Results for “single entity” — Page 7

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 NTRS2014

ADEPT for Secondary Payloads

Deployable entry vehicles provide an enabling capability for large payloads at destinations across the solar system. The primary advantage of such systems derives from the fundamental limitation of available launch vehicle shroads preventing tried-and-true rigid aeroshell technology from being applied. However, little mission-pull exists for deployable entry vehicle technology for missions where the entry vehicle is the primary payload and can fit within available shrouds. The propensity toward applying rigid aeroshell technology is logical given that deployable concepts are higher risk and provide no marginal scientific benefit for missions where a rigid aeroshell is an option. A movement toward flying smaller spacecraft has emerged in recent years and is revealing novel applications for deployable entry vehicles as secondary payloads. Secondary payloads must minimize interference with the primary payload in order to ease accomodation. Advancements in small spacecraft technology have caught the attention of government entities who are now recognizing the high value proposition of small spacecraft for frequent, incremental technology development and science return rather than the traditional high cost and infrequent big-bang approaches. Worldwide, well over 200 small satellites (mass < 180 kg) have launched in recent years for such purposes as eduation, technology development, science, commerce, and defense. The Adaptable Deployable Entry and Placement Technology (ADEPT), a mechanically-deployable entry vehicle technology, has been under development at NASA since 2011. An Ames Center Innovation Fund (CIF) proposal was recently awarded to study ADEPT for EDL of small payloads. The unique capability of ADEPT for small science payloads comes from its ability to stow within a slender volume and deploy passively to achieve a mass-efficient drag surface with a high heat rate capability. The low ballistic coefficient results in entry heating and mechanical loads that can be met by a revolutionary three-dimensionally woven carbon fabric supported with rib structures. This carbon fabric has test-proven capability as both primary structure and payload thermal protection. This presentation will inform the EDL community of the capability of ADEPT for delivery of small secondary payloads as well as provide status of on-going technology development activities. Results of a mission applications study for secondary payloads to Mars and Venus will be presented. A primary goal of these mission design activities is to integrate high-value verification approaches wherever possible. For example, for some mission applications it is possible to test in NASA arc jet facilities at full-scale. This enables endto- end thermostructural requirement verification with a single test. Another important challenge that needs to be solved is the reliability of the decelerator to achieve the desired shape using simple passive mechanical actuators (such as springs) that do not require power from the primary payload for deployment. A configuration of ADEPT is being prototyped and used to evaluate the functionality and reliability of the deployment mechanism through bench-top testing. The prototype will then be tested in a low speed wind tunnel in late 2014 to evaluate aerodynamic load-carrying capability and deflected shape. Results of the deployment testing and status of wind tunnel test plans will be discussed.

Smith, B.↗