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All sourcesNASA NTRSDOE OSTI
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↗
NASA NTRS1984

A blackbody-pumped CO2-N2 transfer laser

A compact blackbody-pumped CO2-N2 transfer laser was constructed and the significant operating parameters were investigated. Lasing was achieved at 10.6 microns by passing preheated N2 through a 1.5-mm-diameter nozzle to a laser cavity where the N2 was mixed with CO2 and He. An intrinsic efficiency of 0.7 percent was achieved for an oven temperature of 1473 K and N2 oven pressure of 440 torr. The optimum laser cavity consisted of a back mirror with maximum reflectivity and an output mirror with 97.5-percent reflectivity. The optimum gas mixture was 1CO2/.5He/6N2. The variation of laser output was measured as a function of oven temperature, nozzle diameter, N2 oven pressure, He and CO2 partial pressures, nozzle-to-oven separation, laser cell temperature, and output laser mirror reflectivity. With these parameters optimized, outputs approaching 1.4 watts were achieved.

Deyoung, R. J.↗
NASA NTRS2010

Power Generator with Thermo-Differential Modules

A thermoelectric power generator consists of an oven box and a solar cooker/solar reflector unit. The solar reflector concentrates sunlight into heat and transfers the heat into the oven box via a heat pipe. The oven box unit is surrounded by five thermoelectric modules and is located at the bottom end of the solar reflector. When the heat is pumped into one side of the thermoelectric module and ejected from the opposite side at ambient temperatures, an electrical current is produced. Typical temperature accumulation in the solar reflector is approximately 200 C (392 F). The heat pipe then transfers heat into the oven box with a loss of about 40 percent. At the ambient temperature of about 20 C (68 F), the temperature differential is about 100 C (180 F) apart. Each thermoelectric module, generates about 6 watts of power. One oven box with five thermoelectric modules produces about 30 watts. The system provides power for unattended instruments in remote areas, such as space colonies and space vehicles, and in polar and other remote regions on Earth.

Saiz, John R.↗
NASA NTRS2003

Review of Laser Ablation Process for Single Wall Carbon Nanotube Production

Different types of lasers are now routinely used to prepare single wall carbon nanotubes (SWCNTs). The original method developed by researchers at Rice University utilized a "double pulse laser oven" process. A graphite target containing about 1 atomic percent of metal catalysts is ablated inside a 1473K oven using laser pulses (10 ns pulse width) in slow flowing argon. Two YAG lasers with a green pulse (532 nm) followed by an IR pulse (1064 nm) with a 50 ns delay are used for ablation. This set up produced single wall carbon nanotube material with about 70% purity having a diameter distribution peaked around 1.4 nm. The impurities consist of fullerenes, metal catalyst clusters (10 to 100 nm diameter) and amorphous carbon. The rate of production with the initial set up was about 60 mg per hour with 10Hz laser systems. Several researchers have used variations of the lasers to improve the rate, consistency and study effects of different process parameters on the quality and quantity of SWCNTs. These variations include one to three YAG laser systems (Green, Green and IR), different pulse widths (nano to microseconds as well as continuous) and different laser wavelengths (Alexandrite, CO, CO2, free electron lasers in the near to far infrared). It is noted that yield from the single laser (Green or IR) systems is only a fraction of the two laser systems. The yield seemed to scale up with the repetition rate of the laser systems (10 to 60 Hz) and depended on the beam uniformity and quality of the laser pulses. The shift to longer wavelength lasers (free electron, CO and CO2) did not improve the quality, but increased the rate of production because these lasers are either continuous (CW) or high repetition rate pulses (kHz to MHz). The average power and the peak power of the lasers seem to influence the yields. Very high peak powers (MegaWatts per square centimeter) are noted to increase ablation of bigger particles with reduced yields of SWCNTs. Increased average powers seem to help the conversion of the carbon from target into vapor phase to improve formation of nanotubes. The use of CW far infrared lasers reduced the need for the oven, at the expense of controlled ablation. Some of these variations are tried with different combinations and concentrations of metal catalysts (Nickel with Cobalt, Iron, Palladium and Platinum) different buffer gases (e.g. Helium); with different oven temperatures (Room temperature to 1473K); under different flow conditions (1 to 1000 kPa) and even different porosities of the graphite targets. It is to be noted that the original Cobalt and Nickel combination worked best, possibly because of improved carbonization with stable crystalline phases. The mean diameter and yield seemed to increase with increasing oven temperatures. Thermal conductivity of the buffer gas and flow conditions dictate the quality as well as quantity of the SWCNTs. Faster flows, lower pressures and heavier gases seem to increase the yields. This review will attempt to cover all these variations and their relative merits. Possible growth mechanisms under these different conditions will also be discussed.

Arepalli, Sivaram↗
DOE OSTI2024

Measuring thermomechanical response of large-format printed polymer composite structures via digital image correlation

Large-format additive manufacturing (LFAM) is a branch of additive manufacturing (AM) research with the ability to create large structures typically measuring several meters in scale. LFAM is advantageous for tooling applications, not only because it offers the ability to create complex geometries not easily made using subtractive manufacturing processes, but the cost savings of pelletized feedstock used by these systems result in larger parts printed at faster speeds than traditional AM systems. Fiber reinforced polymer (FRP) is a commonly used feedstock material in LFAM structures because it reduces the distortion experienced during printing. However, FRP introduces highly anisotropic thermomechanical properties and contributes to a nonhomogeneous microstructure that can result in critical distortion of dimensions during tooling. Measuring the global thermomechanical response of LFAM structures requires a more representative method that accounts for not only anisotropic properties but also the nonhomogeneous nature of the final part. This is where traditional techniques to measure thermomechanical response, such as thermomechanical analysis (TMA), fall short as they assume homogeneity. This study evaluated the coefficient of thermal expansion (CTE) of LFAM structures as measured by TMA as compared to a novel digital image correlation oven (DIC Oven) system. The LFAM structures were made from 20 % by weight carbon fiber reinforced acrylonitrile butadiene styrene (CF-ABS). TMA measurements showed significant variations in CTE across a single LFAM bead, confirming the need for a global technique that captures overall thermomechanical response. The CTE values measured using the DIC Oven compared well to average TMA values obtained from localized measurements across the sample. The DIC Oven was also used to quantify the effects of different layer orientations on thermomechanical properties, which cannot be easily captured using TMA. A predictive model was also developed by using localized TMA values across an LFAM bead to predict the overall thermomechanical response of an LFAM structure.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Temperature Dependence of FDR Response for Thermally Aged Low-Voltage Cables

Frequency Domain Reflectometry (FDR) has attracted significant attention for use in nuclear power plants (NPPs) for non-destructive cable health monitoring. However, cable aging detection using FDR faces challenges due to its high sensitivity to environmental factors such as temperature, vibrations, proximity to other cables, and so on. This work aims to evaluate the influence of measurement temperature on the FDR reflected signal in a low voltage cable undergoing accelerated thermal aging. A 100 ft long multi-core low-voltage unshielded power cable insulated with flame retardant ethylene propylene rubber (FR-EPR) and covered by a chloro-polyethylene (CPE) jacket was selected for this study. The cable was energized during aging by a 480 VAC 3-phase motor, and a 30 ft mid-section of this cable was routed through an air circulating oven held at 140 °C for up to an effective aging time of 62 days. FDR measurements were taken periodically with the oven on (at 140 °C) and with the oven off (at 22 °C). A comparative analysis of data collected at both temperatures showed that the FDR response was strongly dependent on measurement temperature. FDR measurements at ambient temperature showed large peaks corresponding to impedance changes in the aged section of the cable after 3 days of aging. These peaks continued to rise steadily with increasing aging time. However, for measurements taken at 140 °C, slowly rising peaks in the oven region (aged section) were observed only after a lead time of 23 days of aging. This work highlights the importance of measurement temperature on the performance of FDR as a condition monitoring tool for aging cables.

Sriraman, Aishwarya↗
NASA NTRS1985

Real-time measurement of sodium chloride in individual aerosol particles by mass spectrometry

The method of particle analysis by mass spectrometry has been applied to the quantitative measurement of sodium chloride in individual particles on a real-time basis. Particles of known masses are individually introduced, in the form of a beam, into a miniature Knudsen cell oven (1600 K). The oven is fabricated from rhenium metal sheet (0.018 mm thick) and is situated in the ion source of a quadrupole mass spectrometer. A particle once inside the oven is trapped and completely volatilized; this overcomes the problem of partial volatilization due to particles bouncing from the filament surface. Individual particles are thermally volatilized and ionized inside the rhenium oven, and produce discrete sodium ion pulses whose intensities are measured with the quadrupole mass spectrometer. An ion pulse width of several milliseconds (4-12 ms) is found for particles in the mass range 1.3 x 10 to the -13th to 5.4 x 10 to the -11th g. The sodium ion intensity is found to be proportional to the particle mass to the 0.86-power. The intensity distribution for monodisperse aerosol particles possesses a geometric standard deviation of 1.09, showing that the method can be used for the determination of the mass distribution function with good resolution in a polydisperse aerosol.

Sinha, M. P.↗
NASA NTRS1998

Evaluation of Heating Methods for Thermal Structural Testing of Large Structures

An experimental study was conducted to evaluate different heating methods for thermal structural testing of large scale structures at temperatures up to 350 F as part of the High Speed Research program. The heating techniques evaluated included: radiative/convective, forced convective, and conductive. The radiative/convective heaters included finned strip heaters, and clear and frosted quartz lamps. The forced convective heating was accomplished by closed loop circulation of heated air. The conductive heater consisted of heating blankets. The tests were conducted on an 1/8 inch thick stainless steel plate in a custom-built oven. The criteria used for comparing the different heating methods included test specimen temperature uniformity, heater response time, and consumed power. The parameters investigated included air circulation in the oven, reflectance of oven walls, and the orientation of the test specimen and heaters (vertical and horizontal). It was found that reflectance of oven walls was not an important parameter. Air circulation was necessary to obtain uniform temperatures only for the vertically oriented specimen. Heating blankets provided unacceptably high temperature non-uniformities. Quartz lamps with internal air circulation had the lowest power consumption levels. Using frosted quartz lamps with closed loop circulation of cool air, and closed loop circulation of heated air provided the fastest response time.

Daryabeigi, Kamran↗
NASA NTRS2000

Modeling Specular Exchange Between Concentric Cylinders in a Radiative Shielded Furnace

The objective of this research is to develop and validate mathematical models to characterize the thermal performance of a radiative shielded furnace, the University of Alabama in Huntsville (UAH) Isothermal Diffusion Oven. The mathematical models are validated against experimental data obtained from testing the breadboard oven in a terrestrial laboratory environment. It is anticipated that the validation will produce math models capable of predicting the thermal performance of the furnace over a wide range of operating conditions, including those for which no experimental data is available. Of particular interest is the furnace core temperature versus heater power parametric and the transient thermal response of the furnace. Application to a microgravity environment is not considered, although it is conjectured that the removal of any gravity dependent terms from the math models developed for the terrestrial application should yield adequate results in a microgravity environment. The UAH Isothermal Diffusion Oven is designed to provide a thermal environment that is conducive to measuring the diffusion of high temperature liquid metals. In addition to achieving the temperatures required to melt a sample placed within the furnace, reducing or eliminating convective motions within the melt is an important design consideration [1]. Both of these influences are reflected in the design of the furnace. Reducing unwanted heat losses from the furnace is achieved through the use of low conductivity materials and reflective shielding. As evidenced by the highly conductive copper core used to house the sample within the furnace, convective motions can be greatly suppressed by providing an essentially uniform thermal environment. An oven of this design could ultimately be utilized in a microgravity environment, presumably as a experiment payload. Such an application precipitates other design requirements that limit the resources available to the furnace such as power, mass, volume, and possibly even time. Through the experimental and numerical results obtained, the power requirements and thermal response time of the breadboard furnace are quantified.

Schunk, Richard Gregory↗
NASA NTRS1998

Eating on Demand

Under subcontract to McDonnell-Douglas Corporation, Enersyst Development Center developed air impingement technology through oven designs for NASA's Space Station Freedom. Jets of hot air at the top and bottom of the oven are focused on the food, rather than heating the oven cavity as in a traditional thermal oven. By heating the food directly, foods cook faster and more consistently, retaining flavor and texture. Several companies have licensed this technology, including KRh Thermal Systems, which has introduced a line of Hot Choice vending machines. Enersyst has also licensed the first home application to Thermador.

Source record↗
NASA NTRS2025

System for Long-Duration Electrical Testing of SiC IC Generation 12 Chips at 500 °C

The system described in this report is an improved testing rig designed to enhance measurement flexibility, provide a compact oven footprint, and reduce costs for parallel oven-testing silicon carbide (SiC) integrated circuit devices at 500 °C for long durations (greater than 100 h). The testing rig design was characterized in terms of the ovens’ internal and external temperatures, system noise, and the leakage properties of their substrate/inner boards, where the devices under test (DUTs) reside. The test rig employs a National Instruments (NI) Peripheral Component Interconnect eXtensions for Instrumentation (PXI) measurement system, room-temperature pin-switching/customizing boards, and high-temperature compact ovens.

Stephanie Booth↗
DOE OSTI2021

Precision cooking system

The present invention comprises a precision cooking oven that utilizes laser sheets to cook food, thus creating homogeneously heated and uniformly seared food bodies and surfaces. Laser sheets move back and forth evenly injecting heat into items being cooked. All food cold or hot areas can be eliminated since intersecting laser lines can be completely projected on and accommodate an item's exterior surfaces. Items with non-uniform cross-sections and properties can be cooked uniformly by controlling the exact amount of energy projected into differing sections of the food. The oven is also capable of cooking autonomously. Since laser sheets can be precisely controlled, cooking results can be very predictable once the boundary conditions for a thermal analysis are determined. The oven can detect the properties of the items to be cooked and thereafter compute the needed time and power to achieve the desired results stipulated by an oven operator.

Lee, Henry Yu-Heng↗
DOE OSTI2023

Coated optical fiber and method of making same

A method is disclosed of making a coated optical fiber. The method may involve drawing a preform through a furnace to create a fiber having a desired diameter and cross sectional shape. The fiber is then drawn through a slurry, wherein the slurry includes elements including at least one of metallic elements, alloy elements or dielectric elements, and the slurry wets an outer surface of the fiber. As the fiber is drawn through the slurry, it is then drawn through a forming die to impart a wet coating having a desired thickness on an outer surface of the fiber. The wet fiber is then drawn through an oven or ovens configured to heat the wet coating sufficiently to produce a consolidated surface coating on the fiber as the fiber exits the oven or ovens.

Messerly, Michael↗
DOE OSTI2023

Effect of Measurement Temperature on Electrical Cable Frequency Domain Reflectometry Response

In nuclear power plants, electrical cables are exposed to stressors, such as elevated temperature and radiation. Evaluation of the effect of stressors on the lifetime of electrical cables can be conducted using offline electrical reflectometry techniques, such as frequency domain reflectometry (FDR). However, recent work has raised the concern that FDR measurements at temperatures higher than ambient may diminish or reduce the response due to stressors, potentially leading to incorrect predictions of electrical cable damage and lifetime. In this work, we explore the FDR response of an electrical cable exposed to an oven-based thermal stressor up to 140°C, including both ramping up and ramping down temperature. It was observed that, for both the oven entrance and exit, an increase in the FDR measurement temperature led to a decrease in the FDR reflection coefficient. In particular, it was found that the reflection coefficient at the oven entrance decreased from the ambient measurement by approximately 7%, 22%, and 36% at a temperature of 60°C, 100°C, and 140°C, respectively.

Spencer, Mychal P.↗
NASA NTRS1976

Viking GC/MS mechanisms design and performance

The Viking Lander gas chromatograph/mass spectrometer will analyze pyrolyzed samples of the Martian surface for organic content. The surface-sample loader and pyrolyzer assembly (SSPLA) is described, along with the major problems encountered during design and testing. Three mechanisms were developed to implement the required SSLPA functions: (1) a soil loader that forces soil from a filled rotating funnel into each of three ovens located on a carriage, (2) a Geneva drive for rotating and precisely indexing the ovens to receive sample, and (3) a toggle-clamp mechanism for sealing the ovens by forcing circular double knife edges into gold sealing surfaces.

Chase, C. P.↗
NASA NTRS1981

One-step microwave foaming and curing

Process that combines microwave foaming and curing of polyimide precursors in single step produces fire-resistant foam slabs of much larger volume than has previously been possible. By adding selected conductive fillers to powder precursors and by using high-power microwave oven, foam slabs with dimensions in excess of 61 by 61 by 7.6 cm are made. Typical foaming and curing and curing time is 35 minutes in microwave oven with additional 1 to 2 hour postcure in conventional oven.

Gagliani, J.↗
NASA NTRS1985

Equipment for Hot-to-serve Foods

Patented surface heating devices with a much faster air-to-solid heat transfer rate than previous air ovens were developed. The accelerated surface heating can brown, sear or crisp much more rapidly than in conventional ovens so that partially prepared food can be finished quickly and tastefully immediately before serving. The crisp, freshly browned surfaces result from the faster heat transfer which does not dry out the food. The devices are then compared to convection ovens and microwave heating processes.

Smith, D. P.↗
NASA NTRS2003

Determination of Significant Composite Processing Factors by Designed Experiment (MSFC Center Director's Discretionary Fund)

To determie composite material properties' effects from porcessing variables, a 3 factorial designed experiment with two replicates was conducted. The factors were cure method (oven versus autoclave), layup (hand versus tape-laying machine), and thickness (8 versus 52 ply). Four material systems were tested: AS4/3501-6, IM7/8551-7, IM7/F655 bismaleimide (BMI), and shear tests on IM7/F584. Material properties were G(sub 12), v(sub 12), E(sub 1c) and E(sub 2c). Since the samples were necessarily nonstandard, strengths, though recorded, cannot be considered valid. Void content was also compared. Autoclave curing helped material properties for the low modulus fiber material but showed little benefit for higher stiffness fibers. The number of plies was very important for epoxy composites but not for the BMI. E(sub 1) was generally unaffected by any factor. Particularly high void content did correlate to reduced properties. Autoclave curing reduced void content over oven curiing but a moderate amount of voids, less than 1 percent void content, didnot correlate with material properties. Oven cures and hand layups can produce high-quality parts. Part thickness of epoxy composites is important, though cure optimization may improve performance. Significant variations can be caused by processing and it is important that test coupons always reflect the layup and processes of the final part.

Finckenor, J. L.↗