Search NASA⌕ Search

SEARCH · Search NASA

Results for “heat flow calorimetry”

Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 19 records

Quantifying CTFE content in FK-800 using ATR-FTIR and time to peak crystallization

The chlorotrifluoroethylene (CTFE) content in vinylidene fluoride (VDF)-CTFE copolymers greatly influences the chemical and physical properties and ultimately determines the application. The copolymer known as FK-800 has a VDF:CTFE ratio of ~1:3 and is used almost exclusively as the binder in the insensitive high explosive (HE) formulation PBX 9502. Due to the dangerous nature of HE work and the effect CTFE content variations have, the ability to quickly and easily quantify CTFE content is of interest. Two techniques, attenuated total reflectance-Fourier transform infrared spectroscopy (ATR-FTIR) and time to peak crystallization measured by heat flow calorimetry, were evaluated here as potential means for quantifying CTFE content. Based on the certificate of analyses (COAs), FK-800 lots with varied CTFE content encompassing the range historically used in HE applications were used as standards for both methodologies. For FTIR, a linear regression was performed on the peak area of the C-Cl IR stretch and the CTFE content; the methodology was then demonstrated on four samples, two lots of unadulterated material and material recovered from two HE samples. The calculated CTFE content and COAs were in good agreement for all four samples. Heat flow calorimetry revealed the relationship between time to peak crystallization and CTFE content was best fit by a power regression; the methodology was then tested on two different FK-800 lots. Only one sample showed good agreement between the calculated CTFE content and the COA. This discrepancy indicates the method developed is not suitable for quantifying CTFE, but provides valuable insight regarding the crystallization behavior of VDF-CTFE copolymers.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Impact of KOH on the interfacial precipitation rates of C-S-H during the early hydration of C3S

In this work we investigated the influence of alkalis on the hydration of two triclinic samples of C{sub 3}S. One pure C{sub 3}S and one Al-doped C{sub 3}S (0.5 wt.‐% Al{sub 2}O{sub 3}). We added differently concentrated KOH solutions representing alkalis in the pore solution, which lead to an increase of the interfacial precipitation rates of C-S-H during the hydration of C{sub 3}S compared to the hydration without KOH. Isothermal calorimetry was conducted for the determination of the rates of reaction during the hydration process and ICP-OES measurements for the determination of the pore solution composition at certain times of hydration. The increasing effect of KOH solution on the calculated interfacial precipitation rates from pore solution data can explain the enhancement of the rates of reaction recorded by heat flow calorimetry during the early hydration. Therefore, the interfacial precipitation rates of C-S-H can accurately describe the acceleration effect of alkalis on the early hydration of C{sub 3}S.

36 MATERIALS SCIENCE↗

Evaluation of HAN-TEAN Stabilizers using Microcalorimetry

HAN-TEAN (hydroxylammonium nitrate - triethanolammonium nitrate - in water) is being considered for various propellant applications. This propellant has advantages in terms of insensitivity to impact and fire, low vapor pressure and environmentally benign reaction products. One office concerns with HAN-TEAN is its stability and shelf-life, especially when contaminated with trace metals. Stabilizer systems, consisting of anti-oxidants and/or chealating agents were investigated for their ability to control the decomposition of HAN-TEAN. Isothermal microcalorimetry, an ultrasensitive heat measurement technique, was used to monitor the decomposition of HANTEAN at near ambient temperatures. Isothermal microcalorimetry measures the heat flow from a reaction vessel into a surrounding heat sink. Microcalorimetry is approximately 1,000 times more sensitive than accelerating rate calorimetry (ARC) or differential scanning calorimetry (DSC) for measuring heat flow. Samples of HAN-TEAN containing the stabilizers were spiked with 50 ppm iron and the heat evolution monitored for a period of at least 30 days. Ten stabilizer combinations were tested and the rates of HAN-TEAN decomposition were lowered by 74 to 95 percent in the presence of iron.

Hornung, Steven D.↗

Thermal property characterization of phase change materials in building applications: A systematic review of fundamentals, recent progress, and future directions

Phase change materials (PCMs) can reduce building peak loads and enable demand-responsive thermal energy storage (TES), but their deployment depends on reliable measurement and interpretation of thermal properties across laboratory, intermediate, and application scales. Here, this review systematically examines characterization methods, testing protocols, and recent advances for neat PCMs and PCM composites, emphasizing thermal conductivity, enthalpy-related properties (phase change temperature, latent heat, specific heat), and cycling stability. For thermal conductivity, we compare steady-state and transient techniques and note limitations when phase transition and contact resistance affect measurements. For enthalpy–temperature characterization, we discuss differential scanning calorimetry together with intermediate- and bulk-scale methods, including T-history, heat flow meter testing, and three-layer calorimetry (3LC), to generate application-relevant enthalpy–temperature profiles. Cycling stability is organized into four experimental families: thermoelectric–air, fully thermoelectric, water-bath, and in situ chamber approaches, with attention to separating reversible supercooling from true degradation such as phase segregation. We highlight emerging noncontact diagnostics, including infrared thermography and embedded sensing, for spatially resolved validation and multiscale interpretation. Finally, we review the growing use of AI and machine learning for property prediction, inverse characterization from experimental signals, and real-time state estimation in building-integrated TES. Key needs include harmonized protocols, interlaboratory benchmarking, uncertainty reporting, and metadata-rich datasets to accelerate reproducible PCM qualification for grid-flexible buildings.

AI↗

Calorimetry of 25 Ah lithium/thionyl chloride cells

Heat flow measurements of 25-Ah lithium thionyl chloride cells provided a method to calculate an effective thermal potential, E(TP) of 3.907 V. The calculation is useful to determine specific heat generation of this cell chemistry and design. The E(TP) value includes heat generation by electrochemical cell reactions, competitive chemical reactions, and resistance heating at the tabs, connectors, and leads. Heat flow was measured while applying electrical loads to the cell in an isothermal calorimeter set at 0, 20, and 60 C.

Johnson, C. J.↗

Characterization of Thermal Protection Systems: An Analysis of Optical & Thermal Properties

Thermal Protection System Materials & thermal control coatings were characterized by a variety of methodologies including heat flow meter method (HFM), dynamic scanning calorimetry (DSC), fourier transform infrared spectroscopy (FTIR), and Ultra-Violet & Visible light spectroscopy (UV-VIS). Physical properties were measured to aid in the construction of thermal response models for a number a projects including MEDLI and MEDLI2. Comparing pre-flight predictions with actual flight data can allow for a reduction of margins and improve designs. The models enable design of TPS for flight missions and analysis of flight data to understand aerothermal environments experienced on the mission. This presentation reveals critical information: heat capacity (cp vs T), thermal conductivity ( vs T), and emissivity (E vs T) for Super Lightweight Ablative (SLA), Phenolic Impregnated Carbon Ablative (PICA-D), & Heatshield for Extreme Entry Environment Technology (HEEET). These properties were also measured for various thermal control coatings manufactured by AZ Technology. A portion of this work is incomplete and highlights questions to investigate in the future.

Cole, Brian↗

Below Ambient and Cryogenic Thermal Testing

Methods and apparatus for the testing of below-ambient temperature thermal insulation systems have been developed based on boiloff calorimetry. Boiloff calorimetry provides a direct measure of heat flow for below-ambient temperature conditions. The effective thermal conductivity (ke) and heat flux (q) of a test specimen are calculated for a fixed environmental condition (warm boundary temperature; cold boundary temperature; ambient or vacuum pressure). Through its heat of vaporization, liquid nitrogen (LN2) serves as the energy meter. Different apparatus have been built for flat-plate, cylindrical, and pipeline test specimens. Boundary temperatures can range from 353 K down to 77 K (80 C to -196 C). By interposing different insulation layers on the cold boundary, the cryogenic boiloff method is suitable for a wide range of below-ambient temperature applications. A cylindrical apparatus, Cryostat-100, as well as the pipeline test apparatus, Cryostat-P100, are thermally guarded and directly measure absolute thermal performance in watts. Pipe insulation systems can be mechanical, double-walled, or vacuum-jacketed including materials such as foams, cellular glass, aerogel blankets, clam-shell panels, and multilayer insulation. Two test pipelines, 12-meter-long, are mounted between two cold box assemblies. The test pipeline diameter is from 25-mm to 76-mm while the maximum outside diameter including insulation is up to 204-mm. The cold pipe tester design and test methods are discussed, as well as results for select thermal insulation materials. Progress toward a comparative type, bench-top cold pipe tester (Cryostat-P200) is also discussed.

Fesmire, James E.↗

A flow calorimeter for determining combustion efficiency from residual enthalpy of exhaust gases

A flow calorimeter for determining the combustion efficiency of turbojet and ram-jet combustors from measurement of the residual enthalpy of combustion of the exhaust gas is described. Briefly, the calorimeter catalytically oxidizes the combustible constituents of exhaust-gas samples, and the resultant temperature rise is measured. This temperature rise is related to the residual enthalpy of combustion of the sample by previous calibration of the calorimeter. Combustion efficiency can be calculated from a knowledge of the residual enthalpy of the exhaust gas and the combustor input enthalpy. An accuracy of +-0.2 Btu per cubic foot was obtained with prepared fuel-air mixtures, and the combustion efficiencies of single turbojet combustors measured by both the flow-calorimeter and heat-balance methods compared within 3 percentage units. Flow calorimetry appears to be a suitable method for determining combustion efficiencies at high combustor temperatures where ordinary thermocouples cannot be used. The method is fundamentally more accurate than heat-balance methods at high combustion efficiencies and can be used to verify near-100-percent efficiency data.

Evans, Albert↗

Use of calorimetry for end of charge determination

To perform heat flow measurements on batteries, it is necessary to consider the following requirements: establish thermal neutral potential; identify inefficient charging; understand self discharge mechanisms; and provide accurate voltage/temperature data. A discussion is provided in viewgraph format.

Johnson, Chris J.↗

Investigating the Thermal Behavior of Polymers by Modulated Differential Scanning Calorimetry (MDSC) – A Review

Modulated Differential Scanning Calorimetry (MDSC) is a thermoanalytical technique that detects changes in intrinsic heat flow by subjecting a material to two simultaneous heating rates, one linear and one sinusoidal. In this way, MDSC overcomes the limitations of its predecessor- conventional DSC-allowing for complex and overlapping thermal transitions to be resolved without sacrificing sensitivity. The advantages of MDSC lend credence to its extensive use in applications that require superior analytical accuracy, such as the food and drug industries.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Quantifying Uncertainties in Heat Capacity Measurements of Molten Salts Determined Using Differential Scanning Calorimetry

Uncertainty in specific heat capacity values of a molten salt determined by using differential scanning calorimetry (DSC) was assessed based on the precision of replicate measurements of heat flows used in the calculation and effects of corrections that are commonly made to heat flow measurements. The ratio method of determining heat capacity was applied using the results of replicate heat flow measurements made with two empty cells, a sapphire reference material, and three samples of a doped NaCl-UCl 3 salt mixture. Replicate measurements with empty cells were used to quantify the effects of system instabilities and sensitivities on the measured heat flows of sapphire and salt. The combined effects of uncertainties in individual heat flow measurements made with blank cells using this system were quantified to be 2.6 μV based on isothermal holds before and after the scan, with cell placement adding the greatest uncertainty. This value was used as the tolerance for accepting background-corrected heat flows measured with sapphire and salt to calculate the specific heat capacity. The acceptable heat flows measured for sapphire and salt over the temperature range of 540 to 725 °C resulted in calculated specific heat capacity values ranging from 0.53 to 0.91 J g −1 K −1 with an overall average value of 0.70 J g −1 K −1 and an uncertainty of 0.22 J g −1 K −1 at the 99 % confidence level. The combined uncertainty in the specific heat capacity masked detection of any effect of temperature or salt composition that occurred.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗