Self Repairing Composites for Airplane Components

Carolyn Dry, Ph.D., Professor Emeritus, President Natural Process Design, Inc., drycementmixer@aol..com 1250 east 8th street, Winona, Minnesota, 55987, phone 507-452-9113

Abstract
Durability and damage tolerance criteria drives the design of most composite structures. Those criteria could be altered by developing structure that repairs itself from impact damage. This is a technology for increasing damage tolerance for impact damage. Repaired damage would enable continued function and prevent further degradation to catastrophic failure in the case of an aircraft application. Further, repaired damage would enable applications to be utilized without reduction in performance due to impacts. Self repairing structures are designed to incorporate hollow fibers, which will release a repairing agent when the structure is impacted, so that the repairing agent will fill delaminations, voids and cracks in les than one minute, thus healing matrix voids. The intent is to modify the durability and damage tolerance criteria by incorporation of selfhealing technologies to reduce overall weight: The structure will actually remain lighter than current conventional design procedures allow. Research objective(s) were: Prove that damage can be repaired to within 80-90% of original flexural strength in less than one minute, in laminates that are processed at 300350F typical for aircraft composites.. These were successfully met. The main focus was on testing of elements in compression after impact and a larger component in shear at Natural Process Design, Inc. Based on these results the advantages purposes are assessed. The results show potential; with self repairing composites, compressive strength is maintained sufficiently so that less material can be used as per durability and damage tolerance, yielding a lighter structure.

Introduction
The main objective of NPDs Air Force SBIR Phase I and II programs and internal NPD work was to prove that this can be a automatically triggered self repairing system for airplane composites subjected to barely visible impact damage which 1) to stop damage and restore original strength to the composite and repair delaminations to 85% of nondamaged strength and 2) suggest that a lighter weight composite with fewer prepreg

Sensors and Smart Structures Technologies for Civil, Mechanical, and Aerospace Systems 2008, edited by Masayoshi Tomizuka, Proc. of SPIE Vol. 6932, 693212, (2008) 0277-786X/08/$18 doi: 10.1117/12.776497 Proc. of SPIE Vol. 6932 693212-1 2008 SPIE Digital Library -- Subscriber Archive Copy

layers could be used for a durable structure. Also NPD proved that 3) after surviving processing in graphite laminate at 250 for one hour and 325-350 for two hours and 4) can complete the repair within less than a minute. These were accomplished.

The Research
\ Various types of glass encapsulators were tried. Various types of two part adhesives were tried in various locations. After processing at temperatures of 121oC (250oF) and 176o C (350oF) and pressure, the repair fibers were cut open in the matrix and the adhesive was liquid, see figure 1. 1) Repair Chemicals Survive Processing Heat in Graphite Laminates

Figure 1) Repair chemicals survive heating in graphite laminates at 350F for two hours after one hour at 250F. Cut glass repair fibers after processing in the autoclave exhibited liquid inside. Epoxy laminates exhibited regions of cured resin where delamiantion occurred, next to the impact area.. Graphite laminates exhibited the presence of repair chemical in various layers, see figure 2.

Figure 2) Areas of solid repair chemical can be seen in the areas of delaminations side view of repaired graphite epoxy.

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2) Fast Repair Can Be Completed in Under One Minute Compression after impact tests (CAI) were done on the same chemicals at one minute and one week with nearly the same results as seen in figure 3. This showed that the repair occurs in less than one minute.
Speed of Reaction Strength of a Two-Part Free Radical Reaction in CAI Tests at One Week and One Minute

30000

25000

Stren g th (p si)

20000

15000

1 Week 1 Minute

10000

5000

Figure 3) A repair chemical reaction is very fast, less than a minute right and still has similar results when tested after a week, as seen on left. 3) Impact Damage is Repaired and Original Strength Restored Testing has been performed to ASTM Standards for flexure and compression loading, as well as fracture toughness. Shear loading was accomplished as an element test. The drop-tower impactor weight remained constant with change of height to reflect increased energy impacts. This experimental effort was conducted to provide quantitative, feasible proof of structure that repairs itself from impact damage. Studies were done on samples with set parameters, a non-standard set of samples that are nevertheless tested in the same ways, through comparison of a standard set of pristine samples with specimens that were impacted, and specimens that were impacted and subsequently repaired. Flexure Test of Repair ASTM D790 Flexural Properties of Unreinforced and Reinforced Plastics and Electrical Insulating Materials This test method determines the damage resistance of a composite laminate that is subjected to either a three or four point loading system on a simply supported beam. In a four-point loading system, the load is applied at two equally spaced positions from the support points. A composite laminate is constructed in the standard fashion as the other tests. The laminate is then impacted and undergoes a flex test. Testing occurs at a rate of 0.05 in/min and continues until failure.

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Four point bend tests were done on graphite samples. The results showed a repair of 85% in graphite laminates. Three types of controls were made: non-impacted samples no fibers, impacted sample no fibers, and impacted samples empty fibers. Experimental samples were made with different adhesives in eight layered samples of 16 plies and 32. These samples were autoclaved using a vacuum bag at temperature of 121oC (250oF) and also 176o C (350oF) for two hours and low pressure. The samples were impacted and flexed to give quantified results as seen in figure 5.

Figure 4) A research associate demonstrates the fixture set up for four point bend flexure tests, right a flexure test is performed on a graphite laminate sample.
Flexural Modulus (Msi), Hand Calculated, without Outliers Carbon Samples, 16 plies, 2 tubes per repair sample

7.00

6.00

5.00

4.00

3.00

2.00

1.00

0.00

Control, No Impact

Control, Impacted

Repair, No Impact

Repair, Impacted

Figure 5) Repair in flexure test on graphite laminates shows that the modulus of the repaired sample (third form right) was 85% of the controls not impacted, on the left. Testing of Self Repair of the Matrix When damage occurs in a composite there are two materials that can experience the damage: fibers or the resin matrix. Since the fibers are continuous, once the fibers are broken there is no way of reattaching their ends; however they can be rebounded to the matrix. The goal is to repair any damage that has occurred in the matrix especially delaminations as well as cracks and voids. In compression and shear the adhesive and strength properties of the resin matrix are very important. The matrix must maintain the fibers as straight columns and prevent buckling, along with transferring the load across the fibers. Since only repair damage that has

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occurred to the matrix is attempted, tests were performed that isolated the strength the matrix adds to the material. These properties can be seen when compressive and shear loads are applied to the material.

Compression Tests of Controls ASTM D6641 Determining the Compressive Properties of Polymer Matrix Composite Laminates Using a Combined Loading Compression (CLC) Test Fixture Compression Test (without impact): to determine compressive strength of controls with no impact determines the compressive strength of an undamaged composite coupon. The coupon dimensions are 5.5 inches by 1.3 inches by approximately 0.18 inches. The laminate is the standard layout using bi-directional laminates in a quasi-isotropic, symmetric layout with tubes in layers in a horizontal plane. The coupons are tested in a combined loading test fixture and testing occurs at a rate of 0.05 in/min and continues until failure.

Figure 6) The test fixture with a control compression sample in it.

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Non-Impacted Controls Tested in Compression

60000

50000

40000

Peak Stress

30000

20000

10000

Control- Impacted, tested in compression after impact fixture Control- Not impacted, tested in compression fixture

Figure 7) A comparison of compression tests results using the compression after impact fixture and the pure compression fixture, Peak stress is reported in PSI, pounds per square inch. Most of the test results on self repair in compression after impact testing needed to be compared to a non impacted control sample set. To obtain these compression without impact control results, two different sets of tests were run. One set involved the use of the same size sample and fixture as the compression after impact (CAI) tests but without an impact. The other samples, of much smaller physical dimensions, were tested in a small fixture appropriate for pure compression testing. The results from testing in the CAI fixture were consistent among the samples and had a low standard deviation, which indicates that the individual sample results did not vary greatly. The other set of pure compression had much larger standard deviation. It is known among researchers that this pure compression test tends to give varying results, partly due to the test set up and difficulty of preventing sample slippage because the samples not fully restrained. On the other hand if there is a center buckle in the non impacted samples tested in CAI, and the sample had been fully restrained and so did not slip, this lends credence to the accuracy of the result of tests in CAI. Both sample sets numbers were within a close range to each other, 40,000 for the CAI ones and 42,000 for the pure compression set. The CAI sample set was selected as the control set because 1) that set had the least standard deviation and 2) the tests were done in the same fixture used for all the other sample sets to which they would be compared.

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Two sets of experiments were done on the same failure type, i.e. compression. The most accurate control set number was used (obtained with the CAI fixture). The data was normalized to this control number. In charting other results, the experimental sample numbers are normalized to these non impacted controls for ease of comparison. Compression After Impact Tests ASTM D7136 Measuring the Damage Resistance of a Fiber-Reinforced Polymer Matrix Composite to a Drop-Weight Impact Event and ASTM D7137 Compressive Residual Strength Properties of Damaged Polymer Matrix Composite Plates The main compressive test that was used is the Boeing Compression After Impact, BSS7260 Test. This test involves impacting a specimen at a controlled energy level and then performing a compressive strength test, as shown in the picture, with three sides of the specimen clamped, and a compressive load applied to the fourth side. Delamination will cause a premature buckling at the delaminating interfaces. Initially, the delaminated regions remain stable as the load is applied. As the load increases it initiates buckling in the delaminated regions. Eventually, this buckling propagates horizontally until the sample collapses with a loud report. If the delaminations in the sample can be repaired, then this test provides data that can report the repair of the matrix was accomplished. When ASTM standards D7136 and D7137 are used in conjunction, the test method is referred to as a Compression after Impact (CAI) test. In a CAI test, the damage resistance of a 4 inch by 6 inch composite laminate is determined. A flat, rectangular composite laminate is subjected to a drop weight impact. After impact, the sample is placed into the bottom half of the CAI fixture and securely tightened. Then the top half is clamped onto the sample and the sample is placed under the cross head. The cross head is jogged down until it is right above the fixture. The sample is then preloaded until there are 50 pounds on the sample. At this point the testing is started with a rate of 0.05 in/min and continues until failure. The test program will automatically calculate the peak stress from the crosssectional area and the peak load. The samples for CAI testing were made of bi-directional laminates at 90 degrees and layout was quasi-isotropic, symmetric with tubes placed in layers towards the bottom from the impact As per the ASTM standard, to be valid the samples must buckle in the same place at the centerline where impacted. If a sample buckles elsewhere the data is not used. Therefore it is critical to experimentally determine a load which will cause repeatable buckling locations at the centerline. The progression of failure is described in figure 11 as The compression after impact (CAI) failure sequence. (1) At the beginning of the load cycle the damages laminate remains stable. (2) The strain level becomes high enough to initiate buckling at one or more of the delamination interfaces, resulting in a thin, buckled sublaminate and a thicker, more stable sublaminate. (3) As the load increases, the thin sublamination buckles and further out-of-plane loads result around the perimeter of the delamination. The postbuckling continues until the out-of plane loads exceed the critical mode 1 strain

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energy release rate or the interlaminar tension allowable. The final failure occurs as the delamination propagates perpendicular to the principal strain direction and the laminate collapses. This quote is from the Boeing Compression After Impact Test, BSS-7260 T.

Figure 8) At left is a CAI sample in the Boeing fixture after failure and at right is the sample after impact and compression loading by NPD. The failure occurred at the exact place impact occurred.

_______
- Initial loading Load

_______H
2. rnitial buckling Load

t
-H

3. Firtal delamination progagation and colFapse

Figure 9) Illustration of the failure sequence in a compression after impact test. The drawing is taken from the Boeing Compression After Impact Test, BSS-7260. Compression after Impact (CAI) tests were done on graphite samples to assess the repair of the matrix resin and results showed a repair of 87% in graphite laminates. Three types of controls were made: non-impacted samples no fibers, blue, impacted samples no fibers, red, impacted samples dummy repair chemical in fibers, blue. Experimental repair

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samples, yellow were made with adhesives in fibers. These samples were autoclaved using a vacuum bag at temperature of 121oC (250oF) one hour and also 176o C (350oF) for two hours and low pressure. The samples were impacted and then compressed to give quantified results as seen in figure 10.
Compression After Impact Strength From 180 in-lb Impact
1.1 1 0.9

Peak Stress (Normalized)

0.8 0.7 0.6 0.5 0.4 0.3 0.2 0.1 0 Control Control- Impacted Control- Empty Tubes- Impacted Experimental with Repair Chemicals- Impacted

Figure 10) Compression after impact tests impacted by a 9 inch drop of a 20 pound weight, 180 inch pounds. The self repairing sample (called experimental, in black) repairs 87% of the non impacted laminate without tubes, white column. Element Testing: in Shear In-plane Shear BMS 4-23 specifies the procedure for determining the in-plane shear stress of a composite laminate. In this test, the laminate is loaded into a picture frame fixture and is tested under force to determine the in-plane panel shear strength. The laminate is constructed as a 9.5 inch by 9.5 inch laminate and placed in the diamond shaped frame fixture. The standard laminate layout is the same as for the CAI tests: However, doublers are adhered to the laminate, one on each side. They are 9.5 inch by 9.5 inch laminates with a 6.5 inch by 6.5 inch square cut out of the middle. The samples are made of woven plies on each of the doublers and the sample itself is made of woven plies.

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The crosshead movement applies force to create shear that is applied because distributed fasteners on the edges of the picture frame produce a traction load along each side, causing a deformation from square to diamond shape. Testing occurs at a rate of 0.05 in/min and continues until failure. Like the CAI tested samples, these must fail at the same location to be included in the data set; that is at the centerline where impacted. It was critical to use suitable impact force to generate consistency in buckling location. The 500 inch pound impact load was experimentally found to generate buckling at the same center impact location.

Figure 11) Shear sample being placed into fixture frame and right the sample after testing in impact and then shear.

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1.1

Carbon/Epoxy Laminates Tested in Shear

In Plane Shear Stress (Lb/In) (Normalized)

0.9 0.8 0.7 0.6 0.5 0.4 0.3 0.2 0.1 0

Control Control- No Tubes Impacted Control- Empty Tubes Impacted- Experimental 1 Impacted- Experimental 2

Figure 12) A chart of the data points on shear impacted at 25 inches with a 20 pound weight for a total 500 inch pounds. The optimum repair sample had a peak stress that is 82 % restoration of peak shear stress strength when compared to the non-impacted control. Tests on Samples with Variable Thickness These thin samples are .1 inch thick as compared to thicker samples used on other testing. These were organized to the same layout order as thicker samples.

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Compression after Impact Stength for 1/10" Thick Samples 1.20 1.10 Peak Stress (Normalized) 1.00 0.90 0.80 0.70 0.60 0.50 0.40 0.30 0.20 0.10 0.00 No Impact 180 in-lb Impact 340 in-lb Impact Control Control - Impacted Experimental with Repair Chemical - Impacted

Figure 13) Thin samples tested with two different impact forces
Compression After Impact Strength From 180 in-lb Impact
1.1 1 0.9

Peak Stress (Normalized)

0.8 0.7 0.6 0.5 0.4 0.3 0.2 0.1 0 Control Control- Impacted Control- Empty Tubes- Impacted Experimental with Repair Chemicals- Impacted

Figure 14) The thicker CAI samples tested with 180 inch pounds. Thin samples repair slightly better than thicker samples. Thinner samples repaired 93% of non-impacted controls peak stress at 180 in-lb of impact load, whereas the standard set thicker samples repaired 88% of non-impacted controls peak stress at 180 in-lb of impact

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load. This is to show that thinner samples can repair more effectively than thicker ones and the implication is that number of plies in the laminate could be cut.

Conclusions
The feasibility of impact-initiated delivery of repair chemicals from hollow fibers embedded in graphite fiber polymer matrix composites has been illustrated. Selfrepairing structures, through coupon and element tests, were demonstrated, and evaluated. Barely Visible Impact Damage (BVID) was imparted to test coupons. Breaks in the hollow repair fibers released repair chemicals that then flowed into damage areas due to delaminations. Effectiveness of self-repair capability was determined through comparison of measured ultimate strength of non-impacted samples with samples that were impacted, and samples that were impacted and then repaired. The overall objectives for Natural Process Design, Inc. (NPD) were met. The objectives were to show feasibility of: 1) Chemistry and repair system can resist heat of processing for graphite prepregs (325 F for two hours after 250 F for one hour) and then repair composites 2) Chemistry and system can repair is less than one minute 3) Repair system and chemistry can restore strength of 85% to the composite laminate 4) The repair system can allow for thinner composites which will meet durability requirements.

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