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At least 19 records

ASRM test report: Autoclave cure process development

ASRM insulated segments will be autoclave cured following insulation pre-form installation and strip wind operations. Following competitive bidding, Aerojet ASRM Division (AAD) Purchase Order 100142 was awarded to American Fuel Cell and Coated Fabrics Company, Inc. (Amfuel), Magnolia, AR, for subcontracted insulation autoclave cure process development. Autoclave cure process development test requirements were included in Task 3 of TM05514, Manufacturing Process Development Specification for Integrated Insulation Characterization and Stripwind Process Development. The test objective was to establish autoclave cure process parameters for ASRM insulated segments. Six tasks were completed to: (1) evaluate cure parameters that control acceptable vulcanization of ASRM Kevlar-filled EPDM insulation material; (2) identify first and second order impact parameters on the autoclave cure process; and (3) evaluate insulation material flow-out characteristics to support pre-form configuration design.

Nachbar, D. L.↗

Composite Cure Process Modeling and Simulations using COMPRO(Registered Trademark) and Validation of Residual Strains using Fiber Optics Sensors

Composite cure process induced residual strains and warping deformations in composite components present significant challenges in the manufacturing of advanced composite structure. As a part of the Manufacturing Process and Simulation initiative of the NASA Advanced Composite Project (ACP), research is being conducted on the composite cure process by developing an understanding of the fundamental mechanisms by which the process induced factors influence the residual responses. In this regard, analytical studies have been conducted on the cure process modeling of composite structural parts with varied physical, thermal, and resin flow process characteristics. The cure process simulation results were analyzed to interpret the cure response predictions based on the underlying physics incorporated into the modeling tool. In the cure-kinetic analysis, the model predictions on the degree of cure, resin viscosity and modulus were interpreted with reference to the temperature distribution in the composite panel part and tool setup during autoclave or hot-press curing cycles. In the fiber-bed compaction simulation, the pore pressure and resin flow velocity in the porous media models, and the compaction strain responses under applied pressure were studied to interpret the fiber volume fraction distribution predictions. In the structural simulation, the effect of temperature on the resin and ply modulus, and thermal coefficient changes during curing on predicted mechanical strains and chemical cure shrinkage strains were studied to understand the residual strains and stress response predictions. In addition to computational analysis, experimental studies were conducted to measure strains during the curing of laminated panels by means of optical fiber Bragg grating sensors (FBGs) embedded in the resin impregnated panels. The residual strain measurements from laboratory tests were then compared with the analytical model predictions. The paper describes the cure process procedures and residual strain predications, and discusses pertinent experimental results from the validation studies.

Sreekantamurthy, Thammaiah↗

Dynamic dielectric analysis - A nondestructive cure process monitoring method

The cure processes of TGDDM-based epoxy thermosets and polysulfone thermoplastic resins were monitored by means of computer-controlled dynamic dielectric measurements made at frequencies 5 Hz to 5 million Hz. The values of capacitance and conductance were recorded, and the data were used to calculate the complex permittivity, an intensive property which is characteristic of the material's state of cure and independent of the amount of material measured. The frequency dependence of the complex permittivity value was used to determine the conductivity and mean relaxation time. The conductivity which is also an intensive variable and is independent of sample size, was correlated with the viscosity in both the epoxy and polysulfone systems.

Kranbuehl, D. E.↗

Method of controlling a resin curing process

An analytical technique for controlling the curing process of fiber-reinforced composite materials that are formed using thermosetting resins. The technique is the percent gel method and involves development of a time-to-gel equation as s function of temperature. From this equation a rate-of-gel equation is then determined, and a percent gel is calculated which is the product of the rate-of-gel times time. Percent gel accounting is used to control the proper pressure application point in an autoclave cure process to achieve desired properties in a production composite part.

Charles Neal Webster↗

Development of a Fully Automated Guided Wave System for In-Process Cure Monitoring of CFRP Composite Laminates

A guided wave-based in-process cure monitoring technique for carbon fiber reinforced polymer (CFRP) composites was investigated at NASA Langley Research Center. A key cure transition point (vitrification) was identified and the degree of cure was monitored using metrics such as amplitude and time of arrival (TOA) of guided waves. Using an automated system preliminarily developed in this work, high-temperature piezoelectric transducers were utilized to interrogate a twenty-four ply unidirectional composite panel fabricated from Hexcel (Registered Trademark) IM7/8552 prepreg during cure. It was shown that the amplitude of the guided wave increased sharply around vitrification and the TOA curve possessed an inverse relationship with degree of cure. The work is a first step in demonstrating the feasibility of transitioning the technique to perform in-process cure monitoring in an autoclave, defect detection during cure, and ultimately a closed-loop process control to maximize composite part quality and consistency.

Hudson, Tyler B.↗

Modeling the curing process of thick-section autoclave cured composites

Temperature gradients are significant during cure of large area, thick-section composites. Such temperature gradients result in nonuniformly cured parts with high void contents, poor ply compaction, and variations in the fiber/resin distribution. A model was developed to determine the temperature distribution in thick-section autoclave cured composites. Using the model, long with temperature measurements obtained from the thick-section composites, the effects of various processing parameters on the thermal response of the composites were examined. A one-dimensional heat transfer model was constructed for the composite-tool assembly. The governing differential equations and associated boundary conditions describing one-dimensional unsteady heat-conduction in the composite, tool plate, and pressure plate are given. Solution of the thermal model was obtained using an implicit finite difference technique.

Loos, A. C.↗

Modeling the curing process of thermosetting resin matrix composites

A model is presented for simulating the curing process of a thermosetting resin matrix composite. The model relates the cure temperature, the cure pressure, and the properties of the prepreg to the thermal, chemical, and rheological processes occurring in the composite during cure. The results calculated with the computer code developed on the basis of the model were compared with the experimental data obtained from autoclave-curved composite laminates. Good agreement between the two sets of results was obtained.

Loos, A. C.↗

Detection of trace quantities of dimethylacetamide during the curing process of a polyimide film

An experimental study of positive ion clustering of dimethylacetamide (DMAC) with water molecules using high pressure mass spectrometry techniques is reported. The possibilities of using these techniques to determine the concentration levels of DMAC evolved from a polyimide film during the curing process, are examined. The test sample of gas contained DMAC of the order of a few micrograms, water, nitrogen, oxygen, and other compounds that might evolve during the curing cycle of a polyimide film. It is found that PPM concentrations such as DMAC lost from polyimide during curing stages can be detected with this technique. Improvement of the detection of lower concentrations (50 picograms) can be made by using electron multipliers with a gain in the 10 to the 8th power range and pulse counting techniques.

Smith, A. C.↗

Mechanism and kinetics of the curing process in a resin system

The present investigation is concerned with the development of a cure reactivity model for a resin system consisting of tetraglycidyl diaminodiphenyl methane (TGDDM) and diaminodiphenyl sulfone (DDS), taking into account the temperature range from 153 to 177 C. Differential scanning calorimetry and FT-IR spectroscopy have been used to investigate the cure kinetics of the resin with the objective to obtain a correlation between the total conversion and the rates of formation and disappearance of specific functionalities. It was found that the overall process can be satisfactorily described in terms of two first order processes.

Moacanin, J.↗

Addition polymers from 1,4,5,8-tetrahydro-1,4;5,8-diepoxyanthracene and Bis-dienes. 2: Evidence for thermal dehydration occurring in the cure process

Diels-Alder cycloaddition copolymers from 1,4,5,8-tetrahydro-1,4;5,8-diepoxyanthracene and anthracene end-capped polyimide oligomers appear, by thermogravimetric analysis (TGA), to undergo dehydration at elevated temperatures. This would produce thermally stable pentiptycene units along the polymer backbone, and render the polymers incapable of unzipping through a retro-Diels-Alder pathway. High resolution solid 13C nuclear magnetic resonance (NMR) of one formulation of the polymer system before and after heating at elevated temperatures, shows this to indeed be the case. NMR spectra of solid samples of the polymer before and after heating correlated well with those of the parent pentiptycene model compound before and after acid-catalyzed dehydration. Isothermal gravimetric analyses and viscosities of the polymer before and after heat treatment support dehydration as a mechanism for the cure reaction.

Meador, Mary Ann B.↗

Characterization of the relationship of the cure cycle chemistry to cure cycle processing properties

Dynamic Dielectric measurements made over a wide range of frequency provide a sensitive and convenient means for monitoring the cure process in thermosets and thermoplastics. The measurement of dielectric relaxation is one of only a few instrumental techniques available for studying molecular properties in both the liquid and solid states. Furthermore, it is probably the only convenient experimental technique for studying the polymerization process of going from a monomeric liquid of varying viscosity to a crosslinked, insoluble, high temperature solid. The objective of the research is to develop on-line dielectric instrumentation for quantitative nondestructive material evaluation and closed loop smart cure cycle control. The key is to relate the chemistry of the cure cycle process to the dielectric properties of the polymer system by correlating the time, temperature, and frequency dependent dielectric measurements with chemical characterization measurements. Measurement of the wide variation in magnitude of the complex permittivity with both frequency and state of cure, coupled with chemical characterization work, have been shown in the laboratory to have the potential to determine: resin quality, composition and age; cure cycle window boundaries; onset of flow and point of maximum flow; extent of and completion of reaction; evolution of volatiles; T sub g; and, crosslinking and molecular weight buildup.

Kranbuehl, D. E.↗

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.↗

High-Temperature Graphite/Phenolic Composite

Graphite-fiber/phenolic-resin composite material retains relatively high strength and modulus of elasticity at temperatures as high as 1,000 degrees F. Costs only 5 to 20 percent as much as refractory materials. Fabrication composite includes curing process in which application of full autoclave pressure delayed until after phenolic resin gels. Curing process allows moisture to escape, so when composite subsequently heated in service, much less expansion of absorbed moisture and much less tendency toward delamination. Developed for nose cone of external fuel tank of Space Shuttle. Other potential aerospace applications for material include leading edges, parts of nozzles, parts of aircraft engines, and heat shields. Terrestrial and aerospace applications include structural firewalls and secondary structures in aircraft, spacecraft, and ships. Modified curing process adapted to composites of phenolic with other fiber reinforcements like glass or quartz. Useful as high-temperature circuit boards and electrical insulators.

Seal, Ellis C.↗

Dynamic dielectric analysis - A means for process control

The development of dynamic dielectric analysis techniques (as a 'smart' sensor for quantitative NDE) and of intelligent closed-loop cure systems is reported. The cure process of both BF3:R-catalyzed and uncatalyzed tetraglycidyl-4,4'-diaminodiphenyl methane (TGDDM)/diamine epoxy resins was studied. Measurements were made over a frequency range of six decades. The resin was monitored continuously throughout the cure process as it changed from a viscous liquid to a highly crosslinked solid. From the frequency dependence of the dielectric loss, the specific conductivity has been determined and shown to directly monitor the viscosity before the gel point is reached. Dielectric master plots of the cure process, analogous to time-temperature superposition plots for rheological data, have been developed.

Kranbuehl, D.↗

Characterization of the relationship of the cure cycle chemistry to cure cycle processing properties

Dynamic dielectric analysis (DDA) is used to study curing polymer systems and thermoplastics. Measurements are made over a frequency range of six decades. This wide range of frequencies increases the amount of information which can be obtained. The data is analyzed in terms of the frequency dependence of the complex permittivity epsilon sup *, specific conductivity sigma (ohm/cm) and the relaxation time tau, parameters which are characteristic of the cure state of the material and independent of the size of the sample.

Kranbuehl, D. E.↗

Characterization of and sensor-model verification and control of the properties of PMR-13 during processing

This study presents an in situ sensor and a process-simulation model developed for monitoring and controlling the cure process of PMR-15. The time-temperature dependence of the buildup in the molecular network structure, extent of reaction, viscosity, flow, and consolidation during the cure of PMR-15 are discussed. The relationship of the time-temperature cycle used during imidization to the length of the endcapped chains formed is examined. The relationship of the time-temperature cure-processing cycle to the reaction kinetics, viscosity, flow, and consolidation during crosslinking is analyzed using frequency-dependent electromagnetic sensors and the Loos processing model. Application of the FDEMS sensing technique and the process-simulation model for quality assurance processing and automated on-line control of cure is discussed.

Kranbuehl, D.↗