AIAA 2002-1372 Shape Memory Composite Development for Use in Gossamer Space Inflatable Structures David P. Cadogan, Stephen E. Scarborough, John K. Lin, George H. Sapna III ILC Dover, Inc. Frederica, DE 43rd AIAA/ASME/ASCE/AHS/ASC Structures, Structural Dynamics, and Materials Conference & Exhibit AIAA Gossamer Spacecraft Forum April 22-25, 2002 / Denver, CO For permission to copy or republish, contact the copyright owner named on the first page. For AIAA-held copyright, write to AIAA Permissions Department, 1801 Alexander Bell Drive, Suite 500, Reston, VA 20191-4344 2002-1372 SHAPE MEMORY COMPOSITE DEVELOPMENT FOR USE IN GOSSAMER SPACE INFLATABLE STRUCTURES David P. Cadogan*, Stephen E. Scarborough, John K. Lin, George H. Sapna III ILC Dover, Inc. Frederica, DE inflate the structure numerous times on the ground for testing prior to launch, and deployment in space. The materials are initially consolidated at a highly elevated temperature (Ts) to set the material’s geometric shape. This is the shape the structure will naturally return to when heated above its glass transition temperature (Tg) in subsequent heating events. The material is heated above its Tg, but not above its set temperature (Ts), to soften it for packing into small volumes. The packed structure is heated above its Tg prior to deployment in space (or during ground operations), to make it flexible enough to be deployed by inflation. The shape restoration stress Figure 1. ILC Dover SMP Inflatable memory of the composite is a Space Frame 3,4,10 weak function relative to the (Patent Pending) stress realized from 1,2,7 inflation. Stress is required for component deployment, control, and tensioning the wall for optimal shape accuracy. Therefore, the shape memory function is utilized as a microscopic shape restoration feature in most applications. The shape memory function also allows the fabrication of structures that consist of small diameter tubes where it would be inefficient to inflate all elements individually (Figure 1). The individual tubes return to shape by the shape memory of the resin, while an outer polymeric film shell is inflated to deploy the structure.3,4 ABSTRACT Several new shape memory composite materials have been developed that allow the requirements of gossamer space structures (high packing efficiency, low mass, high stiffness, etc.) to be met. A detailed analysis and test program has been conducted on several different materials at the coupon level, as well as at the component level in the form of inflatable deployable columns. Materials have been tested to determine their degradation from folding and packaging, storage life and aging characteristics, vacuum stability, outgassing characteristics, and ability to return to shape when heated after packing. Shape memory composites have also been tested at the sub-component and system level in several applications. Isogrid beam columns have been designed, manufactured, and structurally tested to verify materials performance parameters. The columns were repeatedly packed and deployed to assess the degradation of the materials in actual use and the resultant strength and stiffness loss. Compression, and torsion strength and stiffness were assessed in the test program. INTRODUCTION One of the most important components of the gossamer inflatable structure is the material of which it is composed. A leading candidate among the field of potential materials is shape memory composite material. The shape memory composite consists of a fibrous reinforcement, such as carbon, and a polymeric matrix resin such as polyurethane or epoxy. The matrix resin component provides the shape memory behavior to the composite. The reinforcement can be utilized in several forms such as individual tow elements or fabrics of various weave styles. The fibers are coated with the resin and formed into various structural shapes. Geometric shapes such as monocoque, isogrid, and IsoTruss™ columns can be manufactured from a shape memory composite material. This paper will examine system requirements for rigidizable materials, performance characteristics of several shape memory materials, and relevant test data. Most of the data presented herein is from an isogrid Shape memory composite materials utilize a reversible heating process to provide the ability to collapse and re* [email protected] – Associate Fellow AIAA “Copyright 2002 by ILC Dover, Inc. Published by the American Institute of Aeronautics and Astronautics, Inc., with permission.” IsoTruss is a registered Trademark of Brigham Young University and is licensed to ILC Dover for space applications. 1 American Institute of Aeronautics and Astronautics development program under the Inflatable Solar Array Experiment (ISAE-II) program. bundles (tows) during the packing of a completed structure. When the tows are folded 180o for packing, the fibers on the inside of the bend radius will be in compression, while the fibers towards the outside of the bend will be in tension. To minimize structural damage in a tightly packed structure, the fibers must either be able to move, which is a function of the resin, or they must be able to withstand high strain rates, a function of both the resin and the fiber. IM9 carbon fiber was selected for further study because of its high modulus, high strength, and high strain capability. MATERIAL REQUIREMENTS ILC generated an in-depth requirement list for the development of potential rigidizable materials. Using these requirements, ILC has developed a battery of tests that are conducted in series. This provides a “gated” approach to the development of advanced materials, one that screens out materials efficiently and reduces development cost. The driving requirements are identified as: Ø Ø Ø Ø Ø Table 1. Select Carbon Fiber Properties1 Brand & Type o Tight Packing Without Damage (180 Folds) Low Outgassing (<1.0% TML, <0.1% CVCM) Long Shelf Life (3+ years) Near Zero CTE Low Transient Deformation (Creep) Tensile Tensile Tensile Modulus Strength Strain (%) (MPa) (GPa) Density Avail. Tow 3 (g/cm ) Counts Hexcel IM9 Hexcel IM7(6000 spec) Besfight IM600 304 292 6120 5760 2 2 1.8 1.79 12K 12K 285 5790 2 1.8 A detailed selection process, covering all system requirements, is conducted for candidate resins and additional tests are performed to characterize the best materials with respect to the following requirements: Hexcel IM6 Hexcel AS4D Grafil Pyrofil MR50 Hexcel IM7 Hexcel AS4C 279 241 290 276 231 5510 4550 5400 5080 4205 2 1.9 1.8 1.8 1.8 1.76 1.79 1.8 1.78 1.78 • BP Amoco Thornel T650/35 255 4280 1.7 1.77 6K,12K, 24K 12K 12K 12k 6K 3K,6K, 12K 3K, 6K, 12K BP Amoco Thornel T300 Grafil Pyrofil MS40 Besfight UM46 Besfight UM68 231 3750 1.4 1.76 345 435 650 4610 4705 3330 1.3 1.1 0.5 1.77 1.82 1.97 • • • • Radiation Resistance (10 yr. life LEO/GEO) Mechanical Properties Thermal Conductivity Water Absorption Thermal Cycling Resistance 1K, 3K, 6K, 12K 12K 12K 12K RESIN SELECTION AND DEVELOPMENT Several candidate resins were identified from ILC internal research and development started in 1996, commercially available sources, and through ILC sponsored work at the University of Delaware Center for Composite Materials. Material properties for each of the candidate resins were gathered for comparison (Table 2). Data was gathered from available material data sheets, through rule of mixtures analysis, or through testing. Assumptions made about properties at the early stages of materials development were deemed acceptable to reduce the overall quantity of testing that was to be performed. These values were used to make general trades and identify the candidate materials that were later put through a complete battery of tests. FIBER SELECTION The selection of fibers used in constructing a rigidizable inflatable gossamer structure is driven primarily by specific stiffness, strain to failure (to allow folding without damage), environmental resistance, thermal conductivity, and coefficient of thermal expansion (CTE). CTE is very important in developing a structure that will not suffer shape changes from variable thermal inputs. Four fiber types are acceptable from this standpoint: carbon, KevlarTM, PBO, and VectranTM. Of these, only carbon exhibits the thermal conductivity and environmental resistance desired, with a known interface capability to the resin types being investigated. Further study of the PBO and VectranTM reinforcements is warranted in the future. The individual resin candidates were also evaluated in a trade study to determine the top three candidate materials that would be fully characterized. Some relative composite properties were given for comparison. Weighting factors were applied to each requirement to highlight the importance of certain factors, such as those that would affect folding characteristics or vacuum stability. Several carbon fiber candidates were identified for comparison (Table 1). Factors that affected structural performance, as well as sizing and manufacturing, were evaluated. It was important to select a fiber with a sizing that was compatible with the resin candidates being considered. ILC considers tensile strain to be the most important fiber property for structures fabricated from shape memory polymer (SMP) resins. This is because of the high strains that will occur in the carbon filament 2 American Institute of Aeronautics and Astronautics Table 2. Candidate Resin Properties 5,6,8 ILC Designation Matrix 3 Density (g/cm ) Water absorption (after 24 h) Radiation resistance UV resistance Liquid @ room temperature Fiber Compatibility Tensile Strength @ Yield (MPa) Tensile Modulus (GPa) Modulus vs. Temp. Transition o Deflection Temperature ( C) o Melt Temperature Tm ( C) o CTE (ppm/ C) o o Specific Heat Cp (J/g C) (0 C-Tm) o Specific Heat Cp (J/g C) (Tm-Tf) Thermal cycling o Thermal conductivity (W/m C) Ability to return to shape Packing ability TP 264 Polyester 1.27 0.20% Poor Excellent No Good 53.1 TP275 Epoxy 1.14 0.70% Excellent Excellent Yes Excellent 62.0 2.21 Quick o 80 C o 81-91 C 70 2.76 Slow o 53 C N/A 51 2 2 Excellent 0.205 2.1 N/A Good 0.17-0.25 Very good Very Good Excellent Good TP405 Polyurethane 1.20 0.7% *after 72 h Good Good No Fair o 60.0 (Tg-20 C) o 30.0 (Tg+20 C) 1.0 Quick o 75 C o 190 C o 27.5 (Tg-20 C) o 217 (Tg+20 C) 1.7 + 1.7+ Excellent o 0.35 (Tg-20 C) 0.58 (Tg+20oC) Very good Very Good The results of the trade study indicated that the epoxybased system was the leading candidate, followed by the polyester and polyurethane materials. Out of these three resins, epoxies and polyurethanes were the only resins available as a liquid at room temperature. All of the other candidate resins would have to be heated above their melt temperatures for fiber impregnation. Because a wetwinding manufacturing technique provides the greatest flexibility to the processing parameters, epoxy and polyurethane resins become more attractive for use in development projects. Epoxy is also a good candidate for further study because it can be easily chemically modified. Polyurethane was also identified as a candidate that had a wide range of variables that could be adjusted to vary performance properties. Within 4-5 months, ILC developed several variants to the TP275 epoxy-based material in an attempt to advance the material’s performance. Each of these formulations is chemically unique and provides a wide range of performance capabilities. A summary of the material properties of each of the epoxy variants, including the leading polyurethane candidate (TP406) is shown in Table 3. Tg (oC) Laminate Folding Ability Shape Memory Pot life @ RT Tensile Strength (MPa) TP 406 TP 277 TP 279B Urethane Epoxy Epoxy 55 65 37 Excellent Excellent Very Good Yes Yes Yes <10 min <16 hrs <24 hrs 60.0 69.0* No Data Yes 48 hrs 62.0 1.0 3.1 No Data 2.76 Possibility of Tg increase over time Modulus vs. Temp. Transition Fiber Compatability Initial Mix Viscosity No Yes Yes Yes Quick Slow Slow Slow Fair Low Excellent Excellent Low Low TP230 Polyethylene 0.967 <0.01% Excellent Good No Good 30.5 1.34 Slow o 108 C o 157 C 68-105 1.34 Slow o 95 C o 165 C 68-105 1.0 Slow o 80 C o 133 C 108 2.1 2.7 Excellent 0.17-0.20 2.1 2.7 Excellent 0.17-0.20 2 2.7 Excellent 0.33 Good Very Good Fair Good Very Good Very Good FOLDING TEMPERATURE The folding temperature of the resin is an important parameter that has an impact on the overall spacecraft system design and also has a major impact on ground testing. The folding temperature is defined as the Tg of the resin, plus an added factor of safety, which is typically around 20oC. At these temperatures the resins exhibit a large decrease in stiffness (i.e. they become flexible). It would be ideal to use a resin in the structure that had a Tg that was far above the highest anticipated temperature of the spacecraft. However, since the resin must be heated above the Tg for deployment, a high Tg will require greater spacecraft power. Therefore, a balance between thermal loading and folding temperature must be achieved. It is also of importance to note that formulations with glass transition temperatures below ambient temperatures could be developed if low temperature rigidization is considered as an option for future applications. However this too will affect the ability of the completed structure to be ground tested because these types of materials will require cold chambers for testing. It will also affect the layers of MLI that will be required to maintain the temperature of the structure below its Tg. These additional layers of MLI will lead in increased system mass. TP 283E Epoxy 48 Excellent Tensile Modulus (GPa) TP 221 Polypropylene 0.90 <0.01%-0.03% Fair Good No Good 31.7 The epoxy formulation that shows the greatest overall performance is TP283E. This resin demonstrated a particularly high degree of folding performance and good shape memory. This work greatly advanced the state of the art of SMP resin technology for use in gossamer structures. Further advancement of these resins is ongoing at ILC to improve performance properties and enhance manufacturing characteristics. Table 3. Enhanced Resin Properties1 Property TP220 Polypropylene 0.90 <0.01%-0.03% Fair Good No Good 35.2 Excellent High 3 American Institute of Aeronautics and Astronautics Another area where the folding temperature is significant is in ground handling. The fact that the structure will be packed in a factory ambient environment causes some potential difficulties for structures made with SMP composites. The presence of an atmosphere around the structure will create large convective losses and eliminate the performance benefit of a MLI blanket. Therefore, large amounts of power are required for ground heating of the structures which often necessitate the need for special heating and handling equipment that is radically different than that which will be used in space. It is desirable to maintain a Tg as low as possible to minimize the delta in temperature during ground packing and testing to reduce the potential for structural damage due to premature cooling. Again, a balance in performance must be sought and specific ground handling equipment manufactured. 120 108 Tg (C) By DSC 100 95 80 Tg (C) 80 80 75 65 60 48 40 37 37 40 53 55 43 24 20 Ep ox TP y 28 3B Ep ox TP y 28 3C Ep ox TP y 28 3 A Ep ox TP y 28 3E Ep ox y TP 27 TP 5 Ep 40 ox 6 Po y lyu re tha ne TP 27 TP 7 Ep 40 5 ox Po y lyu re tha TP ne 26 4P TP oly es 23 ter 0P oly TP eth 22 yle 1P ne oly pr TP op 22 yle 0P ne oly pr op yle ne 27 9B TP TP 28 3F Ep ox y 0 ILC Resin Designation Figure 3. Tg of ILC Dover Resins COMPONENT FOLDING TESTS The most critical function of SMP/Carbon fiber composites is to fold without significant degradation in performance. If degradation does occur, it must be predictable and well understood. To this end, ILC developed a procedure for rapidly testing the material’s response to folding. This test was used to obtain first order qualitative test results to generalize folding response. The folding test also included an assessment of the material’s shape memory function, another important parameter in material function. The Tg of the resins studied was determined using Differential Scanning Calorimetry (DSC). The resins tested under ISAE-II exhibited glass transition temperatures from 24oC to 54oC. A sample DSC curve for the TP275 resin (ILC’s base SMP epoxy) can be seen in Figure 2. Resins with Tg’s of 43oC and below were not advanced because of the anticipated thermal environment. However, further testing was performed on resins such as TP279B because of the possibility of using them on future programs where resins with lower Tg’s may be required. In this test, a T300, 1K tow, tri-axial woven fabric (0.18 mm thick) was pre-impregnated with the various resins to a mass fraction of near 50% and consolidated into its finished composite form. This particular fabric was chosen because of its close resemblance to the isogrid beam design (i.e. open weave). In the test, the sample was heated well above its Tg (generally 120oC) and folded 180o over a 0.25mm thick aluminum sheet. Two gauge lines marked on the sample identified the fold line. The sample was then allowed to cool and solidify to its folded shape. At this point, the fold location was microscopically inspected to identify any fracturing to the fibers or resin. If successful, the sample was reheated in an oven to assess its shape memory function. Notations were made regarding the speed and accuracy of return. The process was then repeated multiple times, always folding along the same line, to gather information regarding fatigue resistance. The entire process is shown in Figure 4. Tg=53.06oC Figure 2. TP275 DSC Tg Analysis1 Most of the resins that were selected for advancement exhibited the ability to slightly modify their Tg. This ability was exercised in resin design such that the Tg values could be kept in a range close to the anticipated thermal challenge. Other ILC thermoplastic resins have glass transition temperatures in the range of 60-100oC, but at this time more intensive manufacturing processes would be required for their use because they are not available as liquids at room temperature. The Tg of ILC Dover’s current thermoplastic, polyurethane, and epoxy polymer materials are shown in Figure 3. Some samples were immediately destroyed when folded 180o. Other samples had the ability to be folded over this difficult bend radius, but when they returned to shape, they were extremely brittle at the fold line. Resin systems that achieved an excellent rating for foldability and displayed good shape memory function were advanced to the next level of testing, as tows. This test identified four resins that achieved an excellent rating (TP277, TP279B, 4 American Institute of Aeronautics and Astronautics Traditional composite structures generally have a Vf of 60%. In the case of the SMP/Carbon fiber composite, the results of these tests showed that the test samples and beams should have a Vf of 50% or less for folding. Also, tows sizes from 12K-48K were able to be folded 180o with little or no apparent visual damage. Generally, the only difference under the microscope between pristine and folded tows was a slight loss of sheen at the fold line. TP283E, and TP406). The shape memory effect appeared strongest in TP277 and TP406, while TP283E and TP406 were the most flexible resin systems above their respective Tg’s. Returned to Shape Inspection Repeat As Manufactured The second tow test, the tow tensile test, was devised to gather data on the structural performance of tows when challenged by individual factors that could degrade their performance, and these factors in combination. The factors included lab oven heat exposure, hard vacuum exposure, and folding cycles. The lab oven exposure was evaluated to determine the degradation of the composite when exposed to elevated temperatures that represented a pre-flight bake-out to reduce the volatile content of the system. The hard vacuum exposure was conducted in an ILC vacuum chamber and represented the exposure of the material to space prior to deployment (Figure 6). Thermal exposures were also conducted in the vacuum chamber to simulate the effects on the system from heating during deployment in space. Repeated folding trials were conducted that cycled the tow from a straight to 180o bent condition, for 10 and 20 cycles, to assess cycle fatigue effects. Tensile testing was selected for test simplicity and because it was an accurate Figure 6. ILC Thermal assessment of fiber Vacuum Chamber1 damage. After Folding Folded, Perpendicular to Fold - Inspection Figure 4. Laminate Folding Test Procedure1 ILC developed two tow related tests for further screening resin candidates in a form closer to the isogrid elements, and to obtain design data to use in the design of isogrid booms. One was centered on microscopically studying tow folding, and the other focused on studying the environmental and packing effects more closely associated with the tow elements. The tow-folding test was developed to provide more advanced screening data for resin selection. This test was also used to evaluate the performance of various tow sizes (12K, 24K, 36K, and 48K) to determine if tow size had a significant effect on degradation with folding. This was determined to be important in developing a scalable isogrid or IsoTrussTM structure. The purpose of these tow tests was to assess the damage that may be caused during packing. The test procedure was identical to the Figure 5. 24K TP277 Tow Folded 180o 1 laminate folding test procedure. Figure 5 shows the results of one test. ILC Dover mechanically characterized shape memory thermoplastics in a specific configuration that was consistent with the manufacture of isogrid booms. Prior to testing the tow samples, each one was measured using dial calipers to determine its diameter. This value was then used in the calculation of the tensile modulus for each tow. Four different tow sizes were considered: 12k, 24k, 36k, and 48k. Five data points were taken for each test (5 samples per test type) to develop some statistical significance. A total of 275 individual samples were tested in this effort. Data from the test was used to determine degradation factors for use in analytical models and to help correlate boom test data from the as manufactured state to the after packed & deployed state. ILC considered the worst case heating scenario to be eight hours at 125oC. This represents the maximum time and temperature that the The samples that were tested had fiber volume fractions (Vf) of 41-60%. It was found that the samples that had lower fiber volume fractions were more flexible and less likely to sustain serious fiber damage than samples with higher fiber volume fractions. For this reason, the tows used in actual isogrid manufacturing were purposely coated with more resin than typical composites. 5 American Institute of Aeronautics and Astronautics that vacuum alone for 8 hours at room temperature degrades the material (25.6% decrease in peak load). In the case of the TP277 resin, some epoxy is volatized during vacuum exposure. The reduction in tensile strength can be explained by this loss of resin during vacuum exposure. This material loss may reduce the ability for the tow to transfer load through the matrix. This also appears to occur with other SMP epoxies such as TP283E. This may occur with other thermoplastic resins as well, but at a much lower level because of their reduced volatility. structure would be exposed to while in the packed state prior to deployment. Figure 7 shows the tow tensile fixture used for mechanical characterization. The first tow samples tested were made from TP277 impregnated 12K and 24K IM9 carbon fiber tows. Only TP277 was tested at the 12Ktow level. From these tests, as well as other manufacturing trials, ILC Figure 7. Tow Tensile determined that 12K tows Test at ILC Dover1 would be too small for most applications. The TP277 results indicate that both tensile strength and tensile modulus decrease substantially from various factors. Figures 8 and 9 summarize the 24K IM9 SMP resin tow tensile test results for the three resins tested. As with the 12K IM9 TP277 samples, the 24K IM9 TP277 tows also show substantial degradation when subjected to the worst case scenarios. The peak tensile load of these fibers decreases 60.5% and there is reduction in tensile modulus of 70.8%. Vacuum at room temperature causes a reduction in peak tensile load of 21.6%. Flexing the material 180o ten and twenty times results in similar degradation. This indicates that significant reduction in properties is occurring before 10 folds, but no further reduction occurs between 10 and 20 folds. The 12K TP277 data showed that folding the tows ten times resulted in a 41% reduction in peak tensile load. Folding the tows twenty times after vacuum and heat exposure reduces their peak load values another 11% (for a total of 52% reduction from the baseline values). At this point, the tows seem to reach a maximum amount of degradation and will no longer experience a reduction in performance due to vacuum, heat, or additional 180o folds. The 12K TP277 tows also experienced a 63.7% reduction in tensile modulus when subjected to worst case conditions. The data showed The 24K IM9 TP283E showed much more promising results than the TP277 testing. However, these tows still experienced reductions in peak tensile load (42.1% reduction) and tensile modulus (30% reduction) when subjected to worst case conditions. Flexing the material 10 and 20 times without any vacuum or heat also reduces the peak tensile load (31.8% reduction after 10 2000 SMP Resins vs. Average Tensile Peak Load 1880 1800 Average Peak Load (N) 1600 1699 1739 TP 277 TP 283E TP 406 24k IM9 Carbon Fiber 1644 1571 1528 1529 1449 1422 1358 1400 1262 1257 1159 1200 1159 1155 1154 1186 1056 1000 1003 984 885 865 803 800 726 709 659 600 500 400 200 0 No Bake, Bake @ No Bake, Bake @ No Bake, No Bake, No Bake, No Bake, Bake @ No Bake, No Vac, No 85C for 46 Vac @ RT 85C for 46 Vac @ No Vac, 10 No Vac, 20 Vac @ 85C for 46 Vac @ Flex hrs, No for 8 hrs, hrs, Vac @ 125C for 8 Flex* Flex* 125C for 8 hrs, Vac @ 125C for 8 Vac, No No Flex RT for 7 hrs, No hrs, 10 125C for 8 hrs, 20 Flex hrs, @ Flex Flex* hrs, 20 Flex* 125C for 1 Flex* hr, No Flex Tow Environmenal Exposure Characteristics Figure 8. SMP Resins 24K Peak Tensile Load Results1 6 American Institute of Aeronautics and Astronautics *Folded over 0.25mm radius 200 SMP Resins vs. Average Tensile Modulus 184 180 24k IM9 Carbon Fiber Average Tensile Modulus (GPa) 160 160 156 147 143 140 129 120 100 TP 277 TP 283E TP 406 154 147 141 112 119 117 110 94 88 94 93 93 93 85 85 81 80 60 41 36 40 35 37 35 20 0 No Bake, Bake @ No Bake, No Bake, No Bake, No Bake, Bake @ No Bake, Bake @ No Bake, Vac @ 85C for 46 Vac @ No Vac, 10 No Vac, 20 Vac @ No Vac, No 85C for 46 Vac @ RT 85C for 46 125C for 8 hrs, Vac @ 125C for 8 Flex* Flex* for 8 hrs, hrs, Vac @ 125C for 8 hrs, No Flex hrs, 20 125C for 8 hrs, 10 hrs, No RT for 7 No Flex Vac, No Flex* hrs, 20 Flex* Flex hrs, @ Flex Flex* 125C for 1 hr, No Flex *Folded over 0.25mm radius Tow Environmenal Exposure Characteristics 1 Figure 9. SMP Resins 24K Tensile Modulus Results TP406 has lower baseline properties than the other two resins, but comparing the resins after 20 flexes without heat or vacuum exposure, it is clear that the TP406 resin is the most robust resin in terms of packing. However, it does degrade substantially with the combination of hard vacuum, high temperature, and repeated 180o flexing. Further study is ongoing at ILC with different fiber types to determine their 180o folding damage resistance with SMP resins. folds and 41% reduction after 20 folds). From this data, just as with the TP277 results, there appears to be a point at which the material properties will no longer degrade no matter what influence the material is subjected to. Vacuum exposure at room temperature alone degrades the peak tensile load values by 26.0%. However, the 180o flexing appears to contribute to the degradation more than any other factor. TP406 resin appears to be significantly degraded by hard vacuum at high temperature followed by 10 and 20 cycles of 180o flex. This resulted in a 71.2 % reduction in peak tensile load. Vacuum at room temperature does not affect the resin. In fact, those samples held the highest load relative to all of the other TP406 samples tested. Flexing the material 10 and 20 times without any vacuum or heat reduces the tensile strength only slightly (18.2% reduction). This is the lowest reduction in strength from 180o flexing out of the three resins tested (TP277 had a 71% reduction and TP283E had a 41% reduction). High temperature exposure appears to be the main cause in reduction in physical properties for the TP406 resin. This is most likely because urethanes are known to absorb water, and when heated, this additional water can cause material degradation. However, further research is required to understand and further quantify these effects. Figure 10 is a comparison of calculated, baseline, and worst case values for composite tow tensile modulus for TP283E and TP406. The calculated values in the chart were determined using the rule of mixtures (Ec=Vf*Ef+Vm*Em)9. Where Ec is the tensile modulus of the composite tow, Vf is the fiber volume fraction, Ef is the tensile modulus of the IM9 fibers, Vm is the matrix volume fraction, and Em is the tensile modulus of the resin. These calculated values are based on the average fiber volume fraction of the experimental samples. The baseline values in the chart were obtained experimentally from composite tow samples that were not subjected to any environmental exposure. Baseline values for every resin and every tow size are not available at this time. The experimental values may sometimes be higher than the calculated values because of the diameter variations on each of the tows, which was used to calculate experimental modulus. This data is important for future applications where larger tow sizes may be needed to meet system level load requirements. From this initial data, it can be concluded that larger tow sizes of up to 48K will experience similar degradation in tensile properties as do the smaller (12K and 24K) tows. From Figures 8 and 9, it becomes clear that the TP277 resin is more susceptible to environmental exposure damage than the other resins. TP283E appears to be the best resin in terms of tensile strength and tensile modulus, but it does experience a drop in performance properties from certain environmental exposures. The 7 American Institute of Aeronautics and Astronautics TP283E and TP406 Calculated Vs. Avg. Experimental Tensile Modulus Bake out @ 85C for 46 Hrs, Vacuum 8 hrs @ 125C, 20 Flex* 200 184 180 163 Average Tensile Modulus (GPa) 160 167 156 159 157 155 140 129 119 120 TP 283E Calculated 118 112 110 114 108 TP 283E Baseline 109 TP 283E Experimental 99 100 93 89 TP 406 Calculated TP 406 Baseline 80 TP 406 Experimental 60 IM9 Carbon Fiber 40 20 0 12 k 24 k 36 k 48 k Tow Size *Folded over 0.25mm radius Figure 10. TP283E and TP406 Experimental and Calculated Tensile Modulus1 beam that had been fabricated more than seven months prior to the test and stored at ambient temperature and humidity. The results of this test are provided in Figure 11. Comparing this curve to Figure 2, it is evident that the Tg has risen only 6oC (from 53.0oC to 59.4oC). This shows that the rate of continued cross-linking is very low at room temperature. A gauge length comparison test was also performed during the tow tensile testing to verify that the 20.32cm gauge length used for fabricating all of the tow tensile samples in the study was valid. ILC theorized that the sample gauge length might negatively affect the results of the testing. From the results of the gauge length comparison test it was apparent that the 20.32cm gauge length was valid because of the close proximity of the peak load and modulus values obtained from the 10.16cm tow tensile samples that were tested. Residual Enthalpy STORAGE LIFE / AGING Accelerated aging is an important test that was performed on two of the SMP resins. In actual use, space inflatable systems may be stored at ambient conditions awaiting launch for up to several years. Over that time period, it is imperative that the material properties be well understood. The main concern with some SMP resins is an increase in Tg during the time period when they await launch and deployment. If the Tg rises over this time period, then it is possible that the spacecraft may not have enough power to heat the structure above this higher Tg. If the structure is not heated above its Tg prior to inflation, it will either not deploy (i.e., it will be frozen in the packed position) or deploying the structure will cause damage to the fibers. This could greatly reduce the structural properties of the composite and thus the overall structure. Tg=59.4oC Figure 11. DSC Curve of a TP275 Beam After 7 Months of Room Temperature Storage1 In order to determine what may happen to the resins during long-term room temperature storage, TP283E and TP406 composite samples were placed in ovens set at 80oC and 125oC for up to 168 hours. After their prescribed aging times, the samples were then removed from the oven and DSC testing was performed on three samples of each material. This provided three samples for an average Tg and enthalpy calculation. SMP epoxies, In the case of SMP epoxies, it is possible that they will continue to cross-link over time, especially if they are exposed to high temperatures. The first test that was conducted to address this issue was a DSC on a TP275 8 American Institute of Aeronautics and Astronautics both of these factors assist in the determination of the degree of cross-linking. E1559, Method for Measuring Material Outgassing/Deposition Kinetics, allows for the exposure temperature and time to be varied over the duration of the test. This provided a more realistic evaluation of how outgassing might occur at the elevated temperatures that structures would witness during pre-heating and deployment on orbit. Based on radiation tests results on TP283E’s predecessor, TP275, and the fact that the TP283E resin is an SMP epoxy, it was expected that the TP283E resin would experience an increase in Tg after elevated temperature exposure. It appears that high temperature (125oC) aging does increase the Tg of the resin. TP283E samples aged at 125oC for 1 week had Tg’s of 96oC, while the 80oC samples had Tg’s of close to 74oC after 1 week of aging. Furthermore, the higher the aging temperature, the higher the rate of increase in Tg. Also, based on initial enthalpy testing, it can also be concluded that the degree of crosslinking for TP283E will increase with thermal aging time at high temperature, but the degree of cross-linking will not increase significantly at ambient conditions. TP406 did not experience the same effects of temperature exposure, as did the lightly cross-linked formulations. However, there appeared to be a mild increase in Tg with time at 80oC and 125oC. From the data, the Tg of the resin actually appeared to increase more (from 55oC to 73oC) from the 80oC aging than the 125oC aging. The 80oC thermal aging test was repeated with similar results. Further study is needed to understand the possible chemical reactions between water and the constituents of the polyurethane that lead to these results. The test was performed at 125oC for 24 hours under hard vacuum, to simulate worst case conditions for the material. The heating duration will be much shorter (on the order of hours) in practical application. The temperature selected was based on the glass transition temperature plus a safety factor. These parameters were selected to represent the temperatures and times that a very large structure might see while it is being heated above its Tg to soften it prior to deployment. All of the ASTM E595 and ASTM E1559 samples did not have protective films as they would in actual application. Therefore these outgassing values are higher than what would actually be seen at the system level. Data from each of the 4 materials tested in ASTM E1559, TP406, TP283E, TP277, and TP279B, is summarized below in Table 5. Resin TP220 TP221 TP230 TP264* TP275 TP405 TP415 TP277 Epoxy Resin VACUUM STABILITY Outgassing has been investigated for several thermoplastic resins because of its importance in spacecraft performance. ILC Dover conducted ASTM E595 testing that identified the general performance of SMP resins. The ASTM E595 test was seen as a good screening test to gauge general resin qualities such as Total Mass Loss (TML), Collected Volatile Condensable Materials (CVCM), and Water Vapor Recovery (WVR). Typical NASA acceptance values for TML and CVCM are not to exceed 1.0% and 0.1% respectively. Some values of the preliminary testing can be seen in Table 4. Table 4. ASTM E595 Results1 Matrix TML CVCM (%) (%) Polypropylene 0.26 0.08 Polypropylene 0.25 0.06 Polyethylene 0.13 0.03 Polyester 0.23 0.02 Epoxy 1.95 1.35 Polyurethane 0.36 0.01 Styrene-Acrylic Latex 1.45 0.02 TP283E Table 5. ASTM E1559 Results1 Matrix TML(%) CVCM(%) TML(%) CVCM(%) (4hrs @ (4hrs @ (24hrs @ (24hrs @ 125oC) 125oC) 125oC) 125oC) Epoxy 0.29 0.25 0.75 0.71 TP279B TP406 0.33 0.28 1.23 1.19 Epoxy 0.28 0.22 0.81 0.77 Urethane 0.33 0.31 0.37 0.35 *All samples baked out for 48 hours at 85oC ISOGRID BEAM TESTING From the results of the material testing, TP283E SMP lightly cross-linked epoxy resin was selected and 0.394-meter and 3.0meter long, 0.1778-meter diameter isogrid beams were fabricated and tested after packing and deployment. These results were compared to beams that had not been packed and deployed. One of each tow size (24K, 36K, and 48K) of the 0.4m long Figure 12. Rolled isogrid beams were Isogrid Beam1 flattened and rolled in an oven three times around a 7.62cm mandrel (as in Figure 12). After each folding trial, the beams were placed back into the oven unconstrained and allowed to begin their return to their WVR (%) 0.03 0.04 0.03 0.16 0.10 0.29 0.13 *No bake out. All other resins were baked out for 60 hours at 60oC. The ASTM E595 test provided good general information, but the test conditions did not match those anticipated in actual use. To better characterize the outgassing performance of these resins, another outgassing test, ASTM E1559, was selected. ASTM 9 American Institute of Aeronautics and Astronautics Table 6. 0.4m Isogrid Compression Load Results1 Tow Baseline Packed and Deployed % Change Size Compression 3 Times Failure Load (N) Compression Failure Load (N) original tubular shape. However, it was discovered that the shape memory effect of the resin alone was not enough to fully return the 10.2 cm diameter beams to their original shape. To assist in shape recovery, an inflatable bladder had to be inserted into each of the beams and then pressurized to 1.5psi to bring the beams back to their original shape. This cycle was repeated three times. Following the packing trials, the beams were bonded into aluminum test end caps (Figure 13). and tested for their compressive and torsion properties (Figure 14). 24k 509.8 309.6 -39.3% 36k 1016.5 866.1 -14.8% 48k 1832.3 1570.7 -14.3% Table 7. 0.4m Isogrid Compressive Stiffness Results1 Tow Baseline EA (N) Packed and Deployed % Change Size 3 Times - EA (N) 24k 1.022E+06 7.249E+05 -29.1% 36k 1.600E+06 1.379E+06 -13.8% 48k 1.980E+06 1.998E+06 0.9% Table 8. 0.4m Isogrid Torsional Stiffness Results1 Tow Baseline JG (N- Packed and Deployed % Change Size m2) 3 Times – JG (N-m2) Figure 13. Isogrid Beam Prepared for Testing1 Although the packing did degrade the structural performance of the beams slightly, the results are very promising. The test results from the baseline and packed beams are summarized in Tables 6-8. The peak compressive load data from Table 6 is charted in Figure 15. The load versus deflection curve for the 24K Figure 14. 0.4m TP283E Isogrid Beam During Test1 TP283E 0.4m packed and deployed isogrid tube is provided in Figure 16. Compression Failure Load (N) 2000 1400 -7.8% 1218.8 15.6% 48k 1535.3 1802.3 17.4% TP283E 24K Packed & Deployed Isogrid Compression Data Load (N) 250 200 150 100 50 0 0 1 2 3 4 5 6 7 Deflection (mm) Figure 16. 24K Packed & Deployed Isogrid Compression Data1 As can be seen from these initial results, larger (36K and 48K) tow sizes are less affected by packing and deployment than smaller (24K) tow sizes. In fact, from the data it can be seen that the torsional stiffness increases with the larger tow sizes. This data is based on the average of three baseline isogrid beams and one packed and deployed isogrid beam. Therefore, the packed and deployed data is not statistical, but there is a trend in the data with respect to larger tow sizes. Further study is required to obtain statistical data and verify these initial results. Baseline Compression Failure Load (N) Packed and Deployed 3 Times Compression Failure Load (N) 1200 1000 800 600 400 The 3m isogrid beams were packed slightly differently than the 0.4m beams. After manufacturing the 3m beams, they were permanently bonded into 0.0508m aluminum test end caps. The 3m beams were uniformly 200 0 36k 542.1 1054.6 300 Effect of Packing and Deploying on 0.4m Isogrid Tubes 24k 588.3 36k 350 1800 1600 24k 48k Tow Size Figure 15. Effect of Packing on Compressive Load1 10 American Institute of Aeronautics and Astronautics heated about their Tg and then they were flattened and rolled around the aluminum test end cap starting at the tip. Three of the 3m beams (including one beam that was successfully deployed in a thermal-vac chamber at –80oC) were packed in this way, while one of the 3m beams was Z-folded. The beams were allowed to cool below their Tg in the packed position (Figure 17) and then they were deployed by inflation at 75oC and mechanically characterized. BIBLIOGRAPHY 1. Cadogan, D.P., Lin, J.K, Sapna, G.H., Scarborough, S.E., “Space Inflatable Technology Development for Solar Sails and Other Gossamer Applications: GR/SMP Isogrid Boom Development Final Report,” NASA Task Order 10442, ILC Dover, Inc., October, 2001 2. Cadogan, D. P. and S. E. Scarborough. “Rigidizable Materials for Use in Gossamer Space Inflatable Structures,” AIAA-2001-1417, 42nd AIAA/ASME/ ASCE/AHS/ASC Structures, Structural Dynamics, and Materials Conference and Exhibit AIAA Gossamer Spacecraft Forum, April 1619, 2001. 3. Darooka, D.K., S.E. Scarborough, and D.P Cadogan, “An Evaluation of Inflatable Truss Frame For Space Applications,” AIAA-2001-1614, 42nd AIAA/ASME/ ASCE/AHS/ASC Structures, Structural Dynamics, and Materials Conference and Exhibit AIAA Gossamer Spacecraft Forum, April 1619, 2001. 4. Darooka, D.K., S. Scarborough, S. Malghan, D. Cadogan, C. Knoll, “Inflatable Space Frame,” Final Report, NASA Prime Contract Number: NAS199154, July 2000. 5. Hunt, M., Editor, “1992 Materials Selector,” in Materials Engineering, December 1991. 6. Malghan, S., “Thermoplastic Folding Trials Report, Phase I” ILC Dover IRAD Report 5500-10-A, July 28, 2000. 7. Otsuka, K. and Wayman, C.M., Shape Memory Materials. Cambridge: Cambridge University Press, pp. 203-219, 1998. 8. Paesano, A. and Palmese, G.R., “Carbon-Fiber Reinforced Thermoplastic Materials for Rigidizable Space Systems,” ILC IRAD Supported Work performed by the University of Delaware Center for Composite Materials, March 28, 2000. 9. Vinson, Jack R. and Sierakowski, R. L., The Behavior of Structure Composed of Composite Materials, Martinus Nijhoff Publishers, Dordrecht, Netherlands, 1987. 10. U.S. Patent Application, “Deployable Space Frame and Method of Deployment Therefor,” ILC Dover, Patent Application No. US00/07706. Figure 17. 3m Isogrid Tube Packed With End cap1 SUMMARY Recent shape memory composite developmental work performed at ILC Dover has greatly advanced the state of the art of materials that can be used to construct rigidizable gossamer space inflatable structures. New materials have been developed and tested at both the component and system level proving the viability of this technology. Resins have been developed that meet NASA spacecraft outgassing requirements, that can be stored at room temperature for years, and can be integrated into composite satellite structures that can be tightly packed for launch into space. Isogrid beams fabricated from shape memory polymer resins have been repeatedly packed and deployed to assess damage from folding. Reductions caused by packing in peak compressive load were recorded at levels as low as 14.3%, while compressive stiffness reductions were as low as 0.9%. A 3-meter long, 0.1778-meter diameter, shape memory composite, isogrid beam was also successfully deployed in a thermal vacuum chamber at – 80oC and hard vacuum. Work is continuing at ILC Dover to further improve resin and composite performance and manufacturing characteristics. ACKNOWLEDGEMENTS Much of this work was in support of the ISAE-II program funded by NASA and JPL. Special thanks go to Ms. Jessica Woods-Vedeler and Ms. Judith Watson from NASA Langley Research Center for their program and technical support. The authors also thank technical consultants Dr. Martin Mikulas and Dr. Paul McElroy for their technical advice. 11 American Institute of Aeronautics and Astronautics
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