Resistance Heating for Self-healing Composites NATHAN KWOK* AND H. THOMAS HAHN Department of Mechanical and Aerospace Engineering University of California, Los Angeles Los Angeles, CA 90095, USA ABSTRACT: Thermally remendable polymers have recently become available that are paving the way for the creation of self-healing composites. This article investigates the use of carbon fibers as a resistive heating network for future use in a self-healing composite. Various electrode methods are studied in an attempt to reduce the contact resistance that causes localized heating around the electrode. In addition to localized heating, electrical conduction through the fibers creates heat through composite resistance. It was observed that for short distances between electrodes, contact resistance dominates while over longer distances, composite resistance dominates. The balance between the two types of heating is measured and modeled using finite element modeling (FEM). KEY WORDS: self-healing composite, resistance heating, electrical resistance, finite element modeling. INTRODUCTION R ESISTIVE HEATING HAS many applications and is most commonly seen in electric stoves and heaters. It operates on the principle that current passing through a resistive element must dissipate power according to the equation P ¼ I2R, where P ¼ power (W), I ¼ current (A), and R ¼ resistance (). Heating can be provided in composites by treating the fibers, which are conducting, as resistive elements while the surrounding matrix acts as an insulator. This is applicable in the use of a specially made, heat-activated resin that utilizes a Diels–Alder reaction to heal itself [1]. When this resin is combined with carbon fibers, a self-healing composite can result. The challenge lies in efficiently delivering the heat, without needlessly heating areas far from the crack. There are two kinds of resistance: composite and contact. Composite resistance is associated with the resistivity of the individual fibers, a material property, as well as the *Author to whom correspondence should be addressed. E-mail: natek@ucla.edu Figures 1–3, 5–16 and 18–22 appear in color online: http://jcm.sagepub.com Journal of COMPOSITE MATERIALS, Vol. 41, No. 13/2007 0021-9983/07/13 1635–20 $10.00/0 DOI: 10.1177/0021998306069876 ß 2007 SAGE Publications Downloaded from jcm.sagepub.com at PENNSYLVANIA STATE UNIV on April 8, 2016 1635 1636 N. KWOK AND H. T. HAHN length and diameter of the fibers. In addition, electrons pass internally between adjacent fibers in contact. This internal contact resistance is associated with the contact surface area between two fibers in contact. Because the matrix is almost insulating, most conduction occurs through fibers. These resistances combine to create a highly anisotropic composite resistance. The internal fiber structure can be modeled as a network of interconnected resistors [2], with the resistors running along the fiber direction representing fiber resistance, and resistors running against the fiber direction representing internal contact and matrix resistance. In addition, there is significant external contact resistance between the electrodes for the external power source and the outer surface of the composite itself. This is a function of the method of electrode attachment as well as the presence of the resin-rich upper layer that can interfere with fiber/electrode contact. Although very low contact resistances can be achieved through copper electroplating [3], an attempt is made here to achieve low contact resistance using simpler and more portable methods. Seven different electrode configurations are tested to determine their contact resistance. This external contact resistance is strictly between the electrode and the fiber surface, and is not to be confused with the internal contact resistance between individual fibers, which is a component of composite resistance and is not analyzed separately. The resistance is measured directly using a sourcemeter. Resistive heating experiments are also performed using a DC power supply and IR thermometer. A finite element analysis is done using the FEMLab to simulate the effects of resistive heating. The parameters of the simulation are made identical to those of the actual specimens to test the validity of the model. EXPERIMENTAL PROCEDURE FOR RESISTANCE MEASUREMENT Two laminates were used in testing, both prepared from 255 255 mm sheets of AS4/3502 prepreg, one with a [0/90]S layup (four layers, ‘Composite 1’) and another with a [90/0]S layup (‘Composite 2’). They were autoclave cured at 450 K (350 F) under 0.55 MPa (80 psi). The cured laminates were then cut into strips, with each strip measuring 255 21 0.68 mm. Some of the tests required the specimens to be sanded to remove the resin rich top layer. This was done with 180 grit sand paper until it began to turn black, indicating the fibers were exposed, and then finish sanding was performed using 400 grit followed by 1000 grit. Once sanding was done, the thickness was reduced to 0.62 mm for Composite 1 and 0.61 mm for Composite 2. To test the contact resistance, a Keithley sourcemeter was used in two-probe mode at 2.1 V (Figure 1). The meter measures resistance by applying a DC voltage and measuring the current that passes through the specimen. The meter was connected to the sample using alligator clips, either alone or using one of the six electrodes as an intermediary. The materials used in the intermediate electrodes are listed in Table 1, and the electrode configurations are listed in Table 2. Electrodes 1, 2, and 7 can be considered ‘moving’ electrodes in that they are in no way permanently attached to the composite. This allows for the distance between electrodes to be varied in small intervals (5 mm intervals were used), resulting in many test points. The design for electrodes 2 and 7 is illustrated in Figure 2. These are referred to as ‘contact electrodes’ because they utilize a C-clamp to apply contact pressure on the surface. The contact electrodes were constructed in an attempt to lower contact resistance while still Downloaded from jcm.sagepub.com at PENNSYLVANIA STATE UNIV on April 8, 2016 1637 Resistance Heating for Self-healing Composites Resistance measurement composite 1: [0/90]s Sourcemeter Top surface sanded 0.62 mm d 21 mm 255 mm Vise grip Rubber insulation Bottom surface insulated by electrical tape Alligator clip Figure 1. Sample held in place by clamp and measured using a sourcemeter or LCR. Alligator clips attach either directly to bare composite or to an intermediate electrode. Table 1. List of electrode materials. Material name Manufacturer Catalog no. Copper tape Carbon tape Silver paint Copper sheet Conductive rubber Miniature C-clamp SPI Supplies SPI Supplies SPI Supplies McMaster Carr Zoflex Nelson Hobby 05012-AB 05081-AB 05001-AB 8944K37 CD45.1-6S-2 C100 and C102 Table 2. List of electrode types. No. Material Contact size Measurement distance intervals, d (mm) 1 2 None (alligator clip on bare composite) Small conducting rubber pad, silver paint, copper sheet, C-clamp Single-sided adhesive copper tape Double-sided adhesive carbon tape Narrow silver paint line Wide silver paint line Large conducting rubber pad, silver paint, copper sheet, C-clamp Multiple point contacts 6-mm diameter (circular) 5–235 at 5 mm intervals 10–230 at 5 mm intervals 6 6.5 mm 6 21 mm 6 21 mm 12 21 mm 10 12 mm 5, 100, 200 5, 100, 200 5, 10, 20, 50, 100 20, 50, 100 10–220 at 5 mm intervals 3 4 5 6 7 allowing for portability. The contact surface is composed of a conducting rubber pad made by Zoflex, with a small round version measuring 6 mm in diameter and 0.5 mm in thickness and a large rectangular version measuring 10 12 mm. This pad was then wetted with silver paint and attached to a thin copper plate measuring 6 20 mm for the small version and 10 20 mm for the large version. The plate was then glued to a lightweight plastic C-clamp. The entire assembly allows for multiple electrodes to be attached to the copper plate via alligator clips and then easily loosened and moved from location to location. Electrodes 3–6 were fixed on the composite. This limited the number of distance intervals because too many electrodes could effectively shorten the length of the composites by creating low resistance zones. For the copper and carbon tape (3 and 4), the electrodes were cut to size and pressed onto the surface of the composite. In both cases Downloaded from jcm.sagepub.com at PENNSYLVANIA STATE UNIV on April 8, 2016 1638 N. KWOK AND H. T. HAHN Alligator clip Contact electrode Composite Rubber conducting pad Silver paint interface Copper sheet Alligator clip Composite C-Clamp Electrical tape Crazy glue Figure 2. Alligator clips are a quick method of attachment but have a small contact area. Electrode 2, ‘small contact electrode’ can act as an intermediary and is a better design because it applies pressure to the surface and has more contact area. 5 10 mm mm 20 mm 50 mm 100 mm Figure 3. The thickness of the fixed electrodes limited the interval spacing. the adhesive was designed for such an application and is electrically conductive. In the case of the silver paint strips (5 and 6), these were painted on with a small brush and allowed to dry. Figure 3 is a photograph of electrode type 5: narrow silver paint lines. EXPERIMENTAL PROCEDURE FOR RESISTANCE HEATING The circuit setup and temperature measurement apparatus for resistive heating are shown in Figure 4. The purpose is to use electricity to heat the composite and measure the resulting temperature field. Two methods of electrical contact were used, Figure 4: the simple alligator clip, (electrode 1 from Table 2) and the ‘large contact electrode’ (electrode 7 from Table 2). To measure temperature, a Land Instruments PockeTherm 32C IR thermometer was used with the measurement point occurring every 10 mm, indicated by the dots in Figure 4. The thermometer was calibrated using a thermocouple. To minimize conduction out of the specimen, the specimen was clamped in place by a small vice lined with ceramic insulation. RESULTS: CONTACT RESISTANCE The overall resistance R measured by the Sourcemeter can be modeled as a series of three resistors with the equation: R ¼ R1 þ R2 þ R3 Downloaded from jcm.sagepub.com at PENNSYLVANIA STATE UNIV on April 8, 2016 ð1Þ 1639 Resistance Heating for Self-healing Composites Resistively heating composite 1: [0/90]S DC power supply Ammeter x I+ I− 170 mm Infrared thermometer 21 mm 20 mm V+ V− Voltmeter Ceramic insulation 255 mm Figure 4. Dots represent thermal measurement points. lþ/l and Vþ/V are the attachment points for the power supply and voltmeter, respectively. where R1 and R3 are the contact resistances associated with the two electrodes. We can assume that R1 ¼ R3 because in every case, the positive and negative electrodes are identical. R2 is the resistance of the composite given by R2 ¼ d A ð2Þ where is the effective resistivity of the composite, d is the distance between two electrodes, and A is the cross-sectional area. This equation depends on the assumption that potential remains constant on a cross section and only varies in the axial direction, and is reasonable for a long, thin specimen like the one used. The resistance values should scale linearly as the electrode spacing increases, since the resistivity and cross-sectional area remain constant. While composite resistance scales linearly, the contact resistances R1 and R3 should remain constant as long as the electrode type remains the same. Thus we can solve Equation (1) and (2) for R1 by plotting R(d) at multiple values of d, and using linear regression to arrive at a y-intercept, which is the value of 2R1. Alligator Clips The first test was conducted on Composite 1 with no intermediate electrode, only alligator clips clamped onto a bare composite. The distance was varied from 5 mm to 245 mm at 5 mm intervals. At each interval, the resistance was recorded and is shown in Figure 5. Although the Sourcemeter can read resistance accurately down to 1 m, the precision was limited to 0.1 due to fluctuations caused by the electrode itself. For this electrode there was also extremely poor consistency. Although the reading did appear to trend upward, the residual standard deviation (also known as the standard error of the y estimate) of the measurements was 3.86 , too large to make a conclusion. In addition to Downloaded from jcm.sagepub.com at PENNSYLVANIA STATE UNIV on April 8, 2016 1640 N. KWOK AND H. T. HAHN 40.0 35.0 Resistance (ohms) 30.0 25.0 y = 0.0213x + 24.935 20.0 15.0 10.0 5.0 0.0 0 50 100 150 Distance (mm) 200 250 Figure 5. Resistance varied wildly without an intermediate material. poor consistency, the y-intercept of the linear regression was 24.9 , indicating a contact resistance (R1 þ R3) so large that it dwarfed any composite resistance (R2). The problem lies in the irregularity of the composite surface and the low conductivity of the composite. In addition, even careful sanding can still leave some resin on the surface of the composite which can interfere with the very small contact areas of an alligator clip. By contrast, attaching an alligator clip to a highly conductive copper plate always ensures a good contact. Clearly, an intermediate material would be beneficial. Small Contact Electrode Utilizing the contact electrode shown in Figure 2 greatly improved the results, both in terms of measurement consistency and contact resistance. This time the residual standard deviation was only 0.10 , a 97% reduction. The equation for residual standard deviation is: sffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi P ðyi y^i Þ2 sy ¼ n2 ð3Þ Where yi is the measured y-value, ŷi is the fitted y-value, and n is the number of samples. The resulting equation for resistance is Rðd Þ ¼ 0:0053d þ 1:3178 Downloaded from jcm.sagepub.com at PENNSYLVANIA STATE UNIV on April 8, 2016 ð4Þ Resistance Heating for Self-healing Composites 1641 so that the contact resistance of each electrode is: R1 ¼ R3 ¼ 1:3178 ¼ 0:659 : 2 ð5Þ The composite resistivity, , can also be calculated from Equations (2)–(4) in conjunction with the measured cross-sectional area 13.02 mm2: ¼ 0:0069 -cm ð6Þ This result compares favorably with the measured value from the literature [3] of 0.00293 -cm for unidirectional composite under the assumption that no current passes through the 90-degree plies. In reality, a small fraction of current does pass through the 90-degree plies, but the ratio of conductivity between the 0 and 90 directions has been measured to be as high as 1400:1 [3] and as low as 26:1 [4], meaning even in the best case the amount is very small. The contact resistance for the contact electrode was lower due to a combination of a larger contact area and the rubber pad’s ability to conform to the micron size asperities of the surface. In addition, the C-clamp exerted a downward pressure on the electrode, further improving its performance. By contrast, although the alligator clips also exerted a downward pressure, it had a small net contact area and thus a lower likelihood of contacting any exposed fibers. Interestingly, the contact electrode still utilized alligator clips; however, in this case the alligator clips were attached to a copper sheet instead of directly to the composite. Considering that there were more contact interfaces involved in the use of the contact electrode, one might think this would actually increase contact resistance; however, this was not the case. In fact, the additional contact interfaces actually had a negligible effect on overall contact resistance. Clearly, the critical interface is between the fiber surface and whatever it is in contact with. The composite resistance determined from Figure 6 can be used as a baseline for other electrode materials that do not allow for as many measurements. Since the composite resistance does not change when different electrodes are used, it can simply be subtracted from the total resistance to get contact resistances of other electrodes. Copper, Carbon, and Silver Electrodes The ‘fixed’ type electrodes were either conductive tapes (copper and carbon) or conductive paint (silver). As shown in Figure 3, this allowed for limited measurement intervals. The results are summarized in Figure 7. Results from the small contact electrode as well as the big contact electrode, which utilized a larger rubber pad, are also included. The carbon tape, which is made by SPI Supplies and intended for attaching specimens to scanning electron microscope holders, is designed to provide a conducting path from the specimen (which must be conducting) to the specimen holder (which acts as a ground). For the present purpose, it performed very poorly, actually increasing the contact resistance compared to the alligator contact by itself, in addition to being wildly erratic. Downloaded from jcm.sagepub.com at PENNSYLVANIA STATE UNIV on April 8, 2016 1642 N. KWOK AND H. T. HAHN 3.0 Resistance (ohms) 2.5 R(d ) = 0.0053d + 1.32 2.0 1.5 1.0 0.5 0.0 0 50 100 150 Distance (mm) 200 250 Figure 6. Measurement results greatly improved. 50 Small contact Alligator Copper Carbon Narrow silver Wide silver Big contact Resistance (ohms) 40 30 20 10 0 0 50 100 150 Distance (mm) 200 250 Figure 7. Complete summary of resistance. The adhesive-backed copper tape, which was also designed for the same purpose as the carbon tape, did much better, markedly reducing contact resistance as well as showing reasonable consistency, although it still fell well short of the contact electrode. The silver paint was better than the copper tape but also still short of the contact electrode. Surprisingly, when two versions of the silver paint were tried, one using a narrow 6 21 mm painted area and one using a double size 12 21 mm area, the narrow electrode performed better, nearly matching the contact electrode. One possible explanation is that the silver was applied in a thinner layer for the wider electrode. The reverse result occurred when increasing the size of the contact electrode: the total contact resistance (R1 þ R3) was reduced from 1.318 to 0.788 while still maintaining the same excellent consistency. As expected, the measured composite resistance (R2) was Downloaded from jcm.sagepub.com at PENNSYLVANIA STATE UNIV on April 8, 2016 1643 Resistance Heating for Self-healing Composites Contact resistance of various electrodes for composite 1 35 32.59 30 Resistance (ohms) 25 Double-sided carbon tape Bare composite 24.78 Single-sided copper tape Wide silver paint line 20 Narrow silver paint line Small contact electrode 15 Large contact electrode 9.13 10 5.67 5 2.52 1.32 0.788 0 Method Figure 8. Contact resistance values varied greatly. almost identical. To calculate the contact resistance values listed in Figure 8, the distance, d, at each measurement interval was multiplied by 0.053 /mm, Equation (3) to arrive at the appropriate composite resistance. This was then subtracted from the total resistance measured to obtain the contact resistance. The resulting contact resistance values at each interval were then averaged. Comparison Between [0/90]S and [90/0]S Laminates In addition to comparing electrodes, a second composite laminate, Composite 2, was made identically to Composite 1 with the only difference being that it was cut such that the top and bottom layer of fibers ran in the transverse rather than longitudinal direction. The only other difference was a very slight difference in dimensions. The purpose of this experiment was to verify that the effects of current spreading in the thickness direction are negligible enough that the layup does not affect the overall resistivity, given that the number of transverse and longitudinal layers remains the same. As the thickness goes up, this could cease to be the case. This time the test was done using the large contact electrode since the previous test demonstrated it had the lowest contact resistance. The results are as expected because in the short intervals, Composite 2 displays slightly higher resistances along with less consistent results, until around 100 mm when it begins matching Composite 1 (Figure 9). From that point on, the results are almost identical. One explanation for the discrepancy at the shorter intervals is that the electrodes are connected to a 90 layer which has lower conductivity. As the current spreads out, the effect of electrode location diminishes. Effects of Sanding Top Surface Thus far every test has been performed on a fully sanded specimen. It is known that by sanding the resin rich top layer, more fibers are exposed, improving conductivity. Downloaded from jcm.sagepub.com at PENNSYLVANIA STATE UNIV on April 8, 2016 1644 N. KWOK AND H. T. HAHN 2.5 Resistance (ohms) 2.0 1.5 1.0 [0/90] [90/0] 0.5 0.0 0 50 100 150 Distance (mm) 200 250 Figure 9. The [90/0] specimen displayed some inconsistency in the shorter intervals. The large contact electrode was used in both specimens. Figure 10. Microscopy reveals a resin rich top layer that must be removed by sanding. Magnification is 100, FOV is 2.14 mm wide. Left: before, right: after. To quantify this, another strip of the same dimensions was cut from Composite 1 and resistance tested at various levels of sanding. The ‘large contact electrode’ was used in every case, and three replicates were performed at each location to assess testing variance. The test was done before sanding, then after sanding with 180, 320, 400, and 1000 grit for 5 min each. Photographs at 100 comparing a sanded and an unsanded sample are shown in Figure 10. The resin-rich layer with an imprint left from the peel-ply is clearly seen before sanding, and disappears after sanding with 180 grit. Additional sanding was not evident in the photograph although a continual reduction in contact resistance occurs as more sanding is performed. The other major benefit of sanding is that it greatly improves the consistency of the results. Figure 11 shows the plot of resistances and the lines of best fit while Figure 12 shows the plot of standard deviations. Standard deviation decreases greatly after the first sanding, and then increases slightly before dropping again. Downloaded from jcm.sagepub.com at PENNSYLVANIA STATE UNIV on April 8, 2016 1645 Resistance Heating for Self-healing Composites 3.25 Unsanded 180 grit 320 grit 400 grit 1000 grit Resistance (ohms) 2.75 2.25 1.75 R(d )0 = 0.003812d + 1.5942 R(d )180 = 0.004431d + 1.1301 1.25 R(d )320 = 0.004585x + 1.1097 R(d )400 = 0.004658x + 0.9676 R(d )1000 = 0.004747x + 0.8846 0.75 0 50 100 Distance (mm) 150 200 Figure 11. Contact resistance (y-intercept) steadily declines as a result of sanding. 0.3 Contact resistance residual standard deviation Ohms 0.2 0.1 0 0 180 320 Sandpaper grit 400 1000 Figure 12. Residual standard deviation makes a large improvement after first sanding. Atomic Force Microscope After sanding was finished, the surface was analyzed with a Digital Instruments Nanoscope atomic force microscope at three random locations, Figure 13. The scan area was 50 50 mm, the scan rate was 0.3 Hz, and the number of samples was 256. As the micrographs show, sanding does a good job of exposing the fibers, which appear as Downloaded from jcm.sagepub.com at PENNSYLVANIA STATE UNIV on April 8, 2016 1646 N. KWOK AND H. T. HAHN 10 20 30 10 µm 40 x 10.000 µm/div z 4000.000 nm/div 20 30 40 10 µm x 10.000 µm/div z 4000.001 nm/div 20 30 40 µm x 10.000 µm/div z 4000.001 nm/div Figure 13. Image scale is 10 m per division in the x/y directions, and 4 m per division in the z direction. 200 Temperature (C) 150 Alligator at 0.8 A Contact at 0.8 A Contact at 4.0 A 100 50 Electrode 0 0 50 Electrode 100 150 Position (mm) 200 250 Figure 14. Using alligator clips limited total current due to localized heating, while the contact electrode performed much better. smooth cylinders sticking slightly above the surface. This occurs because the fibers are much harder than the matrix, causing the matrix to wear away while the fibers remain intact. Despite this, there are still some areas where the matrix could potentially interfere by sticking slightly above the nearest fiber. This in part explains why a more pliable electrode such as the rubber contacts, or a liquid such as the silver paint, would perform better than a tape or copper sheet. MEASUREMENT OF TEMPERATURE FIELD A DC power supply was used together with an ammeter in series and a voltmeter in parallel to monitor current and voltage (Figure 4). Current was controlled while voltage was left to vary depending on overall resistance. The test was done on the sanded surface of Composite 1. Power was applied for 5 min to allow the sample to reach steady state, and measurements were then made. Another 5 min were allowed to pass before a second measurement, used to verify that the sample had indeed reached steady-state. Figure 14 compares the usage of the alligator clips to the large contact electrode. When using the alligator clips, 0.8 A was the practical current limit because anything Downloaded from jcm.sagepub.com at PENNSYLVANIA STATE UNIV on April 8, 2016 1647 Resistance Heating for Self-healing Composites 2.20 Resistance (ohms) 2.15 Resistance vs temperature at centerpoint 2.10 2.05 2.00 1.95 1.90 20 30 40 50 Temperature (C) 60 70 Figure 15. Resistance vs temperature, measured at midpoint. higher resulted in burning the composite under the electrode. This is evident by the extreme temperature spike in the figure, which actually underreports the true localized temperature because the measurement interval skips over the area directly under the electrode. By contrast, the contact electrode eliminated any noticeable spike while still heating the area between the electrodes. This allowed the current to be raised all the way to 4.0 A without causing burns. Some localized heating still occurs due to contact resistance, but the elevated area between the electrodes is maintained at nearly the same temperature. These temperatures are enough to activate the healing reaction of the thermally mendable polymer. Outside of the test region, the temperature quickly drops to room temperature (24 C) because there is little current flow. RESISTANCE AS A FUNCTION OF TEMPERATURE Figure 15 plots resistance as a function of temperature with the temperature measurement occurring at the centerline and the resistance measured across the full length of the composite. Although the results are somewhat inconsistent, a clear trend of decreasing resistance as temperature increases is noted, indicating the semi-conductor-like behavior of the composite. A total decrease of 9.2% occurred between 23 and 50 C, after which the change appeared to level off. MODELING WITH FEMLAB The temperature field resulting from resistance heating under 4 A current input is predicted using the FEMLAB [5]. All the physical parameters are made as identical to the actual experiment as possible. The contact electrode is modeled as a very thin layer of material with a very high electrical resistivity. This will create a large voltage drop across a small distance and mimic the effect of contact resistance. The composite itself is modeled in four layers using the appropriate thermal and electrical conductivities. Downloaded from jcm.sagepub.com at PENNSYLVANIA STATE UNIV on April 8, 2016 N. KWOK AND H. T. HAHN 1648 Governing Equations The governing field equations for the steady-state heat and electrical conduction are: r ðkrT Þ ¼ Q r ðrrV Þ ¼ 0 ð7Þ ð8Þ where k is the thermal conductivity tensor, T is the temperature, V is the voltage, r is the electrical conductivity tensor, and Q is the resistive heat source. The resistive heat source is given by Joule’s law: Q¼EJ ð9Þ J ¼ E ¼ rV ð10Þ where E is the electric field and J is the current density. The appropriate boundary conditions are taken as: n ðkrTÞ ¼ hðT Tamb Þ þ e B ðT4 T4amb Þ : convection and radiation on surfaces ð11Þ n J ¼ 4 A : current through positive and negative electrode areas V ¼ 0 V : negative electrode area is grounded ð12Þ ð13Þ n J ¼ 0 : all other surfaces electrically insulated ð14Þ Here h is the convective heat transfer coefficient, Tamb is the ambient temperature, e is the emissivity, and B is Boltzmann’s constant. For simplicity the clamps are approximated by 10 mm tall stainless steel cubes with the same footprint as the rubber electrodes (Figure 16). The electrode itself has its own set of material properties and is treated as a separate subdomain from the clamp. In addition, there is also a very thin ‘resistive layer’ that simulates the effects of contact resistance. The electromagnetic subdomains are analogous to the heat transfer subdomains. Each subdomain is treated as homogeneous and there is no internal current generation. The electrical boundary conditions are different from the thermal ones, with all the composite boundaries acting as electrical insulators except where the two electrodes are located. MATERIAL PROPERTIES Thermal The constants used in the analysis are summarized in Table 3. The conductive heat transfer coefficient for the composite in the 0-degree (k0) and 90-degree (k90) directions are taken from James [6], and for the rubber electrode, k2, and stainless steel clamp, k3, from Mills [7]. The type of rubber used was neoprene although the actual composition of the Zoflex conducting rubber is proprietary. The emissivity, e, was measured using the Downloaded from jcm.sagepub.com at PENNSYLVANIA STATE UNIV on April 8, 2016 1649 Resistance Heating for Self-healing Composites Max:6.0 6 6 Boundary: Electric potential 5 Clamp 4 V 3 2 Electrode Resistive layer 1 0 0 Figure 16. Positive electrode top surface boundary condition is I ¼ 4.0 A while negative electrode top surface is V ¼ 0 V, meaning a total of 4 A flows into the positive electrode while the negative electrode serves as a ground. In addition to having special electrical boundary conditions (all other boundaries are electrically insulated), the electrode top surfaces are also thermally conductive rather than convective, because in reality the rubber electrode is attached to a C-clamp (Figure 2). Table 3. Table of constants. Sym Value Units Description k0 k90 k2 k3 h e kA g T 120 2.6 0.19 15.0 11.42 0.9 0.0267 0.0025 15.66 106 9.81 96 W/(m*K) W/(m*K) W/(m*K) W/(m*K) W/(m2*K) L B Tinf Tamb C E 0 90 t 0.021 5.67 108 297 297 2.115 1000 18282 11.53 1.61 m J/(s*m2*K4) K K (-m)1 (-m)1 (-m)1 (-m)1 (-m)1 0-deg thermal conductivity of composite 90-deg thermal conductivity of composite Thermal conductivity of neoprene rubber Thermal conductivity of stainless steel Convective heat transfer coefficient Emissivity Thermal conductivity of air at 300 K Thermal coefficient of volume expansion Kinematic viscosity of air Acceleration of gravity Average temperature difference between air and surface used for convective calculation Width of slab Boltzmann’s constant Ambient temperature for convection Ambient temperature for radiation Calculated effective contact conductivity Electrode conductivity from Zoflex [8] Simulation conductivity 0-deg Simulation conductivity 90-deg Simulation conductivity thickness W/(m*K) K1 m2/s m/s2 K Downloaded from jcm.sagepub.com at PENNSYLVANIA STATE UNIV on April 8, 2016 1650 N. KWOK AND H. T. HAHN infrared thermometer in conjunction with a thermocouple. The infrared thermometer can utilize an adjustable emissivity reading, and this value was adjusted until the readout on the IR thermometer matched the thermocouple readout. The result is consistent with typical dark colored surfaces including other examples of the same material. The ambient temperature for convection and radiation was simply the measured room temperature. The convective heat transfer coefficient h is calculated by treating the sample as a heated horizontal plate facing up undergoing natural convection. It is given by: kA h¼ NuL L NuL ¼ 0:52Ra1=4 L ¼ 0:52 ð15Þ TgL3 2 1=4 ð16Þ This results in a heat transfer coefficient of 11.42 W/m2 K, which is typical for natural convection [7]. Note that the value T has to be found using iteration, using the experimental data as a starting point. Electrical Unidirectional laminate strips were made using the same methods as their bidirectional counterparts and measured for both contact resistance and composite resistivity in all three directions. These measured values were then applied to the individual layers within the simulation, which was for a bidirectional layup. The effective conductivity of the contact interface is found by using the measured contact resistance, and treating the interface as consisting of a very thin layer 0.1 mm thick. The result is: ¼ L 0:0001 1 ¼ ¼ 2:115 RA 0:394 0:012 0:01 -m ð17Þ MODEL RESULTS A 3-D mesh was used as shown in Figure 17. The model geometry statistics and mesh statistics are shown in Tables 4 and 5, respectively. The high scaling factor allowed for two layers of elements in the thickness direction for each composite layer without an excessive number of elements. Once the model was meshed, a non-linear solver was used to achieve 0.02 0.01 0 0.1 0.2 Figure 17. Mesh. Downloaded from jcm.sagepub.com at PENNSYLVANIA STATE UNIV on April 8, 2016 0 1651 Resistance Heating for Self-healing Composites Table 4. Geometry statistics. (mm) Composite layers (4) Length Width Height 255 21 0.17 Electrodes (2) Length Width Height 10 12 0.5 Clamps (2) Length Width Height 10 12 10 Table 5. Mesh statistics. Pre-set resolution Mesh type Degrees of freedom # Mesh elements # Boundary elements # Edge elements Scaling factor z-resolution of composite 0 Extra fine Subdomain 81,216 25,329 6673 1172 1 : 1 : 100 (x, y, z) Two elements per layer 0.1 0 0.2 V 10.45 Figure 18. Potential varies from 0 to 10.45 V at the negative and positive electrodes. a steady-state solution for both voltage and temperature. The program automatically iterates until it can converge on a solution that is not time-dependent. Figure 18 is a plot of potential over the surface of the composite. A large drop in voltage is observed between the top and bottom surface of the contact interface which is a result of its very low conductivity and represents contact resistance. A more gradual drop in voltage occurs along the length of the specimen and again another large drop occurs on the contact interface layer. The temperature plot in Figure 19 shows the effects of resistive heating. There is a high degree of localized heating around the electrodes, a lower area of heating between the electrodes, and less heating in the end regions outside of the electrodes. The analysis is revealing in that it allows the temperature directly on the electrode surface to be seen, whereas in reality this area is obscured by the C-clamp (in the picture the clamp is also blocking the view of the surface; however the data plots of temperature are recorded under the clamp). Temperatures in all locations were higher than measured values around Downloaded from jcm.sagepub.com at PENNSYLVANIA STATE UNIV on April 8, 2016 1652 N. KWOK AND H. T. HAHN 0 0.1 0.2 T(C) 117 237 Figure 19. Temperature varies from 117 to 237 C. 250 Temperature (C) 200 150 100 Contact at 4.0 A 50 FEMLab Electrode Electrode 0 0 50 100 150 Position (mm) 200 250 Figure 20. The FEMLab simulation predicts higher heating than measured. 0 0.1 0 0.2 V 10.45 Figure 21. View of electric current lines in the x–y plane. the electrodes. The plot in Figure 20 compares the measured values to those predicted from FEMLab. As shown by the plot, the simulation predicts higher temperatures than observed experimentally. Higher temperatures near the edges of the composite indicate that thermal conductivity for this specimen is actually lower than the sample used in the literature. Overall temperatures are also higher because the actual resistivity is lower than simulated, indicating that there is some interaction between layers to improve the resistivity of the middle layers when arranged in a cross-ply layup. The electric current density is plotted in Figure 21. This illustrates the paths that the current takes going from the positive to the negative electrode. A close-up of the current density around the positive electrode (Figure 22) in the x–z plane shows the effects of anisotropy in the model. Since the conductivity for the middle layers is low in the x-direction compared to the top and bottom layers, the current lines tend to jump through the middle layers to get to the bottom layer before traveling in the x-direction. Thus, most of the current flow is found in the top and bottom layers. Downloaded from jcm.sagepub.com at PENNSYLVANIA STATE UNIV on April 8, 2016 Resistance Heating for Self-healing Composites 1653 Figure 22. Close-up view of current lines in the x–z plane reveals the effects of anisotropy. CONCLUSIONS The unique properties of carbon fiber composites require special consideration of contact resistance in any resistive heating application. The two keys to achieving low contact resistance are removal of any resin rich top layers that may interfere with fiber contact, and an electrode with a large surface area in pressure contact with exposed fibers. A challenge lies ahead in reducing contact resistance as much as possible while creating a removable electrode system that works on the composite surface. To this end, the C-clamp electrode is a step in the right direction, having demonstrated to significantly reduce localized heating. However, no matter how good the electrode connection is, it will still be limited by the resin-rich top layer present in all composites. Using conventional resins, the only way to overcome this is to remove the top resin layer, exposing the fibers below. As the data shows, doing so not only greatly reduces contact resistance, but also improves the consistency of the measurements. Another alternative to consider is a conducting resin, although these remain largely experimental. The simulation using FEMLab provides a good approximation of the heating behavior and the same parameters can be applied in the future to more complex geometries. This is particularly useful in predicting temperatures in areas unavailable for measurement, such as underneath the electrode. It is also useful for testing voltages and temperature levels that would normally be unsafe or damaging to the composite, allowing problems to be averted without resorting to destructive testing. Most importantly, the results of these tests are applicable to the self-healing polymer described in the introduction. The simulation can determine beforehand the required current levels and appropriate electrode configuration to achieve the desired temperature at a crack location, in order to effectively heal matrix cracks. ACKNOWLEDGMENTS The present paper is based on work supported by the Air Force Office of Scientific Research through a MURI Grant FA 9550-05-1-0346 to the University of Illinois, Urbana-Champaign. Appreciation is extended to Dr B. Les Lee for his program management. REFERENCES 1. Chen, X., Wudl, F., Mal, A., Shen, H. and Nutt, S. (2003). New Thermally Remendable Highly Cross-Linked Polymeric Materials, Macromolecules, 36(6): 1802 –1807. 2. Yarlagadda, S. and Kim, H. (2002). A Study on the Induction Heating of Conductive Fiber Reinforced Composites, Journal of Composite Materials, 36(4): 401–421. Downloaded from jcm.sagepub.com at PENNSYLVANIA STATE UNIV on April 8, 2016 1654 N. KWOK AND H. T. HAHN 3. Abry, J., Bochard, S., Chateauminois, A., Salvia, M. and Girau, G. (1999). In situ Detection of Damage in CFRP laminates by Electrical Resistance Measurements, Composites Science and Technology, 59(6): 925–935. 4. Todoroki, A., Tanaka, M. and Shimamura, Y. (2003). High Performance Estimations of Delamination of Graphite/Epoxy Laminates With Electric Resistance Change Method, Composites Science and Technology, 63(13): 1911–1920. 5. FEMLab 3.0 Users Manual (2004). COMSOL Inc., Burlington, MA. 6. James, B., Wostenholm, G., Keen, G. and McIvor, S. (1987). Prediction and Measurement of the Thermal Conductivity of Composite Materials, J. Phys. D: Appl. Phys., 20(3): 261–268. 7. Mills, A. (1999). Basic Heat and Mass Transfer, 2nd edn, Prentice Hall, New Jersey, p. 297. 8. Zoflex Conducting Rubber Datasheet, http://www.irmicrolink.com/zoflexcd45_1.pdf Downloaded from jcm.sagepub.com at PENNSYLVANIA STATE UNIV on April 8, 2016
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