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Inter Metallic Matrix Reinforcement Ceramic Fibers by Chemical Vapor Deposition

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Inter Metallic Matrix Reinforcement Ceramic Fibers by Chemical Vapor Deposition High Temperature Materials and Processes, VoL 10, No. 1,1991 Inter metallic Matrix Reinforcement Ceramic Fibers by Chemical Vapor Deposition V. Revankar and V. Hlavacek Ceramic and Reaction Engineering Laboratory, State University of New York at Buffalo, Buffalo, New York 14260, USA CONTENTS Page ABSTRACT 44 1. TECHNICAL BACKGROUND 44 2. EXPERIMENTAL PROCEDURE 44 3. RESULTS AND DISCUSSION 45 3.1. Titanium Diboride Fiber 45 3.2. Boron Carbide and Titanium Carbide Fibers 50 4. SUMMARY 50 5. CONCLUSIONS 54 ACKNOWLEDGEMENTS 54 REFERENCES 54 43 Vol 10, No. 1,1991 Intermetaläc Matrix Reinforcement Ceramic Fibers by Chemical Vapor Deposition impurities in a fiber (e.g., calcium) result in a fast high- ABSTRACT temperature degradation 151. Titanium diboride, titanium carbide, boron carbide and The achievement of consistently high fiber strengths other fibers have been developed in our laboratory for over a long length is important for successful possible use in the intermetallic matrix reinforcement. implementation in many composite systems. This Our paper highlights a process condition required for requires highly controlled processing operation and the development of these fibers with 100-200 μτη conditions 161. Coating defects may also induce some diameter on different core substrate. These fibers kind of flaws or microbending losses in the fiber /7,8/. exhibited good mechanical and physical properties Only two ceramic fibers are available commercially which are discussed briefly. The method for improving (boron and silicon carbide), but these fibers do not the physical and mechanical properties is also explained. match the properties required for the advanced Effect of different reactants on deposition rate and composite system. For the intermetallic matrix deposit morphology has been discussed. reinforcement we are looking for a special kind of fiber. Metal matrix composites offer low weight, high strength, high stiffness, and high temperature 1. TECHNICAL BACKGROUND capabilities to satisfy the performance requirements of future advanced aerospace systems. By choosing a A new generation of composite materials is matrix material that bonds well to the fiber, is ductile, revolutionizing today's aircraft and automotive and stands up to the environment, properties of the industries /l/. In these high technology applications, composite can be tailored to the needs of advanced weight, strength, and stiffness are critical parameters power and propulsion systems. Titanium diboride, which can be achieved by using high-performance titanium carbide, and boron carbide fiber compositions ceramic material composites 121. These ceramic are proposed as reinforcement material for intermetallic materials offer many outstanding properties for high- matrices in this paper. temperature applications. This attention led to the Though the CVD of TiB has been carried out on discovery of fibers which have excellent high- 2 various substrates of different shapes, very little work temperature strength and corrosion resistance, good has been done on fibers /4,9,10/. Even though TiB thermal shock resistance, low density, and low 2 exhibits very good oxidation resistance, the coefficient of thermal expansion. High-performance technological difficulties experienced in manufacturing fibers are available only at high prices and, as a result, of this fiber have so far prevented it from being used on tend to serve specialized and restricted markets. a large scale. There is very little information available Basically, three factors affect this price: raw material, on CVD of TiC and B C fibers. manufacturing, and more importantly new market 4 development cost. Secondly, the use is partly limited because of their brittle nature and large degree of scatter 2. EXPERIMENTAL PROCEDURE in strengths which often lead to catastrophic failure. A number of techniques have been considered to lessen or Reagent grade boron trichloride, methane, and carbon eliminate these problems 131. tetrachloride chemicals were used without further Over the past few years, numerous patents and purification. Argon and hydrogen were purified by publications have revealed the use of simple organo- passing it first through active copper nets heated above metallic compounds, metal halides, and polymer 400°C and then through the series of drying towers. precursors for routes to ceramics fibers /4/. High Gibb's The final oxygen content in the gases was less than free energy of formation or organometallic compound 1 PPM. Reagent grade titanium tetrachloride was frequently allows for lower temperature of formation of redistilled again to reduce the impurities. The final ceramics. This fact is utilized in the CVD process. The composition of impurities in titanium tetrachloride in volatile organometallic precursors allow for simple PPM is Fe < 10, Si=50, Sn=100, C = 50, V=10. purification by superfractionalization so that CVD Different substrate materials were used to find out the process results in an ultra-clean material. Very recent suitability in deposition (C, W, MO, and Ti). The experimental observations predict that traces of substrate material was prepared by cleaning the surface 44 V. Revankar and V. Hlavacek High Temperature Materials and Processes with different methods: (1) steaming the substrate around 200°C for 5 min.; (2) heated to 400°C by 3. RESULTS AND DISCUSSION passing hydrogen for 3 min.; (3) boiling the substrate The hydrogen reduction of halides process is an with HN03 acid for 8 min. The nitric acid treatment effective technique for the synthesis of ceramic fibers by gave the best result for the microcrystalline smooth CVD. The principle of this technique is as follows: deposit. Hydrogen saturated with metal halide (TiCl ) or The equipment used in this study has been discussed 4 nonmetal halide (CC1 , BC1 ) or a mixture of these elsewhere /ll/. The batch system consists of a quartz 4 3 halides is passed into the reactor in which the base reactor with the electrode ports. A small diameter filament is heated resistively. The following fibers have substrate wire runs through the electrodes, and suitable been synthesized by using the above principle: TiB , gases are introduced. The material is deposited on the 2 TiC, and B C. Only TiB fiber was given extra resistively heated wire. In the continuous system 4 2 attention because of its special interest and use. filament to be coated enters the apparatus through a mercury seal and is heated in an inert gas atmosphere, leaving the apparatus through a similar arrangement at 3.1. Titanium Diboride Fiber the exit end. The reacting gaseous mixture enters the reactor at different axial and angular positions to We tried two different ways to synthesize this fiber. The increase accessibility and uniformity of reactants on the first approach was direct boriding of the titanium fiber. filament surface. A motor driven reel draws the fiber In this process boron was deposited on the titanium through the apparatus at a steady controlled rate. The fibers by a BC13+H2 reduction method, and whole total system is shown in Fig. 1. The resultant fibers material was subsequently heated to high temperature to were analyzed by SEM, EPM, X-diffraction, and allow the counter diffusion of boron and titanium. The elemental analysis. resultant fiber (shown in Fig. 2) was irregular in shape j-Ä— Take-up Spool @ Condenser Copper turning [ Oeoxdier at 700 C r-g^-T Caq Reactor Ar DcylngTower» kogcCanJ-tfr Spool Precursor Pump Preheater Mixing l_ Chamber Tank Fiber Spreading System Fig. 1: CVD reactor flow diagram. 45 VoL 10, No. 1,1991 Intermetaltic Matrix Reinforcement Ceramic Fibers by Chemical Vapor Deposition and exhibited very low strength. This was due to the Ar gas stresses produced by the operating conditions. 2BCl3 + TiCl4 + H2 (large excess) The second approach was a chemical vapor deposition 1100-1400°C route: Hydrogen reduction of mixed vaporized halide of TIB2 + 10 HCl + H2 boron and titanium. Fig. 2: Fiber produced from direct bonding. 46 V: Revankarand V. Hlavacek High Temperature Materials and Processes The core material is resistively heated, and deposition is deposit and the core. This procedure gave very carried out using extra pure reactants and gases. In this encouraging results. The pyrolytic soft carbon deposit process the only thermodynamically possible condensed was obtained at low temperature ("900°C) using carbon phases are TiB2 or TiB2 and Β or just B, as shown by tetrachloride, hydrogen, and argon. Carbon tetrachloride Randich and Geilach 1121. Boron is deposited only at was preferred over methane gas because of better high boron to titanium ratios. Increasing the Ti to CI control of the properties and rate of soft carbon deposit. ratio increases the titanium diboride deposition, but it The fiber is shown in Fig. 4. This procedure reduced also increases the co-deposition of boron. Therefore, the the brittleness dramatically and also enhanced the B:Ti ratio was kept between 2.5-3. The H:C1 value was mechanical properties. The strength and carbon kept above 7. Low hydrogen to chlorine ratio in the deposition effect is given in Fig. 5. Recently we tried a system decreases the rate of formation of TiB2, and, in graded deposition method. A few microns of pure addition, many side products were observed for this low pyrolytic carbon layer was first deposited, followed by ratio (e.g., TiCl2, TiCl3, etc.). The resultant fiber is graded deposition of pure titanium diboride material. A shown in Fig. 3 and possesses cracks on the surface. thick pure TiB2 layer up to 80 μνα was obtained. The This is due to the stresses produced by a thermal total thickness of the deposit was in the range of 40- expansion mismatch between the tungsten core and the 150 μτη. TiB2 layer. The resultant strength is very low (of the The reaction producing TiB2 was studied at different order of 30-40 KSI). The value of the elastic modulus flow rates and temperatures. The results are shown in was around 10-15 MIS. Fig. 6. One can see from the figure that there is an Our effort has been concentrated on reducing this optimum flow rate.
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