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By G-L. Wu, S-W. Wu

"The hot deformation behaviour of Nb-Ti microalloyed high-strength steel was investigated. Hot compression tests were conducted in the temperature range 900 to 1100°C under strain rates of 0.1, 1, and 5 s-1. Dynamic recrystallization (DRX) occurs as the main flow softening mechanism at high temperature and low strain rate. The hot deformation activation energy was calculated to be about 404 699 J/mol. The constitutive equation was developed to describe the relationship between peak stress, strain rate, and deformation temperature. The characteristics of DRX at different deformation conditions were extracted from the stressstrain curves using the work hardening parameter. The Cingara-McQueen equation was developed to predict the flow curves up to the peak strain. The processing maps were obtained on the basis of a dynamic materials model. The results predict an instability region in the temperature range 1010 to 1100°C when the strain rate exceeds 0.78 s-1. IntroductionThe 700 MPa grade HSLA steel is widely used in engineering machinery, automotive beams, carriages, and axle tubes, etc. (Pan et al., 2017 ). Generally, such grades contain a moderately high amount of Mn (approx. 1.4% and above), and microalloying elements like Nb, Ti, V, and Mo to impart the desired strength and toughness through solid-solution strengthening, precipitation hardening, and grain refinement dislocation strengthening (Chen and Yu, 2012; Opiela, 2014). However, the production costs can be greatly reduced by replacing part of the Nb, V, or Mo with inexpensive Ti and adopting the compact strip production CSP process (Opiela, 2014; Chen et al., 2015). Furthermore, the microalloying technology coupled with new-generation thermomechanical control processing (NG-TMCP) has proved efficient for achieving the proper balance between strength, toughness, ductility, and formability by means of a suitable combination of chemical composition and thermomechanical treatment parameters (Shukla et al., 2012; Wu, Zhou, and Liu, 2017).In hot forming processes, the complex microstructural evolutions are often induced by multiplicative hot deformation mechanisms, such as work hardening (WH), dynamic recovery (DRV), and dynamic recrystallization (DRX) (Zhang et al., 2014; Liang et al., 2015). Dynamic softening behaviour during hot processing has generated considerable interest because component properties are influenced significantly by its corresponding microstructural evolution (Wu et al., 2010). During deformation in the DRX process, deformed grains are replaced with substructures and newly formed fine and uniformly distributed grains. This occurs only when a critical strain for the onset of DRX is reached, and at the same time, the minimum rate of energy dissipating is reached (Ferdowsi et al., 2014). DRV occurs at a high strain rate and low temperature, reducing the stored energy greatly and making DRX difficult (Liang et al., 2015). The microstructural changes during DRX are sensitive to the processing parameters, such as strain rate, deformation temperature, and strain (Zhang et al., 2014; Ferdowsi et al., 2014). Therefore, in order to optimize the hot processing parameters, it is important to understand the behaviour of hot deformation visà- vis control of microstructural evolution."

May 1, 2019

By Sumantra Mandal

The hot deformed microstructure of the 15Cr-15Ni-2.2Mo-Ti modified austenitic stainless steel (commonly known as alloy D9) was investigated employing electron backscatter diffraction (EBSD). Hot compression tests were conducted in a Gleeble thermo-mechanical simulator at temperatures of 1173K-1373K (in steps of 100K) with a strain rate of 10 and 100 s-1 to different strains. Various kinds of deformation patterns were observed inside the deformed grains. These were inferred as the development of geometrically necessary boundaries or formation of parallel set of micro-bands. Recrystallized grains were partitioned from the deformed grains employing grain orientation spread approach. Extent of dynamic recrystallization (DRX) was found to be minimal at 1173K. DRX was predominantly found to happen at and above 1273K which increases with increase in strain. DRX nucleation and development mechanisms were discussed with respect to bulging of the parent grains and sub-grain rotation. Special emphasize is given on the role of annealing twins on DRX nucleation and subsequent expansion.

Jan 1, 2009

By A. N. Lasseigne

Hydrogenation behavior of the NaAlH4 intermetallics is investigated utilizing thermoelectric power and magnetic analyses. Using both thermoelectric power and magnetic susceptibility measurements on these intermetallics allows for confirmation and further insight into hydrogen's role in altering the material's electronic structure. The electronic and magnetic property correlations will indicate the direction for further alloy development to optimize hydrogen storage.

Jan 1, 2006

By P. D. Roa, O. Noirot, H. Owens, D. E. Walsh, J. R. Mokka

Over a period of eight years (1989 through 1997) the Mineral Industry Research Laboratory (MIRL) at the University of Alaska, Fairbanks, AK, has investigated the effects of temperature, residence time and particle size on the degree of low-rank coal (LRC) upgrading for a nonevaporative, hydrothermal drying process, also known as hot water drying (HWD). The following three Alaskan LRCs were used in this study: Usibelli coal (Seam No. 4) from the Nenana Coal Field, Little Tonzona coal from near McGrath, and Beluga coal from the Beluga-Yentna field on the west side of Cook Inlet. Replicated factorial tests were conducted. Experimental results indicate that most of the low-rank coal upgrading via HWD occurs rapidly within the first 10 to 20 min of residence time. Thereafter, the upgrading process slows down, and more than 100 min of additional residence time is required to produce percentage increases equivalent to what was achieved in the first 10 to 20 min. The properties of the hot water dried products were very sensitive to process temperature. Calorific value, carbon and oxygen contents, equilibrium moisture levels and Hardgrove gindabilities all appear to change linearly with temperature within the 275°C to 325°C (525°F to 61 5 OF) range.

Jan 1, 2000

By D. E. Walsh

Over a period of seven years (1989-1996) the Mineral Industry Research Laboratory (MIRL) University of Alaska Fairbanks, has investigated the effects of temperature, residence time, and particle size on the degree of low-rank coal (LRC) upgrading for a non-evaporative, hydrothermal drying process, also known as hot water drying (HWD). Three Alaskan LRCs were used in this study: Usibelli coal (Seam No.4) from the Nenana Coal Field, Little Tonzona coal from near McGrath, and Beluga coal from the Beluga-Yentna field on the west side of Cook Inlet. Replicated, factorial tests were conducted. Experimental results indicate that most of the low-rank coal upgrading via HWD occurs rapidly within the first 10-20 minutes of residence time. Thereafter, the upgrading process slows down and over 100 minutes of additional residence time are required to produce similar percentage increases in coal properties to those achieved in the first 10-20 minutes. The properties of the hot water dried products were very sensitive to process temperature. Calorific value, carbon and oxygen contents, equilibrium moisture levels and Hardgrove grindabilities all appear to change linearly with temperature within the 275" C to 325" C range.

Jan 1, 1997

By O. Noirot, H. C. Owens, P. D. Rao, D. E. Walsh, J. R. Mokka

Over a period of seven years (1989-1996) the Mineral Industry Research Laboratory (MIRL) University of Alaska Fairbanks, has investigated the effects of temperature, residence time, and particle size on the degree of low-rank coal (LRC) upgrading for a non-evaporative, hydrothermal drying process, also known as hot water drying (HWD). Three Alaskan LRCs were used in this study: Usibelli coal (Seam No. 4) from the Nenana Coal Field, Little Tonzona coal from near McGrath, and Beluga coal from the Beluga-Yentna field on the west side of Cook Inlet. Replicated, factorial tests were conducted. Experimental results indicate that most of the low-rank coal upgrading via HWD occurs rapidly within the first 10-20 minutes of residence time. Thereafter, the upgrading process slows down and over 100 minutes of additional residence time are required to produce similar percentage increases in coal properties to those achieved in the first 10- 20 minutes. The properties of the hot water dried products were very sensitive to process temperature. Calorific value, carbon and oxygen contents, equilibrium moisture levels and Hardgrove gindabilities all appear to change linearly with temperature within the 275°C to 325°C range.

Feb 24, 1997

By S. Yannacopoulos, L. Bichler, P. Wanjara, J. Gholipour

Characterization of a virgin and in-service Inconel 718 alloy was undertaken to study the changes caused by the service conditions on the grain size, ?? phase, MN-type nitrides and MC-type carbides. The size, distribution and volume fraction of these phases and grain size were studied using scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS) and electron backscattered diffraction (EBSD) analyses. A considerable difference in the grain size, as well as distribution and volume fraction of the precipitates was observed in the in-service material as compared to the virgin Inconel 718. As a result of these microstructural changes, a notable dissimilarity in hardness between the materials investigated was observed. The results presented in this study are important for proper development of repair parameters and heat treatment of in-service Inconel 718 material.

Jan 1, 2014

By C. Blais, G. L’Espérance

Characterization of second phase particles is important with regard to their influence on mechanical properties of materials. Analytical electron microscopy offers the possibility to achieve complete characterization of inclusions. Complete characterization of inclusions means quantitative evaluation of their chemistry and the stereological parameters. A characterization technique based on integrated microscopy and involving scanning electron microscopy, image analysis and energy dispersive X-ray spectrometry is presented. A discussion of the use of transmission electron microscopy and electron energy loss spectroscopy is also presented for the characterization of very small particles and compounds (>100 nm).

Jan 1, 1998

By Mohan Ram

Structural impurities in the crystal lattice of rock phosphate of Indian origin is a great challenge for beneficiation and practically possesses remote scope of upgradation to the desired level for industrial utilization. There is a wide occurrence of rock phosphate in different parts of India with different characteristics viz. siliceous, carbonaceous and ferruginous. The structural cationic replacement in the composition of apatite is due to the exchangeable cations present in the external impurities associated with the rock phosphate ore. The Indian rock phosphate ore from Purulia district, West Bengal is characterized as unusual structural composition due to the exchangeable cation in its composition. The elemental distribution of ore exhibits the disproportionate ratio of P2O5 and CaO which is 5.88: 3.31 in reference to the theoretical composition of P2O5: CaO in apatite which is 4.23: 5.55. The substitution by trivalent Al+++ cations within the structure of apatite in place of divalent Ca++ is found upto 18% and substitution of exchangeable cation in place of PO4 and F ion by CO3/SO4 is found upto 0.1% and OH ions upto 0.2% respectively in a lattice of apatite thereby diluting the grade of rock phosphate and restricting its industrial use even after beneficiation. This paper reveals the unusual compositional features of rock phosphate under study and is a guideline to the mineral industries using such rock phosphate. Keywords: external impurities, exchangeable cation substitution, structural compositional features, electron probe micro analyzer

Sep 1, 2012

By J. C. van Dyk

The objectives of this study were firstly to characterize and quantify the inorganic material in the Secunda gasification feedstock. Secondly, the effect of washing on coal properties and sulphur content was investigated. Coal from a single source and a coal blend from 6 different mines were tested. Composite samples were visually sorted by a geologist in the groups containing roof, floor, C-shale, pyrite, carbonates and siltstone material. Inorganic mineral types from the single source and coal blends were characterized separately. Characterization results indicate that the average mineral matter distribution (mass %) of the coal tested was as follows: carbonates (6%), carbon-shale (19%), pyrite (12%), roof (18%), floor (46%) and siltstone (22%). The roof, floor, pyrite, carbon-shale, carbonates and siltstone in the single source and coal blend have similar chemical properties and characteristics, except for the ash melting temperatures of pyrite and kaolinite in the siltstone. By implementing selective mining and increasing mining management practices, the percentage discard in the run of mine coal can be significantly reduced, by up to 45%, if the mining of roof and floor material can be avoided. No significant impact of mining practices on sulphur content is expected in this case due to the low concentrations of sulphur in the roof and floor material. In summary, selective mining practices will probably result in almost45% decrease in the discard content in the run of mine to gasification, an increase in the carbon content from 55.0% to 58% (air dry basis) and a decrease in sulphur content from 1.1% to 0.9% (air dry basis). It is clear from this study that the main source of sulphur is not in the high ash-content mineral types (e.g. floor and roof), but in situ in the coal structure. Keywords: inorganic material, effect of washing, roof, floor, pyrite, C-shale, carbonates and siltstone

Jan 1, 2005

By N. Krishna

The utilization of Electrochemical Impedance Spectroscopy (EIS) in conjunction with Atomic Force Microscopy (AFM) is a powerful surface characterization technique to study the role of sulfur formation during acidic oxidation of chalcopyrite. It has been established that the chalcopyrite dissolution kinetics is controlled by the formation of passive sulfur layer during leaching. The objective of the study was to characterize the intermediate sulfur layer formation at different oxidation conditions in acidic solution. The chalcopyrite samples were subjected to anodic oxidation and the oxidation process was analyzed using impedance spectroscopy. The sulfur growth on the chalcopyrite surface during oxidation was further analyzed using Atomic Force Microscope for sulfur roughness and grain size, peak height and sulfur growth.

Jan 1, 1999

By Luis Giraldo

The installation procedure of fully grouted rebar bolts requires that the bolt be pushed through the resin grout until it is fully inserted in the borehole. Resin grout is a highly viscous fluid that is forced to flow through the annulus between the bolt and the borehole as the bolt advances. Variables such as bolt insertion speed, bolt vs. borehole diameter and grout viscosity determine the magnitude of the pressure generated ahead of the bolt tip. Under weak rock conditions, the magnitude of the pressure of bolt insertion is often sufficient to initiate hydraulic fracturing along joints or bedding planes that allow injection of grout into the strata leading to significant loss of bolt encapsulation. The grout pressure front has also been linked to gloving, a bolt installation problem that reduces bolt effectiveness. A series of tests were conducted to characterize the pressure of bolt insertion during bolt installation under various conditions. Analysis of the data shows three distinct stages of pressure build up during bolt installation. Understanding of the mechanisms involved may allow development of strategies for controlling the pressure buildup and its negative impact during roof bolting under weak rock conditions.

Jan 1, 2006

By M. Misra, J. Nanor

The precipitation and removal of arsenic from process waters can be accomplished with addition of lanthanum chloride alone or in conjunction with ferric sulfate. The long term stability of these corresponding precipitated compounds is critical from the disposal stand-point. In this paper the characterization of ferric, lanthanum and lanthanum-ferric arsenate compounds formed at room temperature in acidic and alkaline pH is presented. The characterization techniques used included zeta potential, XRD and SEM. Zeta potential measurements of ferric and lanthanum hydroxides in the presence of arsenate indicate that oxyanions of arsenate are chemically adsorbed onto the positively charged surfaces of these hydroxides. In alkaline pH there is desorption of arsenate species from the ferric hydroxide surface, hence the product is thought to be unstable. On the contrary, lanthanum arsenate is stable in alkaline pH. XRD patterns show that the ferric arsenate formed in acidic and alkaline pH is amorphous, whereas lanthanum arsenate and lanthanum-ferric arsenate formed in acidic and alkaline pH are crystalline.

Jan 1, 1999

By Yuanbo Zhang, Bingbing Liu, Zhuyin Chen, Xiao Kang, Chen Liu

Composite agglomeration process (CAP) is an effective method to utilize the iron-bearing dusts generated in the ironmaking plants, by which the dust percentage in the sinter feed can be increased up to 20 wt %. In the current study, a comparison on behavior of iron-bearing dust in the conventional sintering process (CSP) and CAP was characterized. The results showed, in the CSP products, the scattered iron-bearing dust in the mixture was disadvantageous for the sintering indexes and consolidation of the finished sinters. In the CAP products, the main phase in the iron-bearing dust pellets was well-crystallized Fe2O3 grain particles. In the matrix parts, there were more Fe3O4 particles generated, which caused to high RDI+3.15 and low RI of the finished products. The pellets and the matrix parts were bonded by iron oxides and acicular calcium ferrite.

Jan 1, 2016

Three high-grade limestone ores (CaO content over than 53 %) with different geological origin have been characterized for the synthesis of aragonite precipitated calcium carbonate. Limestone ores examined in this study showed different crystal particle size that cause difference in disintegration degree and surface area of the synthesized slaked limes. The limestone ore with smaller crystal particle size showed higher disintegration degree and also yielded slaked lime with smaller surface area, which is good for the synthesis of aragonite precipitated calcium carbonate. The synthesis of aragonite PCC using the limestone with a small crystal particle size was yielded needle-shaped aragonite with the aspect ratio of about 14. Keywords: limestone, lime, slaked lime, precipitated calcium carbonate, aragonite, accelerated carbonation

Sep 1, 2012

By Robert L. Parsons

This paper describes the results of a detailed analysis of a loess deposit at the deep foundations test site established by the Kansas Department of Transportation. Multiple CPT, SPT, and pressuremeter tests were conducted as part of the investigation. This paper includes an evaluation of the effectiveness of common correlations used with the CPT, SPT when used for classification of loess and estimating its properties. Results show that common correlations must be used with caution as significant errors in estimation may result from using methods developed for other soil types. Laboratory testing included direct shear, triaxial, collapse, and consolidation testing, with many of the tests conducted on both vertically and horizontally oriented samples to evaluate anisotropic behavior. The results showed that strength properties could be considered to be isotropic.

Jan 1, 2009

By A. D. Neuman, C. C. Davis, M. R. Lopez, A. C. Martinez, T. A. Nothwang, F. G. Hampel, S. L. Voit

"One of the thrust areas for the Global Nuclear Energy Partnership (GNEP) program is the development of actinide bearing fuels for transmutation in a fast reactor. Mixed Oxide (MOX) fuel has an extensive fast reactor irradiation history and thus is being considered for use as a baseline composition from which minor actinides can be incorporated for use as a transmutation fuel. The current study involves characterization of precursor powders and pellets destined for the Advanced Test Reactor in Idaho. These pellets will have three compositions: one standard MOX composition, (U0.80Pu0.20)O1.98, and two compositions of minor actinide mixed oxide (MAMOX) with oxygen to metal ratios (O/M) of (U0.75Pu0.20Am0.03Np0.02)O1.98 and (U0.75Pu0.20Am0.03Np0.02)O1.95. The precursor powders were characterized using a field emission gun scanning electron microscope (FEG-SEM) to determine particle morphology, size, and size distribution. An electron probe microanalyzer (EPMA) was used to characterize element distributions in the pellets.IntroductionThe fundamental purpose of GNEP is to enable a fuel recycling partnership between member nations. The customer nations utilize the fuel for electricity generation provided by and subsequently recycled by the supplier nation. The supplier nation recycles the actinide constituents, mainly uranium and plutonium, in advanced nuclear power reactors, and thus reducing waste volumes [1, 2]. Nuclear materials are strictly controlled through the International Atomic Energy Agency. One of the thrust areas supported by the GNEP program is the development of actinide bearing fuels for transmutation in a fast reactor under the U.S. Advanced Fuel Cycle Initiative (AFCI) in order to transmute long-lived transuranic actinide isotopes into shorter-lived fission products [3].MOX fuel has an extensive fast reactor irradiation history and thus is being considered for use as a baseline composition into which minor actinides can be incorporated for use as a transmutation fuel [4]. Irradiation performance data on oxide fuels with high concentrations of minor actinides is limited, which has prompted this study. This paper discusses the characterization results of precursor powders and pellets prepared for the Advanced Test Reactor in Idaho to determine the effects of including minor actinides in the fuel, and addresses two fuel test matrices proposed by Hilton et al. [3]. The pellets will have three compositions: one standard MOX composition, (U0.80Pu0.20)O1.98, and two compositions of MA-MOX with O/M of (U0.75Pu0.20Am0.03Np0.02)O1.98 and (U0.75Pu0.20Am0.03Np0.02)O1.95. The precursor powders, uranium oxide (depleted, DUO2 and highly enriched, HEUO2), neptunium oxide, NpO2, americium oxide, AmO2, and plutonium oxide, PuO2, were characterized using a FEG-SEM for particle morphology, size, and size distribution. The morphology of the actinide powders was studied in the areas of flowability and porosity in order to predict manufacturability. The MOX pellets were characterized using an EPMA in order to determine impurity levels and locations."

Jan 1, 2008

By Dongok Kim

Regardless of the advantages of the Friction Stir Process (FSP), for age-hardened aluminum alloys, the mechanical properties such as hardness in the stir zone decreased after FSP due to the growth or dissolution of strengthening precipitates. Here, as a new technique, FSP was introduced to alloy copper nanopowders in Al7075 T651. Mechanical properties of copper nanopowder- alloyed Al7075 T651 together with micro and nanostructures were compared with those of as-FSPed Al7075 T651 using SEM, TEM, and Vickers hardness testing to understand structure-property relationships. It was observed that Vickers hardness of the stir zone in copper nanopowder alloyed Al7075 T651 increased by 20% compared to that of the heat affected zone, while the as-FSPed samples did not show a noticeable increase in hardness in the same zone. Xray mapping showed traces of copper nanopowder after the process. TEM is being used to verify if there was CuAl2 formed in the copper alloyed sample.

Jan 1, 2006

By Zhangm Mingming

Three samples received from the EAF shop were characterized by chemical, X-ray diffraction (XRD), optical microscopy (OM) and scanning electron microscopy (SEM) methods. The objective of this characterization work was to investigate the occurrence of nickel, copper, zinc, sulfur and phosphorus and to identify their origin and associations with iron minerals in the concentrate samples from the mines. The samples were identified as MINERAL, PELLET, and HRD. The latter is the DRI product. All three samples were received as fine powders. The results indicate that, in the mineral sample, magnetite is the major iron oxide mineral with hematite as a second phase based on the OM and XRD studies. Pyrite [FeS2], chalcopyrite [CuFeS2] and bravoite [(Fe,Ni)S2] are the major sulfide minerals. Trace amounts of apatite [Ca5(PO4)3(F,Cl,OH)], wardite [Na4CaAli2(PO4)8(OH)8 6H2O], giniite [Fe;(PO4)4(OH)3 2H2O] and vivianite [Fe3(PO4)2 8H2O] were identified by SEM and XRD. Microscopic studies also indicated that most of the sulfide grains in the mineral sample are present either as liberated fine particles (about 10 microns) or as inclusions within the magnetite and hematite grains. XRD studies revealed magnetite as the major mineral with subordinate amounts of hematite and pyrite confirming the microscopic findings. Copper, nickel, and zinc are mainly present as chalcopyrite, bravoite, and franklinite [(Zn,Mn,Fe)(Fe,Mn)2O4] in trace amounts in the mineral samples, respectively. Impurities carry over to the pellet and HRD samples. Chemical analyses of the three iron-bearing samples indicate that sulfur and phosphorus in the pellet sample exceeded the specification. Since liberated pyrite and chalcopyrite particles were observed in both the mineral and pellet samples, magnetic and flotation processing routes should be effective for sulfide removal but at the cost of iron losses. The high phosphorus content of all three samples indicates that there are phosphates which are difficult to remove by the current concentrating processes (magnetic separation and flotation).

Jan 1, 2012

By Susanne Pignolet-Brandom

Fourteen samples of crushed Duluth Complex rock were characterized by the QEM?SEM automated scanning electron microscope image analysis system to evaluate the application of the system to mining waste rock characterization. The system can reliably distinguish the iron sulfides, the copper-iron sulfides and the nickel-iron sulfides. Calcite was distinguished from all other minerals except fluorite. The volumetric abundances were verified by comparing elemental abundances calculated using the QEM"SEM volumetric percentages and appropriate mineral compositions with elemental abundances determined by standard laboratory procedure. The pH and sulfate concentrations of rinse water from laboratory leach experiments correlated well with the mineralogical data.

Jan 1, 1989