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580 records · Page 33
All sourcesNASA NTRSDOE OSTI
NASA NTRS2018

Impact of Powder Variability on the Microstructure and Mechanical Behavior of Selective Laser Melted Alloy 718

Powder-bed additive manufacturing processes use fine powders to build parts layer-by-layer. Alloy 718 powder feedstocks for selective laser melting (SLM) additive manufacturing are produced commercially by both gas and rotary atomization and are available typically in the 10-45 or 15-45 microns size ranges. A comprehensive investigation was conducted to understand the impact of powder variability on the microstructure and mechanical behavior of SLM 718 heat treated to Aerospace Material Specification (AMS) 5664. This study included sixteen virgin powders and three once-recycled powders within the 10-45 and 15-45 microns size ranges that were obtained from seven direct source suppliers and one reseller. Although alike as highly regular spheroids, these powders showed distinct differences in composition (especially Al, C and N contents), particle size distributions, and powder features such as degree of agglomeration, fusion and surface roughness. Compositional differences expectedly had the strongest impact on microstructure. High N and C contents formed TiN-nitrides and/or (Nb,Ti,Mo)-C carbides on the grain boundaries, prevented recrystallization during heat treatment, and resulted in retained (001)-scalloped shaped grains that ranged from 19 to 41 microns in average size. In the absence of this particle pinning, the average grain size of the heat treated SLM 718 ranged from 51 microns to 90 microns. Room temperature tensile and high cycle fatigue (HCF) testing compared as-fabricated (AF) and low stress ground (LSG) surface conditions. Tensile testing revealed consistent behavior between the two surface conditions and amongst the powder lots. The finer grained SLM 718 builds displayed the lowest tensile properties. A SLM 718 build fabricated from a powder with eight times lower C content showed statistically better tensile properties presumably due to enhanced coarsening of (delta)-Ni3Nb precipitates. The specimens from once-recycled powders had slightly higher tensile strengths and slightly higher ductility compared to their virgin equivalents; once-recycling also did not substantially degrade the mean HCF life. The LSG fatigue lives agreed with conventionally manufactured 718 data, while AF lives exhibited a knock-down due to surface roughness. The fatigue lives of AF specimens were statistically equivalent across powder lots except for one and failures typically initiated at stress concentrators associated with SLM surface asperities. Fatigue testing of low stress ground specimens result in both transgranular and within facet crack initiations. More than half of the cracks initiated from these facets for the machined condition; however, these facets appeared to be within grains that were larger-than-average in size. A nitrogen-atomized powder with fine prior particles of TiN-nitrides and M(Ti,Nb,Mo)C carbides from atomization on powder surfaces resulted in the best fatigue performance with segregation of these particles to the SLM 718 grain boundaries leading to higher resistance to early-stage crack propagation. Typically the fine-grained builds with minor phases along the grain boundaries did not perform well in fatigue, whereas a larger-grain build with lower carbon content and coarser delta-Ni3Nb precipitates showed the next best HCF response. Further details of the build microstructure and its impact on tensile and fatigue behavior was considered.

laser deposition↗
NASA NTRSDate not supplied

In-Situ Detection of Process-Induced Porosity During Cure of Out-of-Autoclave Composites

Composite materials offer unique benefits in aerospace applications, including high strength-to-weight ratio, and are becoming increasingly used by industry manufacturers. Current manufacturing and processing methods can lead to defects in the composites, which are identified after fabrication using inspection methods. This study utilized a high-temperature ultrasonic inspection system to detect process-induced porosity in an out-of-autoclave (OOA) composite panel during cure. In order to perform ultrasonic scans in-situ during cure, the system needed to be able to operate at oven temperatures up to 200 °C. There are no commercially available ultrasonic scanning systems that can operate continuously at these temperatures, so an enclosure was fabricated to insulate the ultrasonic system in the curing oven. The enclosure housed a MISTRAS® motorized X-Y raster scanner and contact transducer (Olympus® X2002). The Olympus® X2002 contact transducer is a continuous high-temperature delay line transducer with a center frequency of 2.25 MHz. In order to prevent the inside of the enclosure from reaching high temperatures, a sparge pipe inside the cooling enclosure was connected to a liquid nitrogen (LN2) tank outside of the oven via insulated hoses. The cooling system was automatically controlled by a temperature controller that was programmed to open a solenoid valve along the hose at 31 ℃ and close at 28 ℃ inside the cooling enclosure. When the solenoid valve was open, LN2 would flow from the LN2 tank and vaporize prior to reaching cooling enclosure. A U-shaped sparge pipe had holes drilled along its length to uniformly introduce cold nitrogen gas into the cooling enclosure. This prevented the motors from ever reaching the maximum desired operating temperature of 38 ℃. In the bottom of the enclosure, the tool plate was placed with the composite facing the outside of the enclosure, exposing it to the temperatures of the oven. The tool plate was 63.5 mm thick borosilicate glass, which was chosen for its low ultrasonic attenuation and moderate thermal conductivity. A thin layer of ultrasonic couplant was placed on the tool plate. The transducer sent and received ultrasonic waves through the tool plate into the composite. A MISTRAS® Remote UT System performed all wave generation, analog to digital conversion, and data acquisition and processing. The transducer was connected directly to the Remote UT System via a high-temperature BNC cable (CD International, RG-316). Polyimide insulated copper wire was used to connect the scanner to a 2-axis motor drive, which was connected to the Remote UT System. The motor drive and Remote UT System were located outside the industrial oven. A diagram of the ultrasonic system is shown in Figure 1. Figure 1: Diagram of ultrasonic in-situ defect detection system. In this study, a porosity gradient was introduced into the carbon fiber reinforced polymer (CFRP) composite through a misfit of the part and caul plate. A 24-ply quasi-isotropic ([0/90, ±45]12S) composite panel was laid up using Newport® AS4C-M/NB321 out-of-autoclave (OOA) plain weave (PW) prepreg (42% resin content, 195 g/m2). The first 16 plies were 203 mm × 203 mm. Ply drops were incorporated into the panel by decreasing the length of plies 17-24. The sizes of each ply are included in Table 1. All plies were centered along their length (x-axis) creating a trapezoidal type cross-section. Table 1: Ply sizes Plies Length (mm) Width (mm) 1-16 203 203 17-18 102 203 19-20 85 203 21-22 68 203 23-24 51 203 A 15-5 stainless steel caul plate (Size: 203 × 203 × 1.2 mm) was placed on the laminate. The composite and caul plate were vacuum bagged to the tool plate. Per the product datasheet, Newport 321 can be cured between 121 °C and 149 °C, depending on service temperature, with a hold for 90-120 minutes. Based on prior thermal testing of the cooling enclosure, the desired composite temperature cycle could be attained when the air temperature of the oven was ramped to 160 °C at a rate of 1.7 °C/min with a 3 hour hold. The extended hold was not necessary to cure the composite, but did allow for additional scans at the cure temperature during preliminary testing. The composite panel was under vacuum pressure for the entire cure cycle. Under vacuum, the caul plate deformed causing high and low pressure regions. The low-pressure regions formed high porosity in the composite part. The ultrasonic data collected showed that the inspection system was able to monitor the evolution of porosity within the composite throughout the cure cycle. Fifty scans of a 203 mm × 51 mm (8 in. × 2 in.) area of the composite were completed throughout the cure cycle. The scan speed was set to 43 mm/s in the x-direction and 36 mm/s in the y-direction, with a 1.0 mm/pixel resolution in both directions. Each scan took approximately five minutes to complete. Figure 2 shows C-scan amplitude data (top view) from one scan during the cure cycle. The color map indicates the maximum amplitude (%) measured with a time gate that contains reflections from the back surface (furthest from the transducer in contact with the caul plate) of the composite. Because porosity in the composite increases the ultrasonic attenuation in the composite part, a higher amplitude (red) indicates low porosity and a lower amplitude (blue) indicates high porosity. The regions where the caul plate was applying increased pressure (center and ends of the panel) resulted in reduced porosity, whereas the ply drop regions had reduced pressure and thus had higher porosity. Figure 2: Amplitude C-scan (top view) of OOA composite from one scan during the 160 °C temperature hold. Higher amplitude (red) indicates low porosity. Lower amplitude (blue) indicates high porosity. A B-scan is a two-dimensional image plotting the ultrasonic signals from a single y-position at every x-location of the composite panel. The travel time (μs) of the ultrasonic wave (representing the through-thickness location) is plotted along the y-axis, and the ultrasonic wave signal is represented as a contour map. Based on the B-scan data, the location of the defects with respect to the composite thickness was able to be determined. The ply drop regions had high porosity near the front (tool plate) surface of the composite (Figure 3). Figure 3: B-scan (cross-section view) of OOA composite from one scan during the 160 °C temperature hold. Using the data obtained from amplitude C-scans and B-scans throughout the cure cycle, the high and low porosity regions within the composite laminate were detected and localized with high spatial resolution. This paper will discuss the evolution of porosity content in the OOA composite during cure. OOA tests aided the transition of this system to an autoclave, which is the primary method of curing aerospace-grade thermoset composites.

Tyler B. Hudson↗
DOE OSTI2021

Characterization of Nanoscale Pores in Tight Gas Sandstones Using Complex Techniques: A Case Study of a Linxing Tight Gas Sandstone Reservoir

Pore structures with rich nanopores and permeability in tight gas reservoirs are poorly understood up to date. Advanced techniques are needed to be employed to accurately characterize pore structures, especially tiny pores which include micron and nanopores. In this study, various experimental techniques such as scanning electron microscopy (SEM), nuclear magnetic resonance (NMR) T 2 , nitrogen adsorption method, and NMR cryoporometry (NMRC) are combined to interrogate the complex pore systems of the tight gas reservoir in the Linxing formation, Ordos Basin, China. Results show that tight gas sandstones are primarily comprised of residual interparticle and clay-dominated pores. Clay and quartz are two dominate minerals while pyrite occupies a nontrivial amount as well. The permeability of tight gas sandstones is very low, exhibiting an extremely poor positive correlation with porosity. While pore types and relative pore contents are more influential factors on the permeability, accurate characterization of pore size distribution is critical for the permeability of tight gas sandstones. Therefore, complementary characterization methods are carried out, indicating that neither small pores with radii < 100 nm (around peak 1 in NMR T 2 distribution) nor large pores with radii > 5 μ m (around peak 3 in NMR T 2 distribution) control the permeability by analyzing the connectivity of the pores in various size ranges, but rather pores averaging approximately 350 ± X nm (around peak 2 in NMR T 2 distribution) have sufficient connectivity to host and transmit hydrocarbons. The pore size of tight gas sandstones is dominated by the clay-rich mineral assemblage. The study shows that the NMRC technique can be a very promising method, especially when referred to as a promising “roadmap” on how to interrogate tight formations such as the tight gas sands or even shale especially for the nanopore characterization.

15 GEOTHERMAL ENERGY↗
DOE OSTI2023

Stability study of aqueous foams under high-temperature and high-pressure conditions relevant to Enhanced Geothermal Systems (EGS)

In Enhanced Geothermal System (EGS) hydraulic fracturing is carried out by injecting cold water into deep Hot Dry Rocks (HDR) under carefully controlled conditions to create new or reopen existing fractures. Water-based fracturing fluids demonstrate some challenges including immense quantity of water usage, water sensitivity of the formations, water blocking, and lack of proppant carrying capacity and transportation. Thus, an alternative is to use foam-based fracturing fluid which offers potential advantage over conventional water-based fracturing fluid such as minimum water usage, reduced wellbore damage, high proppant carrying capacity, and less environmental damage. However, foams are complex mixture of gaseous phase and liquid phase which are thermodynamically unstable at downhole conditions, and their stability can decrease over time due to liquid drainage, bubble coarsening, and coalescence. This paper shows laboratory experiments executed to study foam stability at high temperature (200°C) and high pressure (6.9MPa) conditions which simulates the geothermal environment. Foam stability was characterized by half-life of foam, which is defined as the time taken by the foam to decreases by 50% of its original height due to drainage. In this paper, two types of gaseous phases, nitrogen (N 2 ) and carbon dioxide (CO 2 ) were investigated. Also, based on successful practice of foam-based fracturing fluid in oil and gas industries, four surfactants, including Alpha olefin sulfonate (AOS), Sodium dodecyl sulfonate (SDS), Tergitol™ (NP – 40), and Cetyltrimethylammonium chloride (CTAC) at optimum concentration of 1wt.% were tested for best stability performance. In addition, different stabilizing agents including guar gum, bentonite clay, crosslinker, silicon dioxide nanoparticles (SiO 2 ), graphene oxide (GO) were also studied. Experimental results showed that N 2 foams were more stable than CO 2 foams. It was observed that foam half-life decreased with the increase in temperature. Among all the surfactants, AOS foams showed the most promising thermal stability at high temperatures. Moreover, with the addition of stabilizing agents, foam's half-life was enhanced. Stabilizing agents such as crosslinker and GO dispersion showed the most stable foams with half-life recorded at 20min and 17min, respectively, at 200°C and 6.9MPa. Finally, pressure also showed a positive effect on foam stability; with increased pressure, foam half-life was increased. Based on the experimental data, analytical models for the effect of temperature and pressure were developed, considering foam degradation is a first-order kinetic reaction that linearly depends on the foam drainage mechanism. The effect of temperature on foam half-life was studied as an exponential decay model. In this model, foam half-life is a function of drainage rate constant (D A ) and activation energy (E a ) of the foam system. The effect of pressure on foam half-life was found to obey a power-law model where an increase in pressure showed an increase in foam half-life. Furthermore, a linear relation was studied for the effect of pressure on foam activation energy and drainage rate. Then the combined effects of temperature and pressure were studied, which yielded an analytical model to predict the foam stabilities in terms of half-life for different foam compositions. In conclusion, this research indicates that with an appropriate selection of surfactants and stabilizing agents, it is possible to obtain stable foams, which could replace conventional water fracturing fluid under EGS conditions.

15 GEOTHERMAL ENERGY↗