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At least 217 records · Page 12

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NASA NTRS1999

Effects of Melt Processing on Evolution of Structure in PEEK

We report on the effects of melt processing temperature on structure formation in Poly(ether-ether-ketone), PEEK. Real time Small Angle X-ray Scattering, SAXS, and thermal analysis are used to follow the melting behavior after various stages of processing. Assignment of peaks to structural entities within the material, the relative perfection of the crystals, and the possibility of their reorganization, are all influenced by the melt processing history. With the advent of high intensity synchrotron sources of X-radiation, polymer scientists gain a research tool which, when used along with thermal analysis, provides additional structural information about the crystals during growth and subsequent melting. PEEK is an engineering thermoplastic polymer with a very high glass transition temperature (145 C) and crystal melting point (337 C). PEEK has been the subject of recent studies by X-ray scattering in which melt and cold crystallization were followed in real-time. X-ray scattering and thermal studies have been used to address the formation of dual endothermic response which has been variously ascribed to lamellar insertion, dual crystal populations, or melting followed by re-crystallization. Another important issue is whether all of the amorphous phase is located in interlamellar regions, or alternatively whether some is located in "pockets" away from the crystalline lamellar stacks. The interpretation of scattering from lamellar stacks varies depending upon whether such amorphous pockets are formed. Some groups believe all of the amorphous phase is interlamellar. This leads to selection of a smaller thickness for the crystals. Other groups suggest that most amorphous phase is not interlamellar, and this leads to the suggestion that the crystal thickness is larger than the amorphous layer within the stacks. To investigate these ideas, we used SAXS and Differential Scanning Calorimetry to compare results of single and dual stage melt crystallization of PEEK using a treatment scheme involving annealing/crystallization at T(sub a1) followed by annealing at T(sub a2) where either T(sub a1) < T(sub a2) or T(sub a1) > T(sub a2). We proposed a model to explain multiple melting endotherms in PPS, treated according to one or two-stage melt or cold crystallization. Key features of this model are that multiple endotherms: (1) are due to reorganization/recrystallization after cold crystallization; and, (2) are dominated by crystal morphology after melt crystallization at high T. In other words, multiple distinct crystal populations are formed by the latter treatment, leading to observation of multiple melting. PEEK 45OG pellets (ICI Americas) were the starting material for this study. Films were compression molded at 400 C, then quenched to ice water. Samples were heated to 375 C in a Mettler FP80 hot stage and held for three min. to erase crystal seeds before cooling them to T(sub a1) = 280 C . Samples were held at T(sub a2) for a period of time, then immediately heated to 360 C. In the second treatment samples were held at T(sub a1) = 31 C for different crystallization times t(sub c) then cooled to 295 C and held 15 min. In situ (SAXS) experiments were performed at the Brookhaven National Synchrotron Light Source with the sample located inside the Mettler hot stage. The system was equipped with a two-dimensional position sensitive detector. The sample to detector distance was 172.7 cm and the X-ray wavelength was 1.54 Angstroms. SAXS data were taken continuously during the isothermal periods and during the heating to 360 C at 5 C/min. Each SAXS scan was collected for 30 sec. Since the samples were isotropic, circular integration was used to increase the signal to noise ratio. After dual stage melt crystallization with T(sub a1) < T(sub a2) the lower melting endotherm arises from holding at T(sub a1). During cooling a broad distribution of crystals forms, and the low-melting tail is perfected during T(sub al). Heating to T(sub a2) melts these imperfect crystals and allows others with greater average long spacing to form in their place. After dual stage crystallization with T(sub a1) > T(sub a2), the amount of space remaining for additional growth at T(sub a2) depends upon the holding time at T(sub a1). The long period of crystals formed at T(sub a2) is smaller than that formed at T(sub a1) due to growth in a now-restricted geometry. Perfection of crystals is seen as an increase of the intensity of the population scattering at higher s, while the intensity of the population scattering at lower s stays constant. During heating from below to above the minor endotherm, we see rapid decrease of the intensity of the X-ray scattering corresponding to the population of crystals scattering in the shoulder. Another important observation is that after the sample is annealed at 295 C, the shoulder intensity is restored once again. The population scattering at higher s remains longer before it disappears in the sample treated to the second stage of melt crystallization, compared to the sample crystallized with a single stage. This could be interpreted as an effect of continued perfection of the less perfect population, which is also reflected in the increased melting temperature of the smaller endotherm as the holding time at 295 C increases. In the corresponding DSC scans we see a shift in the area and the peak temperature of the lower melting endotherm with an increase of the annealing time.

Georgiev, Georgi↗

NASA NTRS1977

Study of the ablative effects on tektites: Atmosphere entry of a swarm of tektites

The large variety of ablation markings observed on recovered tektites lead to the previously proposed swarm wake model which states that the lead peripheral tektites bore the blunt of aerodynamic heating upon entry, and that the bulk of tektites in the wake enjoyed partial shielding at the expense of the leaders. Further considerations are presented in support of this model. Quantitative assessments indicate that wake shielding might indeed have provided for substantially less heating than would have been experienced by a tektite entering an undisturbed atmosphere along a similar trajectory. For the case of strong wake shielding it is even possible that the surface temperature of a falling tektite had barely reached its melting point. In the distribution of tektites, there is a size band (near R = 0.5 cm) which is least susceptible to melting.

Sepri, P.↗

NASA NTRS1982

Solid impingement erosion mechanisms and characterization of erosion resistance of ductile metals

Experimental results pertaining to spherical glass bead and angular crushed glass particle impingement are presented. A concept of energy adsorption to explain the failure of material is proposed. The erosion characteristics of several pure metals were correlated with the proposed energy parameters and with other properties. Correlations of erosion and material properties were also carried out with these materials to study the effect of the angle of impingement. Analyses of extensive erosion data indicate that surface energy, strain energy, melting point, bulk modulus, hardness, ultimate resilience, atomic volume and product of linear coefficient of thermal expansion, bulk modulus, and temperature rise required for melting, and ultimate resilience, and hardness exhibit the best correlations. It appears that both energy and thermal properties contribute to the total erosion.

Rao, V. P.↗

NASA NTRS1984

Microgravity containerless processing in long drop tubes

Extensive experience in utilizing long drop tubes for studying effects of microgravity on the solidification of alloys was obtained. While some modifications are necessary to improve versatility, the facility proved to be most useful. Both an electron beam furnace and an electromagnetic levitation furnace can be used. The electron beam furnace is used with vacuum environments (0.00001 torr), whereas the levitation furnace is presently used only in inert gas environments (above 100 torr). Experiments are best applied to refractory alloys because of the sensitivity of the detectors now being used to observe solidification. Processing of lower melting point metals and alloys simply cannot be recorded. On the other hand, expected improvements in detector sensitivity will allow experimentation with relatively low melting alloys. In such cases, solidification will occur in flight only if higher inert gas pressure is used (100 to 760 torr) to increase heat loss by convection. Under these conditions microgravity conditions no longer apply. However, as shown by results to date, it is not microgravity as such that is important in drop tube solidification. Instead it is the containerless nature of the process that is significant, leading to large degrees of undercooling before solidification and therefore to unique alloys.

Bayuzick, R. J.↗

DOE OSTI2021

Development of Bismuth and Platinum Bi-Metallic Nanoparticles to Enhance Melt Wire Temperature Resolution

Advanced manufacturing (AM) based on direct-write (DW) technologies has emerged as the predominant enabler for the fabrication of active and passive sensors to be deployed in harsh operating environments seen in a nuclear reactor. Recently, Idaho National Laboratory and Boise State University have recently established capabilities to incorporate advanced manufacturing (AM) methods to accelerate, modernize and enhance functionality of nuclear sensors and instrumentation to achieve the goal of enhancing the safety and efficiency of nuclear reactors. A significant thrust of this work includes the development of nuclear relevant feedstock materials compatible with a variety of direct-write processes for the development, fabrication and testing of AM sensors for peak temperature detection and neutron flux monitoring. For this report, bismuth and bismuth/platinum (BiPt) bi-metallic nanoparticles were synthesized using wet chemical approaches to develop bi-metallic feedstock materials to enhance the sensitivity of melt wires for peak temperature detection. Nanoparticle characterization was performed with Transmission Electron Microscopy (TEM) for nanoparticle composition and size, Transmission X-Ray Diffraction Fluorescence (TXRF) for nanoparticle composition, and Differential Scanning Calorimetry to elucidate the melting point of BiPt bi-metallic nanoparticles. Preliminary results indicate bi-metallic BiPt nanoparticles as a viable pathway for fabricating high resolution AM melt wires.

36 MATERIALS SCIENCE↗

NASA NTRS1985

Characterization of solid particle erosion resistance of ductile metals based on their properties

This paper presents experimental results pertaining to spherical glass bead and angular crushed glass particle impingement. A concept of energy absorption to explain the failure of material is proposed and is correlated with the erosion characteristics of several pure metals. Analyses of extensive erosion data indicate that the properties - surface energy, specific melting energy, strain energy, melting point, bulk modulus, hardness, atomic volume - and the product of the parameters - linear coefficient of thermal expansion x bulk modulus x temperature rise required for melting, and ultimate resilience x hardness - exhibit the best correlations. The properties of surface energy and atomic volume are suggested for the first time for correlation purposes and are found to correlate well with erosion rates at different angles of impingement. It further appears that both energy and thermal properties contribute to the total erosion.

Rao, P. V.↗

DOE OSTI2022

Bi-metallic Nanoparticle Synthesis for Advanced Manufactured Melt Wires

Science Undergraduate Laboratory Internship (SULI) Program Report: Additive manufacturing (AM) based on direct-write technologies has emerged as the predominant method for the fabrication of passive sensors for the harsh operating environments seen in a nuclear reactor. Through the modification of previous methods, Idaho National Laboratory and Villanova University have improved the synthesis process for AM feedstock, which will allow for the improvement of advanced nuclear sensors and instrumentation. A major part of this work includes the synthesis process of relevant AM compatible feedstock to support the development, fabrication, and testing of AM sensors for peak temperature detection. For this report, bismuth, bismuth/platinum, tin, tin/silver, tin/zinc, indium, and indium/silver bi-metallic nanoparticles were synthesized using the polyol method, which will enhance temperature sensitivity and allow for miniaturization. To characterize the synthesized nanoparticles, we used x-ray fluorescence to evaluate the elemental composition of the nanoparticles and differential scanning calorimetry and thermogravimetric analysis to determine the melting point and mass loss of the samples. Results show that bi-metallic nanoparticles are a viable option for the fabrication of high-resolution AM melt wires. The temperature sensitivity can be brought to within 5°C and melt wires can be fabricated that are in the micrometer scale. This will expand the range of irradiation experiments melt wires can be used for and the measured temperature will be significantly more accurate.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

NASA NTRS1987

Cellular monotectic model solidification

Succinonitrile (sn) was purified to a superior level using a fractional recrystallization method. The melting point of the best twice recrystallized sn was not raised by following with double distillation. This was tested using differential scanning calorimetry. The peak shape on melting also proved that double distillation after double recrystallization did not improve the quality. Stability and phase diagrams for succinonitrile and glycerol are presented.

Kaukler, William F.↗

NASA NTRS1980

Critical analysis of nitramine decomposition data: Activation energies and frequency factors for HMX and RDX decomposition

A summary of a literature review on thermal decomposition of HMX and RDX is presented. The decomposition apparently fits first order kinetics. Recommended values for Arrhenius parameters for HMX and RDX decomposition in the gaseous and liquid phases and for decomposition of RDX in solution in TNT are given. The apparent importance of autocatalysis is pointed out, as are some possible complications that may be encountered in interpreting extending or extrapolating kinetic data for these compounds from measurements carried out below their melting points to the higher temperatures and pressure characteristic of combustion.

Schroeder, M. A.↗

NASA NTRS1985

Solder Bonding for Power Transistors

Indium solder boosts power rating and facilitates circuit changes. Efficient heat conduction from power transistor to heat sink provided by layer of indium solder. Low melting point of indium solder (141 degrees C) allows power transistor to be removed, if circuit must be reworked, without disturbing other components mounted with ordinary solder that melts at 181 degrees C. Solder allows devices operated at higher power levels than does conventional attachment by screws.

Snytsheuvel, H. A.↗

DOE OSTI2021

Investigation of Surface Skidding Response of PBX 9501 and PBX 9502

Introduction: Assess the hazards of handling polymer bonder explosives(PBX) for the case of skidding with grit particles in the frictional interface. High explosive (HE) materials tested: PBX 9501 and 9502. High melting point materials at the skidding interface between HE and a substrate is known to increase the probability of ignition by creating hot spots not subject to reduced heating from the melting of HE material. Skidding occurred at peak forces of 6-26 kN normal force, and 0.6-3.4 kN of frictional force. Velocities for skidding range from 5-30 m/s, see figure 7. Sparse amounts of 300 μm silica grit is applied loosely to the HE surface before testing. Previous works have tested ignition by grit. Testing parameters include angle of impact, drop height, grit size, grit density, substrate material. This study focuses on pre ignition conditions and detailed thermal imaging of the frictional interface. Conclusions: Temperature hot spots were observed at high points in HE surface topology. These high points may be created by grit particles. Since these points impact first high frictional work is concentrated and quickly increases temperature. Small amounts of grit do not affect the overall frictional force but do concentrate the frictional work to create hot spots.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Predicted Heat Flux Performance of Actively Cooled Tungsten-Armored Graphitic Foam Monoblocks

Tungsten (W)–armored graphitic foam monoblocks were developed for applications requiring high-Z plasma-facing material in long-pulse fusion experiments and ultimately deuterium-tritium fusion reactors. The monoblocks are an integrated material system combining the advantages of a chemical vapor deposited (CVD) W coating with a high-conductivity graphitic foam. The W is a high-melting-point, high-Z material with low tritium retention. The graphitic foam coupled to a swirl tube serves as a high-thermal-conductivity heat sink that cannot melt, although it can sublime at much higher temperatures than copper melts. Together, they comprise a robust plasma-facing component (PFC) weighing roughly 5% of an all-W component or 17% of a traditional W-coated copper heat sink.A single-channel mock-up consisting of four graphitic foam monoblocks equipped with a water-cooled swirl tube was fabricated for eventual testing in the 60-kW, EB-60, rastered electron beam at the Applied Research Laboratory of The Pennsylvania State University. Two monoblocks have a thin 50-μm-thick coating of pure W chemically vapor deposited over NbC and pure Nb interlayers. Two others have a 2-mm-thick pure W coating CVD on graphitic monoblocks using the same interlayers. The mock-up will be cooled with available 10 m/s, 0.7 MPa water with a 22°C inlet temperature and subjected to varying uniform heat loads up to 20 MW/m 2 . It is equipped with type-K thermocouples at various depths, and calibrated infrared thermography and spot pyrometry will be used to characterize the heated surface. Real-time water calorimetry will be used to ascertain the absorbed steady-state power and infer the heat flux during testing. Since testing cannot be done under prototypic divertor flow conditions, it is necessary to predict the thermal response of this novel PFC system and investigate the power sharing between radiation and convection at divertor heat flux levels and its inherent ability to avoid critical heat flux. Results are reported for predictions obtained from computational fluid dynamics models up to 30 MW/m 2 of steady-state uniform heat flux. Leading-edge heat loads of 30 MW/m 2 on a 2-mm-wide side strip were also investigated to ascertain if coating delamination is likely.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

DOE OSTI2022

Optimization of Preparation Method, Nucleating Agent, and Stabilizers for Synthesizing Calcium Chloride Hexahydrate (CaCl2.6H2O) Phase Change Material

This study investigates improvements in low-cost latent heat storage material calcium chloride hexahydrate (CaCl2.6H2O). Its melting point is between 25 and 28 °C, with relatively high enthalpy (170–190 J/g); however, this phase change material (PCM) shows supercooling and phase separation. In CaCl2.6H2O incongruent melting causes lower hydrates of CaCl2 to form, which affects the overall energy storage capacity and long-term durability. In this work, PCM performance enhancement was achieved by adding SrCl2.6H2O as a nucleating agent and NaCl/KCl as a stabilizer to prevent supercooling and phase separation, respectively. We investigated the PCM preparation method and optimized the proportions of SrCl2.6H2O and NaCl/KCl. Thermal testing for 25 cycles combined with DSC and T-history testing was performed to observe changes in enthalpy, phase transitions and supercooling over the extended period of usage. X-ray diffraction was used to verify crystalline structure in the compounds. It was found that the addition of 2 wt.% of SrCl2.6H2O reduced supercooling from 12 °C to 0 °C compared to unmodified CaCl2.6H2O. The addition of 5 wt.% NaCl or KCl proved to effectively suppress separation and the melting enthalpy achieved was 169 J/g–178 J/g with congruent melting over 25 cycles, with no supercooling and almost no reduction in the latent heat.

42 ENGINEERING↗

DOE OSTI2022

Laser pulse shaping for additive manufacturing

The present disclosure relates to an apparatus for additively manufacturing a product in a layer-by-layer sequence, wherein the product is formed using powder particles deposited on an interface layer of a substrate. A laser generates first and second beam components. The second beam component has a higher power level and a shorter duration than the first beam component. A mask creates a 2D optical pattern in which only select portions of the second beam components can irradiate the powder particles. The first beam component heats the powder particles close to a melting point, where the particles experience surface tension forces relative to the interface layer. While the particles are heated, the second beam component further heats the particles and also melts the interface layer before the surface tension forces can act on and distort the particles, enabling the particles and the interface layer are able to bond together.

DeMuth, James A.↗

DOE OSTI2023

Laser pulse shaping for additive manufacturing

DeMuth, James A.↗

DOE OSTI2022

Multicomponent Nanoparticle Synthesis for Advanced Manufactured Melt Wire Development

Additive manufacturing (AM) based direct-write technologies have emerged as a predominant enabler for the fabrication of advanced passive sensors in-pile applications. This work continues previous efforts with the modification and optimization of synthesis methods for multi-component nanoparticle systems used to support the development, fabrication and testing of AM sensors for peak temperature detection. For this report, bismuth, bismuth/platinum, tin, tin/silver, tin/zinc, indium, and indium/silver bi-metallic nanoparticles were synthesized using the wet chemical methods. The nanoparticles were then characterized with x-ray fluorescence to evaluate the elemental composition and differential scanning to determine the melting point and mass loss of the samples. Results continue to show that bi-metallic nanoparticles are a viable pathway for the fabrication of high-resolution AM melt wires.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Thermal Analysis of High Entropy Rare Earth Oxides

Phase transformations in multicomponent rare earth sesquioxides were studied by splat quenching from the melt, high temperature differential thermal analysis and synchrotron X-ray diffraction on laser-heated samples. Three compositions were prepared by the solution combustion method: (La,Sm,Dy,Er,RE) 2 O 3 , where all oxides are in equimolar ratios and RE is Nd or Gd or Y. After annealing at 800 °C, all powders contained mainly a phase of C-type bixbyite structure. After laser melting, all samples were quenched in a single-phase monoclinic B-type structure. Thermal analysis indicated three reversible phase transitions in the range 1900–2400 °C, assigned as transformations into A, H, and X rare earth sesquioxides structure types. Unit cell volumes and volume changes on C-B, B-A, and H-X transformations were measured by X-ray diffraction and consistent with the trend in pure rare earth sesquioxides. The formation of single-phase solid solutions was predicted by Calphad calculations. The melting point was determined for the (La,Sm,Dy,Er,Nd) 2 O 3 sample as 2456 ± 12 °C, which is higher than for any of constituent oxides. An increase in melting temperature is probably related to nonideal mixing in the solid and/or the melt and prompts future investigation of the liquidus surface in Sm 2 O 3 -Dy 2 O 3 , Sm 2 O 3 -Er 2 O 3 , and Dy 2 O 3 -Er 2 O 3 systems.

36 MATERIALS SCIENCE↗

NASA NTRS1984

Hot melt adhesive pad surface attachment assembly concept for on-orbit operations

The use of a hot melt adhesive concept to develop a Surface Attachment Assembly (SAA) for on-orbit attachment and detachment operations for the Manned Maneuvering Unit (MMU) was investigated. The concept involved impregnation of the hot melt adhesive into a fiberglass covered pad which contained electrical heating and thermoelectric cooling devices. The polyamide hot melt adhesive selected can be repeatedly heated to its melting point in a vacuum and provide good adhesion to various surfaces, i.e., reusable surface insulation tiles, metals, and composites, when cooled. After a series of adhesive screening tests, Jet-Melt 3746 was selected from a group of commercially available thermoplastic adhesive candidates which met or exceeded many of the criteria established for the SAA system. The SAA system was designed and fabricted with the goal of proving the concept with a working model rather than attempting to optimize all facets of the system. This system evolved by investigating alternate attachment concepts, designing and fabricating electronic systems to heat and cool the adhesive, and then fabricating electronic systems to heat and cool the adhesive, and then fabricating and testing two prototype full-size units.

Progar, D. J.↗