Mechanical Properties of Silicon Carbide Micro-Fibers Alexander J. a Wirtz , Brian J. b Jaques , aThe College of Idaho, bBoise State University Experimental Procedure Silicon carbide (SiC) fibers have many notable properties such as low density, high elastic modulus, and high temperature mechanical strength. Such properties make these fibers desirable in engineering products such as aerospace heat-resistant tiles, fiber optics communications, and semiconductor electronics. These fiber were investigated as various processing speeds to increase the carbon to silicon carbide conversion may have effects on mechanical properties. Laser diffraction was used to measure the diameter of each fiber to accurately determine the mechanical properties of the processed fibers. Fracture strength and Young’s modulus were found and evaluated using Weibull statistics relative to processing parameters of the fibers. Background Creation Process: Carbon fiber tows were heat treated in a siliconcontaining gas at different processing speeds to increase the amount of conversion from carbon to silicon carbide. The effects of the processing speeds on the mechanical properties should affect the silicon carbide conversion, and thus, the mechanical properties of the fiber. [3] Laser Diffraction Benefits and Theory: Rapid measurement: 2 minutes per sample Accuracy: ± 0.1 μm [5] Cost: << SEM and other forms of microscopy Bragg’s Law (Equation 1), along with Babinet’s Principle, can be applied to determine the diameter (𝑎) of a carbon and/or silicon carbide fiber because the diffraction pattern of light around a small fiber mimics the single-slit experiment, with the exception of the light intensity [2] [4] (Figure 1). Variables in Equation 1 are defined in Figure 3. Figure 1 Analogous to Mechanical Properties: Fiber Preparation: Figure 2b Figure 2a Results 0.2μm/sec ACF LLC. provided four different samples for characterization: • No Heat Treatment • 5 in/min • 3 in/min • 1 in/min Precise cardstock test frames were fabricated using a CNC laser to provide a 1 inch gauge length Individual fibers were fixed to the test frames with cement and a secondary frame was fixed on top of the fiber to provide a more rigid test fixture (Figure 2a). The completed frames were cured for 24 hours before any further testing. Laser Diffraction: Laser diffraction was conducted with a 5 mW heliumneon laser system. Images of the diffracted laser nodes were captured and spacing was measured (similar to Figures 3 - 4) Calculations were performed using Bragg’s Law in Equation 1 (variables defined in Figure 3) The diameters measured from diffraction testing are shown in Table 1. 𝐿𝑖𝑔ℎ𝑡 𝐼𝑛𝑡𝑒𝑛𝑠𝑖𝑡𝑦 𝐬𝐢𝐧 Fiber Set Table 1 No H.T. 5 in/min 3 in/min 1 in/min Average Diameter (μm) 7.1 7.2 7.5 7.2 m2 = 0.9 𝑛=2 ∆𝑍 2 𝐿 m2 = 1.8 -2 -3 𝜃 -4 m1 = 3.9 m = 3.7 m1 = 6.9 -5 𝑆𝑖𝐶 𝐹𝑖𝑏𝑒𝑟 -2.5 -2.0 -1.5 -1.0 -0.5 λ = 632.8 𝑛𝑚 a) No H.T. fracture surface b) No H.T. fiber surface c) 5 in/min fiber tow d) 3 in/min fracture surfaces a b c d Figure 3 Each test frame was mounted in a Shimadzu mechanical testing system (Figure 6). The frame sides were cut to isolate the fiber to the applied tension (Figure 2b). Mechanical testing: 10 N load cell Strain rate of 0.2 μm/sec Young’s modulus (E) and fracture strength (σf) were calculated for each fiber. An example stress vs. strain graph for 3 in/min fibers is shown in Figure 5. Sample 3 Sample 8 Sample 15 Sample 12 Sample 23 0.5 1.0 1.5 2.0 Conclusions: SEM Fractography and Imaging: 𝐻𝑒𝑁𝑒 𝐿𝑎𝑠𝑒𝑟 0.0 ln(σf) Figure 7 Mechanical Testing: 1.5 m2 = 1.2 No H.T. 1 in/min 3 in/min 5 in/min m1 = 9.4 Standard Deviation (μm) ±0.4 ±0.4 ±0.3 ±0.3 Table 2 -1 Figure 4 Stress (GPa) Equation 1 3.5 ± 0.9 1.6 ± 0.9 1.4 ± 0.7 0.5 ± 0.5 𝑛=1 Weibull modulus for each fiber type was found and can be used to better understand fracture mechanisms and to predict failure probability. Treated fibers show two Weibull moduli which represent two distinct flaws causing failure. Initial Weibull moduli (m1) increase as the processing speed decreases. A sample size of 30 produced a below average Weibull distribution with low confidence. An increased sample size (for each distinct flaw) is recommended for more reliable data. [1] Both fracture strengths and Young’s moduli decrease as processing speeds decrease (more C-SiC conversion), which is expected when compared to literature. [3] [6] References 1. 2. 3. 4. 1 5. ∆𝒁 𝟐𝑳 240 ± 57 210 ± 35 220 ± 23 190 ± 37 1 𝒏𝝀 𝒕𝒂𝒏−𝟏 No H.T. (n=30) 5 in/min (n=30) 3 in/min (n=30) 1 in/min (n=30) 2 Diameter Results SiC Fiber 𝒂= Fracture Strength (GPa) Table 1 2 𝒂𝒔𝒊𝒏𝜽 = 𝒏𝝀 Young’s Modulus (GPa) Weibull statistics (Figure 7) were used to determine the Weibull modulus (m) by plotting a linear relationship between fracture strength (σf) and probability of survival (Ps). [1] 2.5 Single Slit Fiber Set SiC Fracture Analysis: Weibull Statistics lnln(1/Ps) Abstract and Darryl P. b Butt 0.5 6. Carter, C. Barry, Norton, M. Grant. 2007. Ceramic Materials: Science and Engineering. Pg. 302-305. New York: Springer Science, Business Media, LLC. Halliday, David, Resnick, Robert, Walker, Jearl. (2001). Fundamentals of Physics. Sixth Edition, Pg. 893-896. New York: John Wiley & Sons, Inc. Hinoki, Tatsuya, Lara-Curzio, Edgar, Snead, Lance L. (2001). Mechanical Properties of High Purity SiC Fiber-Reinforced CVI-SiC Matrix Composites. Metals and Ceramics Division, Oak Ridge National Laboratory, Oak Ridge, TN37831. Li, Chi-Tang, Tietz, James V. (1990). Improved accuracy of the laser diffraction technique for diameter measurement of small fibers. Journal of Materials Science, 25, 4694-4698. Meretz, S., Linke, T., Schulz, E., Hampe, A., Hentschel, M. (1992). Diameter measurement of small fibers: laser diffraction and scanning electron microscopy technique results do not differ systematically. Journal of Materials Science Letters, 11, 1471-1472. Summerscales, John. (2014). Composites Design and Manufacture: Reinforcement Fibers. ACMC University of Plymouth, Plymouth University, Plymouth. Acknowledgements 0 0 0.2 0.4 0.6 Strain (%) 0.8 1 Figure 5 1.2 Figure 6 This research was made possible by Boise State University and the National Science Foundation’s Research Experiences for Undergraduates (REU) Program Award DMR-1359344. Special thanks to: Advanced Ceramic Fibers, LLC, Materials in Energy and Sustainability REU/RET Director Rick Ubic, and the Advanced Materials Laboratory research group.