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Reaction Bonded Refractory Metal Carbide/Carbon Composites

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Reaction Bonded Refractory Metal Carbide/Carbon Composites Polyhedrm Vol.13, No. 8, pp. 131S1327, 1994 Pergamon Ekvier Science Ltd. Printed in Great Britain REACTION BONDED REFRACTORY METAL CARBIDE/CARBON COMPOSITES ANDREW N. MacINNES and ANDREW R. BARRON” Department of Chemistry, Harvard University, Cambridge, MA 02138, U.S.A. and JASON J. LI and THOMAS R. GILBERT Department of Chemistry and Barnett Institute of Chemical Analysis and Materials Science, Northeastern University, Boston, MA 02115, U.S.A. Abstract-A simple chemical process has been developed that allows the rapid conversion of carbon substrates to the refractory metal carbides (MC) of titanium, zirconium, hafnium, vanadium, niobium, tantalum and tungsten. As a demonstration of the technique, graphite rods are infiltrated with an ethanolic solution of various metal oxide-halides, and resistively fired (1350-3000°C) under an argon atmosphere. The final composite produced is found to contain a residual carbon core within a fully dense metal carbide-carbon matrix outer layer. The effects of both firing temperatures, and the number of infiltration-fire treatments, have been investigated in order to determine optimum firing conditions (i.e. maximum carbide formation) for each individual metal carbide. To demonstrate the applicability of the technique for a range of substrate materials, niobium and titanium carbides were formed on carbon fibre tows and non-porous substrates, respectively. The formation of mixed Nb- Ti carbide coatings of varying composition were investigated in order to determine the factors controlling the formation of ternary phases. The identity of the transition metal precursors and the possible pathway of their conversion to the appropriate carbide is discussed. All the composites have been characterized by X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM) with associated energy-dispersive X-ray (EDX) analysis, and X-ray diffraction (XRD). INTRODUCTION carbide to provide physical compatibility with the carbon substrate and prevent the outward diffusion Carbon fibre reinforced carbon matrix (carbon- of carbon. The outer layer in the multi-layered coat- carbon) composites are currently being proposed ing scheme would then be a suitable oxide (possibly as candidate structural materials for aerospace use the native oxide formed on the carbide inner layer) based on their high specific strength at elevated providing a barrier to the ingress of oxygen into the temperatures (> 2OOo”C).’However, the successful carbon substrate. application of such composites will be dependent Although inert barriers coatings formed by tra- on the development of a suitable high temperature ditional methods [e.g. physical vapour deposition coating system to alleviate the susceptibility of the (PVD), chemical vapour deposition (CVD) and sol- carbon based materials to oxidation above 400°C. gel techniques] do provide diffusion barriers: they Strife and Sheehan’ have reviewed coating require- are, however, generally not resistant to thermal ments and proposed a multi-layered coating system. cycle operations imposed on the composite The inner layer would consist of a refractory metal material. This failure during thermal cycling is due to the thermal expansion mismatch between the *Author to whom all correspondence should be coating (metal carbide or oxide) and the carbon addressed. matrix. Cracking and spallation of the coating 1315 1316 A. N. MacINNES et al. Coating Coating Substrate Substrate I I I (I) (11) ensues as a result of thermal stresses generated at We have previously communicated that niobium an essentially atomically abrupt interface (I). It carbide (NbC) coatings can be produced on gra- becomes clear, therefore, that before full exploi- phitic carbon by the infiltration of an ethanolic tation of carboncarbon composites can be solution of niobium pentachloride into the carbon realized, it is essential to alleviate the thermal stress substrate followed by resistive firing.Y In addition, generated in these materials during thermal cycling. we have shown, in preliminary studies, that this A common approach in the matching of two dis- process may be extended to the more dense carbon similar materials such as quartz and borosilicate fibre substrates.“,” In this present paper we extend glass is to produce a graded interface ; in terms of these communications to the formation of carbide chemical composition and mechanical properties coatings of the refractory metals titanium, (II). If a graded interface will overcome the thermal zirconium, hafnium, vanadium, niobium, tantalum expansion mismatch between carbon substrates and and tungsten. In addition, the formation of ternary ceramic coatings, the problem then becomes one of carbides, the effect of the carbon substrate identity developing suitable routes to the formation of such on carbide formation, and the possible mechanism a graded interface.4 In a related study we have for carbide formation are presented. reported the formation of graded interfaces between niobium metal and ceramic coatings via thermal, RESULTS AND DISCUSSION ion beam and laser treatment.5.6s7 However, these physical techniques do not lend themselves to appli- Dissolution, in wet (as received) ethanol, of the cation for carbon substrates. We have, therefore, early transition metal halides listed in Table 1 initiated a program of research to examine the results in the evolution of HCl and the exothermic possibility of facile chemical reactions leading to the formation of solvated oxide--chlorides (see after). production of a graded interface between graphite The immersion of carbon graphite rods in these carbon substrates and refractory metal carbide oxide-chloride solutions followed by drying and coatings.’ resistively firing in the apparatus shown in Fig. 1, Table 1. Chemical characterization and optimum firing temperature for the metal carbide coated carbon rods Optimum firing temperature (“C) XPS peak shift for carbide Max. carbide content Max. metal content Metal Precursor system XRD XPS XPS c 1s M 2~312 Titanium TiClJEtOH 2200 2000 2200-2500 281.5 454.63 Zirconium ZrCL,/EtOH 2200 2250 1500-1700 Hafnium HfCl,/EtOH 2200 Y 150&1750 Y L1 Vanadium VCl,/EtOH 2000 2200-2500 2200 282.24 513.10 Niobium NbC&/EtOH 1800 223@-2750 210&2750 282.5 203.6’ Tantatum TaCl,/EtOH 1800 2000 2000-2250 281.75 226.96 Tungsten WCl,/EtOH 2200 LI 2750 n 31-5 n No carbide detected on the surface by XPS. b Nb 3d5/2. 1317 BNchimber electrode clamps ----)- power supply -----_ t Ar Fig. 1. Schematic diagram of apparatus used for resistively firing carbon rods. Fi g. 2. SEM cross sectional micrographs of untreated (a), and Nb treated (b) rod. In the latter can be seen residual graphite particle (A) within a NbC/C matrix (B). 1318 A. N. MacINNES et al. Fig. 2-continued. results in the formation of the appropriate metal The XRD spectrum of the pulverized fired rods carbide in a carbide-carbon compact. (Fig. 3) exhibit reflections due to the presence of The SEM cross sectional micrograph of an un- graphitic carbon and the appropriate refractory- treated rod is shown in Fig. 2a, while the equivalent metal carbide. Oxides are only observed by XRD view for a niobium treated rod is shown in Fig. as a minor constituent for some of the samples 2b. Whereas the untreated rods are porous, but of (Fig. 3). It should be noted that the minimum firing homogeneous composition, it can be clearly seen temperature required for the detection of the metal from Fig. 2b that under the reaction conditions carbide by XRD (see Table 1) is dependent on the of the experiment a fully impregnated composite identity of the metals. As is discussed below, sig- material is produced. The composite consists of nificant quantities of the carbides are formed at residual carbon particles (Fig. 2b. A) within a metal lesser firing temperatures, but are presumably carbide-carbon matrix (Fig. 2b. B). Similar bulk amorphous. microstructures are obtained for all the other metal The surface chemical analysis of the fired rods carbides. was enabled by X-ray photoelectron spectroscopy Reaction bonded refractory metal composites 1319 0.4 0.0 0.3 2.2 4.2 6.1 8.1 10.0 ANGLE ( degrees 2 theta ) [x 1O1] Fig. 3. XRD of pulverized niobium treated carbon rod (Cu-K, radiation NbC peaks are indexed, C refers to graphite peaks). (XPS), the results of which are given for the opti- mum firing conditions in Table 1. As a typical result Carbide Fig. 4 shows the Nbxd and Cl, regions for a NbCl, treated rod, with the peak-fits performed for the Carbon chemical states of niobium and carbon present.‘* The niobium is present as both carbide and oxide (Nb205 and a suboxide) and the carbon as graphite, VW carbide and adventitious hydrocarbons. In all the samples the signal for the adventitious hydrocarbon that the carbide : carbon ratios of the bulk material and oxides are eliminated after argon ion beam as determined by XRD are lower than those found sputtering of the surface. The oxide present is there- by EDX (a near-surface technique) of the surface fore due to surface oxidation of the carbide rather of an uncleaved rod. These results are consistent than as a result of unreacted precursor. It should with the absorption of the precursor solution into be noted that no chlorine was detected for any of the carbon rod followed by carbide formation the samples, consistent with the complete decompo- throughout the rod during the subsequent firing sition of the precursors. step. In the cases where carbide is detected the metal The relative carbide content of the treated rods to carbon ratio is higher for EDX (a near surface will clearly be dependent on a number of possible technique) than the metal carbide to carbon graph- factors, including : the number of infiltration-firing ite ratio determined by XRD (a bulk technique). sequences, the firing temperature, and the identity Although this may be due, in part, to the formation and quantity of the transition metal.
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