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At least 37 records · Page 2

Minor Elements and Solidification Cracking During Laser Powder-Bed Fusion of a High $\gamma ^{\prime }$ CoNi-Base Superalloy

Here, the cracking behavior of a high γ' volume fraction CoNi-base superalloy fabricated via laser powder bed fusion (LPBF) is studied in relation to the content of carbon and boron. Severe cracking occurred with the increase in boron content from 0.08 to 0.16 at. pct (0.015 to 0.029 wt pct), while compositions with 0.1 to 0.36 at. pct C (0.02 to 0.076 wt pct) and 0.08 at. pct B exhibited minimal cracking. Assessment of cracks in the high-boron composition shows a variation in crack density with printing parameters, and alignment of the cracks with the build direction. Scanning electron microscopy (SEM) of the crack surfaces shows evidence of a solidification cracking mode. Differential thermal analysis (DTA) reveals a decreased incipient melting temperature for the high-boron composition, and atom probe tomography (APT) is used to measure the enrichment at grain boundaries, revealing distinct boron segregation. Scheil-Gulliver solidification simulations for the different C and B levels are consistent with the incipient melting behavior observed with DTA. Evaluation of the solidification cracking susceptibility from the simulations allow for comparison of the CoNi alloy behavior to Ni-base superalloys studied for LPBF fabrication and displays how such metrics may aid in the design of new precipitation-strengthened superalloys for additive manufacturing (AM).

36 MATERIALS SCIENCE↗

Transformation of a ceramic precursor to a biomedical (metallic) alloy: Part I – sinterability of Ta 2 O 5 and TiO 2 mixed oxides

Mixed Ta 2 O 5 – TiO 2 binary system was studied by a combination of differential thermal analysis (DTA), scanning electron microscopy-energy dispersive spectrometry (SEM-EDS), X-ray diffraction (XRD) and in situ high temperature X-ray diffraction (HT-XRD) techniques. Different compositions of the mixed oxide powders were fabricated by ball–milling the powdered compositions, pelletizing the homogenized composite powders, and heating the green pellets in air at different temperatures for fixed time intervals. The sintered pellets were evaluated and characterized with respect to porosity, morphology, and phase distribution. DTA runs of the un-sintered powders indicated the onset temperatures for both exothermic and endothermic changes in the binary system. Significant amount of sintering was observed to take place at temperatures higher than 900 °C. Both room and high temperature X-ray diffraction patterns exhibited consistency in phase formation. A ternary compound (TaTiO 4 ) and a ternary solid solution (Ti 0.33 Ta 0.67 O 2 ) were observed to form in both room and high temperatures in addition to the respective binary phases (Ta 2 O 5 and TiO 2 ). A sintering temperature in the range 900–1000 °C was observed to be adequate to achieve the requisite mechanical strength and optimum internal porosity (40–48%) for subsequent electrochemical polarization experiments.

36 MATERIALS SCIENCE↗

Zeta potential measurements of SiO 2 and TiO 2 particles in anionic and cationic surfactant solutions

Zeta potential measurements can provide valuable insights into colloidal stability and may reflect changes in the electrochemical double layer that influence electrocatalysis. In this study, we used zeta potential measurements to monitor and investigate the adsorption behavior of anionic sodium dodecyl sulfate (SDS), cationic dodecyl trimethyl ammonium bromide (DTAB), and cationic cetyl trimethyl ammonium bromide (CTAB) surfactants on SiO 2 and TiO 2 particles in DI water. The zeta potentials of SiO 2 and TiO 2 particles were measured as a function of particle concentration in 1.0 mM, 5.0 mM, and 10.0 mM surfactant solutions. Results indicate that there is no significant adsorption of DS - ions on SiO 2 particles across all SDS concentrations investigated in this study. The zeta potential of TiO 2 particles shifts from negative to positive as particle concentration increases at 1.0 mM SDS, indicating a decrease in DS - ions adsorption per TiO 2 particle. Adsorption plateaus at 5.0 mM SDS for all TiO 2 concentrations studied. In contrast, DTA + and CTA + ions showed clear adsorption on SiO 2 particles, but DTA + exhibited no apparent adsorption on TiO 2 particles. Interestingly, CTA + adsorption on TiO 2 was only evident at higher surfactant concentrations. This study presents a systematic investigation of zeta potential behavior as a function of particle and surfactant concentration, highlighting adsorption saturation and electrostatic reversal. Unlike prior work that was limited to single particle concentration measurements, our approach reveals how surfactant adsorption per particle decreases with increasing surface area. Despite the structural similarity between DTAB and CTAB, this study captured the different adsorption behaviors of both surfactants on SiO 2 and TiO 2 , emphasizing the role of the overall structure of the surfactant on surfactant adsorption behavior. These insights refine the interpretation of zeta potential data and advance understanding of surfactant adsorption on oxide particles. The insight provided in this study about surfactant adsorption on SiO 2 and TiO 2 particles could have important implications for the design of more effective colloidal and catalytic systems.

32 ENERGY CONSERVATION, CONSUMPTION, AND UTILIZATI↗

Differential thermal analysis and gas release studies of Apollo 11 samples.

The liquidus-solidus behavior of Apollo 11 lunar fines and the evolution characteristics of CO, nitrogen, He, Ne, and Ar were investigated by use of the combined techniques of high-vacuum differential thermal analysis (DTA) and mass spectrometry between 100 and 1500 C. The DTA thermogram has shown that the lunar fines undergo partial melting over a broad range of temperature from about 915 to 1300 C, with a significant initial melting of glassy and crystalline components within the fines at about 1140 C. The lunar material becomes a homogeneous melt at about 1300 C.

Wachi, F. M.↗

Study of recrystallization and devitrification of lunar glass

The technique of differential thermal analysis (DTA) was applied to the study of the Apollo 17 orange soil (74220,63) and the Apollo 16 glass coated anorthite (64455,21). These glasses show accentuated exotherms of strain relief in the annealing range which is indicative of rapid cooling. These are amenable to interpretation by comparison to the known history of synthetic glasses. Synthetic glasses were prepared whose similarity in behavior between the lunar glasses and their synthetic analogs is striking. Approximate rates of cooling of the lunar glasses were determined from comparative DTA of lunar and synthetic glasses and from the determination of the relation of strain relief in the annealing range to quench rate. At higher temperatures the glasses show exotherms of crystallization. The crystallization products associated with the exothermic reactions have been identified by X-ray diffraction and the surface morphologies developed by strain relief and crystallization have been characterized with scanning electron microscopy.

Ulrich, D. R.↗

Determination of liquid-phase immiscibility in the lead-zinc system

A number of different techniques in the past have yielded inconsistent equilibrium measurements of immiscibility in the Pb-Zn system above 600 C. Accurate differential thermal analysis (DTA) measurements were performed on well-homogenized samples of high-purity Pb-Zn, and they indicate that the immiscibility curve is higher than previously accepted for Zn compositions between 20 and 70 at. %. The maximum deviations observed correspond to about 20 C. Below 600 C the DTA results agree with previous results.

Trahan, J. F.↗

On the barrier to crystal nucleation in lunar glasses

The paper describes an analytical method for calculating in detail the size distributions of small crystallites and nuclei in supercooled liquids as they are being quenched to form a glass and subsequently reheated above the glass transition to produce crystallization. This method is applied to experiments performed using differential thermal analysis (DTA) to estimate the barriers to crystal nucleation and the cooling rates required to form glasses or bodies with various degrees of crystallinity. DTA data and derived nucleation barriers are reported for anorthite and for the following lunar compositions: 15498, 15418, matrix and intrusion compositions of breccia 15286, Apollo 15 green glass, Luna 24 highland basalt, and 65016.

Yinnon, H.↗

Characteristics of the handling and positioning aid

The handling and positioning aid which (HPA) provides a wide range of adjustable work stations both inboard and outboard of the cargo bay is discussed. It can assist with berthing and docking, it is robust, stiff, has a simple control system, and is modular. An articulated arm version of HPA employed in a typical servicing mission is shown. Mounted on a base frame that spans the Orbiter cargo bay, the 6 m arm is long enough to hold the satellite being serviced and keep its solar array clear of the Orbiter radiators. By adjusting the length and angle of the support platform mast, and rotating the tip of the HPA arm, almost every item on the satellite can be reached. Spares and change-out units can be brought to and from the work site by the RMS, which is controlled from the aft flight deck. The fore and aft position of the base frame can be changed between Orbiter flights and this, together with the 5 degrees of freedom (DOF) of the long arm, allows work sites to be chosen that meet the clearance, reach and vision requirements of many missions. Flight article activities are shown are shown above the dashed horizontal line and Development Test Article (DTA) work below. Flight article requirements and concepts and the design of the DTA are developed.

Goodwin, C. J.↗

Experimental results for the rapid determination of the freezing point of fuels

Two methods for the rapid determination of the freezing point of fuels were investigated: an optical method, which detected the change in light transmission from the disappearance of solid particles in the melted fuel; and a differential thermal analysis (DTA) method, which sensed the latent heat of fusion. A laboratory apparatus was fabricated to test the two methods. Cooling was done by thermoelectric modules using an ice-water bath as a heat sink. The DTA method was later modified to eliminate the reference fuel. The data from the sample were digitized and a point of inflection, which corresponds to the ASTM D-2386 freezing point (final melting point), was identified from the derivative. The apparatus was modifified to cool the fuel to -60 C and controls were added for maintaining constant cooling rate, rewarming rate, and hold time at minimum temperature. A parametric series of tests were run for twelve fuels with freezing points from -10 C to -50 C, varying cooling rate, rewarming rate, and hold time. Based on the results, an optimum test procedure was established. The results showed good agreement with ASTM D-2386 freezing point and differential scanning calorimetry results.

Mathiprakasam, B.↗

Crystallization kinetics of BaO-Al2O3-SiO2 glasses

Barium aluminosilicate glasses are being investigated as matrix materials in high-temperature ceramic composites for structural applications. Kinetics of crystallization of two refractory glass compositions in the barium aluminosilicate system were studied by differential thermal analysis (DTA), X-ray diffraction (XRD), and scanning electron microscopy (SEM). From variable heating rate DTA, the crystallization activation energies for glass compositions (wt percent) 10BaO-38Al2O3-51SiO2-1MoO3 (glass A) and 39BaO-25Al2O3-35SiO2-1MoO3 (glass B) were determined to be 553 and 558 kJ/mol, respectively. On thermal treatment, the crystalline phases in glasses A and B were identified as mullite (3Al2O3-2SiO2) and hexacelsian (BaO-Al2O3-2SiO2), respectively. Hexacelsian is a high-temperature polymorph which is metastable below 1590 C. It undergoes structural transformation into the orthorhombic form at approximately 300 C accompanied by a large volume change which is undesirable for structural applications. A process needs to be developed where stable monoclinic celsian, rather than hexacelsian, precipitates out as the crystal phase in glass B.

Bansal, Narottam P.↗

Crystallization kinetics of BaO-Al2O3-SiO2 glasses

Barium aluminosilicate glasses are being investigated as matrix materials in high-temperature ceramic composites for structural applications. Kinetics of crystallization of two refractory glass compositions in the barium aluminosilicate system were studied by differential thermal analysis (DTA), X-ray diffraction (XRD), and scanning electron microscopy (SEM). From variable heating rate DTA, the crystallization activation energies for glass compositions (wt percent) 10BaO-38Al2O3-51SiO2-1MoO3 (glass A) and 39BaO-25Al2O3-35SiO2-1MoO3 (glass B) were determined to be 553 and 558 kJ/mol, respectively. On thermal treatment, the crystalline phases in glasses A and B were identified as mullite (3Al2O3-2SiO2) and hexacelsian (BaO-Al2O3-2SiO2), respectively. Hexacelsian is a high-temperature polymorph which is metastable below 1590 C. It undergoes structural transformation into the orthorhombic form at approximately 300 C accompanied by a large volume change which is undesirable for structural applications. A process needs to be developed where stable monoclinic celsian, rather than hexacelsian, precipitates out as the crystal phase in glass B.

Bansal, Narottam P.↗

Determining the nucleation rate curve for lithium disilicate glass by differential thermal analysis

The crystallization of lithium disilicate (Li2O+2SiO2) glass nucleated at various temperatures was studied by differential thermal analysis (DTA). A plot of the DTA crystallization peak height versus nucleation temperature closely resembles the classical nucleation rate curve for lithium disilicate glass whose maximum is at 453 C. The glass becomes saturated with internal nuclei when heated at 453 C for 10 h. The activation energy for crystallization and the heat of crystallization are independent of the concentration of nuclei and are 249 + or - 10 and 67 + or - 3 kJ/mol, respectively. The Avrami exponent, n, depends strongly on the concentration of nuclei in the glass.

Ray, Chandra S.↗

The position of the magnetotail neutral sheet in the near-earth region

The position of the near-earth neutral sheet throughout the nightside region between R = 5 R(E) and R = 8.8 R(E) is examined statistically using magnetic field data from AMPTE/CCE. As has been demonstrated previously, the latitudinal position of the neutral sheet is primarily controlled by the dipole tilt angle. The position also depends on local time, radial distance, and magnetic activity. These dependencis may be represented by the empirical formula MLAT = - (0.14 Kp + 0.69) /cos(Phi)/exp 1/3 (0.065 R exp 0.8 - 0.16) DTA, where MLAT is the position in degrees of the neutral sheet relative to the magnetic equator, Kp is the 3-hourly magnetic activity index, Phi is the magnetic local time in degrees (midnight = 0 deg), R is the radius in R(E), and DTA is the dipole tilt angle in degrees.

Lopez, Ramon E.↗

A study of microstructural characteristics and differential thermal analysis of Ni-based superalloys

The objective of this work is to correlate the mechanical properties of the Ni-based superalloy MAR M246(Hf) used in the Space Shuttle Main Engine with its structural characteristics by systematic study of optical photomicrographs and differential thermal analysis. The authors developed a method of predicting the liquidus and solidus temperature of various nickel based superalloys (MAR-M247, Waspaloy, Udimet-41, polycrystalline and single crystals of CMSX-2 and CMSX-3) and comparing the predictions with the experimental differential thermal analysis (DTA) curves using Perkin-Elmer DTA 1700. The method of predicting these temperatures is based on the additive effect of the components dissolved in nickel. The results were compared with the experimental values.

Aggarwal, M. D.↗

Nucleation and crystallization of Na2O-2CaO-3SiO2 glass by differential thermal analysis

DTA is presently used to characterize the nucleation and crystallization processes of the Na2O-2CaO-3SiO2 glass. A nucleation rate-temperaturelike curve is obtained by plotting either the reciprocal of the temperature corresponding to the crystallization peak maximum, or the height of the crystallization peak, as a function of nucleation temperature. The nucleation-temperature range for this glass composition, 550-650 C, and the maximum nucleation temperature of 600 + or - 5 C, are found to be in excellent agreement with those associated with the classical nucleation technique, followed by isothermal crystallization. It is noted that when most of the nucleation occurs during the DTA measurements, a modified Kissinger equation must be used to calculate the crystallization energy.

Xu, Xiaojie J.↗

Demonstration of rapid and sensitive module leak certification for Space Station Freedom

A leak detection and quantification demonstration using perflurocarbon tracer (PFT) technology was successfully performed at the NASA Marshall Space Flight Center on January 25, 1991. The real-time Dual Trap Analyzer (DTA) at one-half hour after the start of the first run gave an estimated leak rate of 0.7 mL/min. This has since been refined to be 1.15 (+ or -) 0.09 mL/min. The leak rates in the next three runs were determined to be 9.8 (+ or -) 0.7, -0.4 (+ or -) 0.3, and 76 (+ or -) 6 mL/min, respectively. The theory on leak quantification in the steady-state and time-dependent modes for a single zone test facility was developed and applied to the above determinations. The laboratory PFT analysis system gave a limit-of-detection (LOD) of 0.05 fL for ocPDCH. This is the tracer of choice and is about 100-fold better than that for the DTA. Applied to leak certification, the LOD is about 0.00002 mL/s (0.000075 L/h), a 5 order-of-magnitude improvement over the original leak certification specification. Furthermore, this limit can be attained in a measurement period of 3 to 4 hours instead of days, weeks, or months. A new Leak Certification Facility is also proposed to provide for zonal (three zones) determination of leak rates. The appropriate multizone equations, their solutions, and error analysis have already been derived. A new concept of seal-integrity certification has been demonstrated for a variety of controlled leaks in the range of module leak testing. High structural integrity leaks were shown to have a linear dependence of flow on (Delta)p. The rapid determination of leak rates at different pressures is proposed and is to be determined while subjecting the module to other external force-generating parameters such as vibration, torque, solar intensity, etc.

Dietz, R. N.↗

A DTA/GC for the in Situ Identification of the Martian Surface Material

The composition and mineralogy of the Martian surface material remain largely unknown. To determine its composition and mineralogy, several techniques are being considered for in situ analyses of the Martian surface material during missions to Mars. We have successfully developed, constructed, and tested a laboratory DTA/GC. The DTA is a Dupont model 1600 high temperature DTA coupled with a GC equipped with a MID detector. The system is operated by a Sun Sparc 11 workstation. When gas evolves during a thermal chemical event, it is shunted into the GC and the temperature is recorded in association with the specific thermal event. We have used this laboratory instrument to define experimental criteria necessary for determining the composition and mineralogy of the Martian surface in situ (e.g., heating of sample to 1100 C to distinguish clays). Our studies indicate that DTA/GC will provide a broad spectrum of mineralogical and evolved gas data pertinent to exobiology, geochemistry, and geology.

Mancinelli, R. L.↗

Magnetite: What it reveals about the origin of the banded iron formations

Magnetite, Fe3O4 is produced abiotically and biotically. Abiotically, magnetite is a late magmatic mineral and forms as a consequence of the cooling of iron rich magma. Biotically, magnetite is produced by several organisms, including magnetotactic bacteria. Hematite, Fe2O3, is also produced abiotically and biotically. Abiotically, hematite rarely occurs as a primary mineral in igneous rocks, but is common as an alteration product, fumarole deposit, and in some metamorphosed Fe-rich rocks. Biotically, hematite is produced by several types of microorganisms. Biologically-produced magnetite and hematite are formed under the control of the host organism, and consequently, have characteristics not found in abiotically produced magnetite and hematite crystals. To determine if the magnetite and hematite in the Banded Iron Formation was biologically or abiotically produced, the characteristics of biologically-produced magnetite and hematite (concentrated from Aquaspirillum magnetotacticum) and abiotically-produced magnetite and hematite obtained from Wards Scientific Supply Company, were compared with characteristics of magnetite and hematite concentrated from the Gunflint Banded Iron Formation (Ontario, Canada) using thermal and crystallographic analytical techniques. Whole rock analysis of the Gunflint Banded Iron Formation by x-ray diffraction (XRD) and differential thermal analysis (DTA) revealed the presence of quartz, hematite, siderite and dolomite as the major minerals, and magnetite, greenalite, pyrite, pyrrhotite and apatite as the minor minerals. Analysis of a crude magnetic fraction of the Gunflint showed the minerals quartz, hematite, siderite, dolomite, and magnetite. Analysis of the crude magnetic fraction from Aquaspirillum magnetotacticum revealed organic compounds plus hematite and magnetite. The mineral identification and particle size distribution data obtained from the DTA along with XRD data indicate that the magnetite and hematite from the Gunflint BIF share some similarities with biologically formed magnetite and hematite.

Schwartz, D. E.↗