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From Materials Evaluation, Vol. 70, No. 3, pp: 367377. Copyright 2012 The American Society for Nondestructive Testing, Inc.

Detection of Discontinuities in Carbon-carbon Composites using X-ray Compton Backscatter Radiography: Radiography by Selective Detection
by Ching-Tang Bill Liu*, Min-Jui Huang*, Yicheng Peter Pan, Daniel Shedlock and Tsuchin Philip Chu

ABSTRACT

There has been an increase in the use of nondestructive testing techniques to detect discontinuities in carbon-carbon (C/C) composite materials. A type of X-ray Compton backscatter radiography, radiography by selective detection (RSD) is a proven technology that has been successfully tested on a wide variety of materials and applications. For example, RSD has been used for inspection of the spray-on foam insulation on the external tank of the space shuttles 2005 return to flight. This paper evaluates the effectiveness of RSD to identify discontinuities on C/C composites. Experimental results obtained in different simulated discontinuity conditions are reported. These results are compared with findings given by infrared thermography. The RSD technique is capable of evaluating discontinuities in C/C composite materials with results comparable to, or better than, infrared thermography. With some application specific optimization, the RSD technique will be efficient and easy to implement. Additionally, rapid assessment of detecting discontinuities in C/C materials can be achieved in manufacturing process quality control systems. KEYWORDS: X-ray Compton backscatter radiography, radiography by selective detection, carboncarbon composites, infrared thermography.
* National Chung Hsing University, Department of Mechanical Engineering, 250 Kuo Kuang Rd., Taichung 402, Taiwan R.O.C.; 886-422851951; fax 886-04-22877170; e-mail liubill@ms6.hinet.net. Therm-O-Disc, Inc., Emerson, 1320 South Main St., Mansfield, Ohio 44907. Nucsafe, Inc., 601 Oak Ridge Turnpike, Oak Ridge, Tennessee 37830. Southern Illinois University Carbondale, Department of Mechanical Engineering and Energy Process, 1230 Lincoln Dr., Carbondale, Illinois 62901.

Introduction Carbon-carbon (C/C) composites are widely used in many industries because of their material and thermal properties. These properties include: low density, low coefficient of thermal expansion, high heat capability and good wear resistance. The strength of the material can actually increase with increasing temperatures, making C/C composites the premier material for friction disks in aircraft brake applications. In particular, 63% by volume of the C/C composites produced in the world are used for aircraft braking systems. Other applications include aircraft clutches, rocket motors, heat shields for re-entry vehicles and refractory components. The two primary advantages of C/C composites are heat capacity (2.5 times greater than that of steel) and high strength at elevated temperatures (twice that of steel). Compared to steel brakes, the weight of C/C brakes is lighter by approximately 40%, and the service life of C/C brakes is twice as long (Savage, 2003). The manufacturing process for C/C composite disk brakes is relatively complex and tedious compared to other carbon-based material processes because of the multiple steps involved in the carbonization and densification cycle that improves the density and thermal conductivity of the material (Fitzer and Weiss, 1987). In one manufacturing approach, the C/C composite disk brakes are first made by producing a pre-form from either one of the two different carbon fibers (polyacrylonitrile-based or pitch-based), which is placed in a pre-form and carbonized to create the desired shape, and then densified by a chemical vapor infiltration (CVI) process (Fitzer and Weiss, 1987; Savage, 2003). Pre-forms made with thermosetting resins as matrix precursor processes have low density (0.00155 to 0.00175 g/mm3). Pre-forms of the carbon fibers can be random, organized and even stitched to obtain the desired characteristics needed for the C/C composites application. In other words, the purpose of the CVI process is to infiltrate hydrocarbon gases into the pores and inter-filamentary spaces and then crack. The CVI process is carried out on the C/C composites at high temperatures near 1273.2 K (1000 C) for approximately 5 to 6 days, causing the composites to become denser. Densification is repeatedly carried out until a desired density (0.0018 to 0.002 g/mm3) of the C/C composite disk brake is reached. The C/C composite material will reach a point where the
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matrix is so impervious to the vapor that no more carbon can be deposited on the fibers. Over-crusting and pore blockage can occur during the CVI process due to pressure gradient; therefore, surfaces need to be machined in between densification processes. Using the CVI process to obtain the desired density is time consuming, taking upwards of 1000 h (Ko and Hone, 1992). After material properties of the C/C composites are met, the piece will be machined to the final dimensions and heat-treated if high thermal properties are desired. Heat treatment can increase the thermal diffusivity and thermal conductivity of C/C composite disk brakes, as the carbon molecules are allowed to arrange in a manner that changes the characteristics of the thermal properties. Heat treatment can range from 1873.2 to 2773.2 K (1600 to 2500 C), and the higher the temperature, the larger the thermal conductivity and diffusivity values can be obtained. In general, the total manufacturing process time is six months. Discontinuities in the C/C composite materials can be detrimental, causing structural degradation and thermal irregularities. Discontinuities of carbon disk brakes typically consist of delaminations, voids, inclusions, porosity and impact damage. To ensure safety and reliability right after the production process, nondestructive testing (NDT) techniques are needed for inspection of C/C composite disk brakes (Pan et al., 2009). For this reason, this research has used X-ray backscatter radiography by selective detection (RSD) to characterize commercial C/C composite aircraft brake disks. The results obtained by means of RSD were compared with results obtained by infrared thermography testing.
X-ray Compton Backscatter Radiography Compton backscatter radiography (CBR) is an NDT technique that utilizes penetrating X-ray or gamma ray radiation, commonly referred to as Compton backscatter imaging (CBI). CBI, or X-ray, is a common test performed in the external tank thermal foam insulation of space shuttles. In contrast to transmission X-ray imaging systems where inspected objects must pass between source and detector, CBI allows both the illuminating source, as well as the X-ray detector, to be on the same side of the target object, enabling the inspection to occur rapidly and in a wide variety of spaceconstrained situations (Dinca et al., 2008). This research uses RSD, a particular variant of conventional X-ray CBI first applied at the University of Florida for the detection of buried landmines. The landmine testing results demonstrated the ability of this technique to detect voids and air spaces, which are the most common discontinuities in C/C composite materials (Shedlock et al., 2005). RSD is based on moving the X-ray source in the transverse direction to the illuminating collimated X-ray beam, similar to ultrasonic C-scan. RSD is sensitive to scattering to absorption ratio (electron density) variations in the photon transit path. This allows the detection of discontinuities inside the material from the accessible
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outside surface (Dugan et al., 2004; Jacobs et al., 2002; Shedlock et al., 2005). In general, RSD, which is the most effective type of CBI, employs selective detection of scattered field velocity components (RSD) using specially designed X-ray beam collimators, detectors and detector collimators to obtain high-contrast X-ray backscatter images. RSD is based on image contrast generated by the scatter of probe X-ray radiation in the direction transverse to the illumination radiation beam. Because RSD is sensitive to electron density variations in these directions, thin, but large density variations, such as cracks and delaminations, generate signal-to-background ratios sufficient to produce images of features that are not even detectable in the usually interrogated thin dimension (Dugan et al., 2004). This research used uncollimated detectors, leaving the collimation optimization for future work. The particular configuration employed to acquire the images presented herein is illustrated in Figure 1.

X-ray tube X-rays Collimator Detector Collimated X-ray beam Detector Backscatter X-rays

Testing sample Test platform

Figure 1. Simplified schematic of radiography by selective detection experimental setup.

Experimental Techniques

The material used in this study was a 3D ex-polyacrylonitrile felt needle stitched in the Z-direction, CVI infiltrated and non-heat treated C/C composite disk brake material. These samples had a density of 0.001516 g/mm3. Sets of simulated discontinuities were produced by drilling flat-bottom holes and side-drilled holes to various depths from the surface, as well as various diameters. RSD and infrared thermography tests were conducted on all samples. These simulated discontinuities will help to better explain the limitations of the RSD and infrared thermography technique as a means of detecting subsurface discontinuities in C/C composite materials. The two sets of holes tested were as follows: G Blind flat-bottom holes: the depth at which these discontinuities occur has a crucial influence on the detection capability

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Figure 2. Carbon-carbon sample blind flat-bottom hole discontinuity mapping: (a) 1.588 mm diameter discontinuity; (b) 3.175 mm diameter discontinuity; (c) 6.35 mm diameter discontinuity.

from the surface. The sets of simulated discontinuities were produced by drilling blind flat-bottom holes to various depths from the surface with various diameters. Figure 2 shows the mapping of each of the sample discontinuities drilled into the C/C disk brake, along with their associated diameters and depths. Figure 2a shows 1.588 mm diameter at 0.5, 1 and 2 mm deep. Figure 2b shows 3.175 mm diameter. Figure 2c shows 6.35 mm diameter at 3, 5 and 10 mm deep. Figures 2ac were a portion of the blind hole discontinuity samples to provide a better idea of the capabilities of the camera for small discontinuities and comparison between the two systems. This figure has been divided into three sections so that the schematic can display the diameter and depths of each of the discontinuities created in the non-heat treated C/C disk brake. Since three 6.35 mm discontinuities were already created in another sample at depths of 0.5, 1 and 2 mm, this sample continued with 3, 5 and 10 mm depths to determine the limits of the infrared camera. In Figure 2 the left image is the actual picture of the drilled discontinuities in the C/C disk brake; the right image is a schematic of the depth and location of each of the drilled discontinuities in the C/C disk sample. Blind side-drilled holes: the second set of tests using the RSD and infrared thermography techniques involved creating sidedrilled hole discontinuities, or discontinuities that are drilled from the sides of the C/C samples and cannot be viewed from either the front or back. Three sets of the same C/C composite samples had side hole discontinuities drilled into them at varying depths and sizes. Figures 3ac are schematics of the three C/C samples used and the location and size of the side hole discontinuities drilled into them. Figure 3a shows the mapping of the side-drilled hole discontinuities

with a 12.7 mm diameter hole drilled from the side. The discontinuities were measured from the top edge of the drilled discontinuity to the top surface of the C/C composite material. The different depths ranged from approximately 0.5 to 7 mm deep in increments of 1 mm, and were drilled halfway into the sample from both sides. Figure 3b shows the mapping of the side-drilled hole discontinuities with a 3.175 mm diameter hole. The different depths ranged from approximately 0.5 to 5 mm deep in increments of 1 mm, and were drilled halfway into the sample from both sides. Finally, Figure 3c shows the mapping of the side-drilled hole discontinuities with a 1.588 mm diameter hole. The different depths ranged from approximately 0.5 to 4 mm deep in increments of 1 mm, and were drilled halfway into the sample from both sides.
Experimental Setup for the Radiography by Selective Detection System

The RSD system of this research included an X-ray generator with articulating collimator; two X-ray detector panels with embedded data acquisition; a computer and display; digital control electric motors to provide articulation and positioning for the X-Y scan table; and an electric power generator, all mounted on a suitable rack mount cart. Communication and control of all system components was over Ethernet. The experimental setup for the RSD system is shown as Figure 4. The forced air-cooled version of the X-ray generator provided an excellent source from the standpoint of performance, size and weight. The generator had a maximum X-ray spectrum energy of 160 kVp and a maximum power level of 3000 W. The X-ray tube was unipolar with a 0.4 and 1.0 mm focal spot according to EN 12543 (CEN, 2011). The X-ray tube had an 800 and 1800 W
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continuous rating for the small and large focal spot, respectively. The optimum X-ray source energy for the detection of C/C composite materials is in the range of 65 to 130 kVp. A pixel of 1 1 mm provided good resolution for inspection of the simulated discontinuities; however, resolution down to 0.1 mm is currently available. The motion profile was fixed head gantry and

the distance to the target was 100 mm. The image acquisition time varied depending on the sample size. For this research, the X-ray generator was run at 100 kVp and 6 mA with a small filament, that is, an electric power of 600 W. For the scan speed setting, pixel dwell time was 8.3 ms, exposure time per pixel was 83.3 s and scan velocity was 720 mm/s.

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(c) Figure 3. Carbon-carbon sample blind side-drilled hole discontinuity mapping: (a) 12.7 mm diameter discontinuity; (b) 3.175 mm diameter discontinuity; (c) 1.588 mm diameter discontinuity.

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Figure 4. Experimental setup for radiography by selective detection.

Experimental Setup for the Infrared Thermography System

The first infrared thermography system used in the experiments was an infrared camera with a resolution of 0.06 K at 303.15 K (0.06 C at 30 C), a measurement accuracy of 2 K (2 C) of reading, and 320 240 dpi. The thermal image infrared camera unit incorporated a grayscale image viewing screen as well as a colored viewing screen for more refined and sharper imaging. The infrared camera was linked to a computer, which used the commercial thermal image processing software that came with the infrared camera. This software allowed for even further rendering and processing of the images. The software could record in real time and create video recordings or take snapshots as the sample was heated. A model of the test setup is shown in Figure 5a. The second infrared thermography system used in the experiments was a commercial turnkey infrared thermography system. It also used two xenon flash tubes to flash the surface of the sample. The second infrared thermography system incorporated postprocessing programs to further render the infrared images. The following shows the experimental setup for the modified flash and traditional flash systems, respectively. G Modified flash system: the first infrared thermography system used a modified flash thermography technique to test the C/C material. The outside edges of the samples were well insulated by the thermal foam insulators. In these experiments, an infrared camera was used, as shown in Figure 5b. The four linear halogen bulbs were used as the flash source. The halogen bulbs were turned on and left on until they reached steady state conditions (no more temperature increase); the hood had a shutter that blocked the light from escaping the hood, preventing any heat loss. When the sample was positioned in front of the hood, the shutter was open for approximately 3 to 5 s. The infrared camera recorded the thermal response of the C/C composite samples every 0.25 s for determination of discontinuities. Figure 5b shows photos of the actual setup for the first infrared thermography system.

Traditional flash system: the second infrared thermography system used a traditional flash thermography system to conduct testing on the C/C samples. The hood was positioned upright to view the samples. The heat flux was applied to the surface of the sample and the infrared camera recorded the thermal response of the same surface, similar to the first infrared thermography system setup. This system was a traditional flash thermography system that used two xenon flash tubes to supply a heat burst to the surface of the C/C for a duration of 4 to 10 ms. Both the side-drilled hole discontinuities and the blind flat-bottom hole discontinuities were tested using a flash heating infrared thermography system. The system setup can be seen in Figure 5c. The first and second derivative is image reconstruction to allow deeper and clearer discontinuity detection from the thermal images.

Results and Discussion In the simulated discontinuity inspection, four inspections (Inspection 1, Inspection 2, Inspection 3 and Inspection 4) were conducted for non-heat treated CVI C/C samples. These inspections tested various diameter flat-bottom hole discontinuities and side-drilled hole discontinuities at various depths to more closely resemble real discontinuities within the C/C composite material. Inspection 1 was tested with multiple blind flat-bottom hole discontinuity sizes and depths. In Inspection 2, one sample was tested with a discontinuity diameter of 12.7 mm at various depths and can be seen in Figure 3a of the mapping section. Inspection 3 was tested with a discontinuity diameter of 3.175 mm and can be seen in Figure 3b of the mapping section. The final test, Inspection 4, had only one sample with a discontinuity diameter of 1.58 mm and can be seen in Figure 3c of the mapping section. The results from the RSD and infrared thermography systems show differences in discontinuity detection. The RSD system can simply and undoubtedly define the size, shape and location of all simulated discontinuities in the thicker C/C composite materials. The second infrared thermography system using the
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post-processing program can more clearly define the partial simulated discontinuities in the thicker C/C composite material. The first infrared thermography system, using the raw infrared files can comparably detect fewer large simulated discontinuities in the same C/C composite material with less thermal contrast due to the use of the raw infrared images. Figure 6 shows the comparison between RSD and infrared thermography systems in detection of discontinuities in the C/C composite. When comparing the results for the blind flat-bottom hole discontinuities tested for various depths from the surface with varying diameters, the RSD system performed significantly better than infrared thermography. The spatial detection resolution of the sample was 1 mm/pixel, which could be used to calculate the diameter of discontinuities. This error is associated with the resolutions of inspection, which could be more accurate if the resolutions of inspection decreased to 0.1 mm. However, in regards to infrared thermography systems, results showed that they are capable of detecting partial simulated discontinuities for

the 1.588 mm diameter at 0.5 mm deep, 1.588 mm diameter at 1 mm deep, 3.175 mm diameter at 0.5 mm deep, 3.175 mm diameter at 1 mm deep, and 6.35 mm diameter at 3 mm deep. Figure 6 also shows a comparison of the results for the side-drilled hole discontinuities tested. Again, the results in the RSD system were better than in the infrared thermography system. The RSD system can easily outline the size, shape and location of all simulated side-drilled hole discontinuities. However, discontinuity detection of infrared thermography systems is still comparable with the depth and diameter of discontinuities detected. The results for the 12.7 mm diameter side-drilled hole discontinuity show that the RSD system is capable of detecting this diameter discontinuity at a maximum depth of 13 mm and the calculated dimension of discontinuities is 13 38 mm, which is in good agreement with actual discontinuity size. This is 8 mm deeper than Southern Illinois University at Carbondales current setup. It also shows the RSD system results for the 3.175 mm

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Figure 5. Experimental setup for the infrared thermography systems: (a) a typical transient thermography system; (b) experimental setup for the first infrared thermography system; (c) experimental setup for the second infrared thermography system.

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Figure 6. Comparison between Compton backscatter radiography (CBR) and infrared thermography: (a) radiography by selective detection system (CBR Image); (b) first infrared thermography system (raw image); (c) second infrared thermography system (second derivative).

diameter discontinuity and is capable of detecting all simulated side-drilled hole discontinuities. The calculated discontinuity dimensions were 4 15 mm, which is in good agreement with actual discontinuity size. The results for the 1.588 mm diameter side-drilled hole discontinuity show that the RSD system is capable of detecting all simulated sidedrilled hole discontinuities and calculating dimensions of

discontinuities of 2 11 mm, which are in agreement with actual discontinuity size. In infrared thermography systems, the results show its capability of detecting simulated discontinuities only down to 3 mm deep. The 3D surface plots of comparison between RSD and infrared thermography in simulated discontinuities are shown in Figures 7 and 8. As Figure 7a indicates, the

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Figure 7. Comparison of flat-bottom hole discontinuities 3D surface plot between radiography by selective detection (RSD) and infrared thermography: (a) RSD system; (b) first infrared thermography system; (c) second infrared thermography system.

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RSD image had a better signal-to-noise ratio and capabilities to define the size, shape and location of all simulated flat-bottom hole discontinuities. Infrared thermography raw images had more noise to interfere in discontinuity evaluation, as demonstrated in Figure 7b. An advanced data processing algorithm (second derivative technique) used for enhancement of signal-to-noise ratio of thermal images is illustrated in Figure 7c. Similarly, the 3D surface plots in the side-drilled hole discontinuities at 12.7, 3.175 and 1.58 mm diameter are displayed in Figure 8. Again, the RSD system detected all simulated side-drilled hole discontinuities and pointed out the exact location and size of the discontinuities. The ability for the infrared thermography to detect the discontinuities in these samples became increasingly difficult the further the discontinuity went into the samples and the smaller the diameter became. Although the second derivative technique enhanced the signal-to-noise ratio of the images, the second derivative technique only implies the apparent location of the discontinuities by temperature gradient variation. Figures 9 and 10 show the image line profiles for the multiple flat-bottom hole discontinuities and side-drilled hole discontinuities at 12.7, 3.175 and 1.58 mm diameter. The blue line is the RSD system, the red line is the first infrared thermography system and the green line is the

second infrared thermography system. The graph in Figure 10a shows two different line profiles of gray level intensity for flat-bottom hole discontinuities. The spatial resolution of the sample was found to be 0.375 mm/pixel. With this information, the discontinuity diameter can be determined for the samples tested. The RSD system calculated diameters of discontinuities are 2, 4 and 7 mm in the left side picture of Figure 9a and calculated diameters of discontinuities are all 7 mm in the right side picture of Figure 9a, which follow the true diameters. For the infrared thermography system, partial discontinuities could be distinguished and located, but it was more difficult to determine the size of the discontinuity. Figure 9b shows the line profile for the side-drilled 12.7 mm diameter discontinuity. The line profile of the RSD system pointed out all discontinuities, and the calculated diameters of the discontinuities were all 13 mm. The line profile of the infrared thermography raw image only distinguished partial discontinuities down to 4 mm deep. Using the second derivative technique, the discontinuity detection could be down to 5 mm deep. Figures 10a and 10b show the line profiles for the drilled 3.175 and 1.58 mm diameter discontinuities. The spatial resolution of the sample was found to be 0.46 mm/pixel. The graphs in Figures 9 and 10 indicated that the RSD system could detect all discontinuities. These discontinuities could be

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Figure 8. Comparison of side-drilled hole discontinuities 3D surface plot between radiography by selective detection (RSD) and infrared thermography: (a) RSD system; (b) first infrared thermography system; (c) second infrared thermography system.

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distinguished and located, but it was more difficult to determine the size of the discontinuity. Unexpectedly, the infrared thermography system could barely make out all discontinuities due to their known locations, but some discontinuities were not displayed by a bright white spot on the infrared thermography image; rather it was found by using the line profile over the area. This error is associated with the limitations of the camera. The infrared camera had difficulties observing the thermal gradients of

increasingly smaller discontinuity diameters in the non-heat treated C/C samples. In summary, the detection capability of the infrared thermography system will significantly decrease when detection depths increase, and the infrared thermography system can only detect depths in C/C composites up to 5 mm. However the RSD system could easily and clearly define all simulated discontinuity dimensions and locations in the thicker C/C composite materials up to 13 mm.

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Figure 9. Comparison of discontinuities 2D profile plot between radiography by selective detection (RSD) and infrared thermography: (a) comparison of flat-bottom hole discontinuities; (b) comparison diagram of 12.7 mm side-drilled hole discontinuities.

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Figure 10. Comparison of discontinuities 2D profile plot between radiography by selective detection (RSD) and infrared thermography: (a) comparison diagram of 3.175 mm side-drilled hole discontinuities; (b) comparison diagram of 1.58 mm side-drilled hole discontinuities.

Conclusion Non-heat treated CVI C/C composite materials were scanned and extensively evaluated using RSD 1D line profiles, 2D images and 3D surface analysis. The RSD system could simply and obviously define all simulated discontinuities dimension and location in the thicker C/C composite materials. The results validate the RSD variant of an X-ray CBR system as a quantitative tool for the
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determination of simulated discontinuities of C/C composite material, sensitive enough to distinguish the discontinuity area and size. It was shown that discontinuities with diameters of 12.7 mm could be accurately detected at depths of up to 13 mm from the surface. Discontinuities with diameters of approximately 3.175 mm could be accurately detected at depths of approximately 5 mm and less, and discontinuities with diameters of approximately 1.578 mm

could be accurately detected at depths less than 4 mm. The sample was analyzed by means of two infrared thermography systems, which only allowed the detection of partial simulated discontinuities. It was shown that discontinuities with diameters of 12.7 mm could be detected at depths of up to 3 mm from the surface. Discontinuities with diameters of approximately 3.175 mm could be detected at depths of approximately 2 mm deep, and discontinuities with diameters of approximately 1.578 mm could be detected at depths less than 1 mm. Discontinuities smaller than 1.578 mm in diameter are increasingly difficult to detect due to the amount of temperature variation that is associated with the size and resolution of the camera being used to conduct the experiments. An infrared thermography system is only suitable for shallow discontinuity detection. It can be concluded that the RSD variant of an X-ray CBR analysis presents the most reliable and advantageous technique to be used in deep discontinuity detection for C/C composite materials.
ACKNOWLEDGMENTS

The authors thank the Center for Advanced Friction Studies (CAFS) of Southern Illinois University Carbondale and all of the CAFS industrial sponsors for their support and for acting as technical monitors on this research.
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