optimal mixing procedures for production of a homogeneous and workable mixture and quality concrete using a two-stage mixing operation. The specific objectives of the study are as follows: (1) To achieve optimal mixing energy and time for a homogeneous cementitious material, (2) To characterize the homogeneity and flow property of the pastes, (3) To investigate effective methods for coating aggregate particles with cement slurry, (4) To study the effect of the two-stage mixing procedure on concrete properties, (5) To obtain the improved production rates. Parameters measured for Phase I included: heat of hydration, maturity, and rheology tests were performed on the fresh paste samples, and compressive strength, degree of hydration, and scanning electron microscope (SEM) imaging tests were conducted on the cured specimens. For Phases II and III tests included slump and air content on fresh concrete and compressive and tensile strengths, rapid air void analysis, and rapid chloride permeability on hardened concrete.

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The major objective of this project is to evaluate image analysis for characterizing air voids in Portland cement contract (PCC) and asphalt concrete (AC) and aggregate gradation in asphalt concrete. Phase 1 of this project has concentrated on evaluation and refinement of sample preparation techniques, evaluation of methods and instruments for conducting image analysis, and finally, analysis and comparison of a select portion of samples. Preliminary results suggest a strong correlation between the results obtained from the linear traverse method and image analysis methods for determining percent air voids in concrete. Preliminary work with asphalt samples has shown that damage caused by a high vacuum of the conventional scanning electron microscope (SEM) may too disruptive. Alternative solutions have been explored, including confocal microscopy and low vacuum electron microscopy. Additionally, a conventional high vacuum SEM operating at a marginal operating vacuum may suffice.

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Many early Iowa Portland Cement Concrete (PCC) pavements provided good performance without deterioration for more than 50 years. In the late 1950's, Iowa was faced with severe PCC pavement deterioration called D cracking due to crushed limestone containing a bad pore system. Selective quarrying solved the problem. In 1990, cracking deterioration was identified on a three year old US 20 pavement in central Iowa. The coarse aggregate was a crushed limestone with an excellent history of performance in PCC pavement. Examination of cores showed very few cracks through the coarse aggregate particles. The cracks were predominately confined to the matrix. A high resolution, low vacuum Hitachi Scanning Electron Microscope (SEM) with an energy dispersion detector was used to investigate the deterioration. Subsequent evaluation identified very little concentration of silica gel (silicon-Si), but did identify substantial amounts of sulfur-s and aluminum-Al (assumed to be ettringite) in the air voids. Some of these voids have cracks radiating from them leading us to conclude that the ettringite filled voids were a center of pressure causing the crack. The ettringite in the voids, after being subjected to sodium chloride (NaCl) brine, initially swells and then dissolves. The research has led to the conclusion that the premature deterioration may be due to ettringite and may have been mistakenly identified as Alkali-Silica reactivity (ASR).