Soluble precursors possessing both Al-N and B-N backbones have been prepared from LiAlH 4 , LiBH 4 , and RNH 2Á HCl (R = Me and Et) in one pot. The infrared (IR) and nuclear magnetic resonance (NMR) spectra of the precursors indicate that the precursors possess Al-H and B-H groups as well as Al-N, B-N, Al-(-H) 2 -Al, and Al-(-H) 2 -B bonds. TG analysis reveals that the ceramic yield of the precursor [AB11 Me (LiAlH 4 /LiBH 4 /MeNH 2Á HCl = 1/1/2)] up to 1000 C under an argon atmosphere is 74.4 mass %. The transmission electron microscopic (TEM) images and the X-ray diffraction (XRD) pattern of AB11 Me that was pyrolyzed at 1600 C indicate that the average size of crystalline aluminum nitride (AlN) is about 14 nm and that crystalline AlN particles are distributed homogeneously in an amorphous matrix.Pyrolytic conversion of precursors, so-called preceramic materials, is a chemical route to obtaining non-oxide ceramics and ceramic-based composites. [1][2][3][4] Using this approach, highpurity materials with a homogeneous distribution of component elements on an atomic scale and a controllable microstructure can be obtained at relatively low temperatures. When preceramic materials are fusible at relatively low temperatures or soluble in common organic solvents, this process can also offer fabrication routes to desirable shapes, including coatings and fibers, which are essentially unattainable by a conventional powder process. 4 Aluminum nitride (AlN)-boron nitride (BN) composites possess many attractive properties, including high thermal conductivity and high electrical insulation as well as excellent machinability and lubricativity.5-10 These properties suit them various applications, 5,7 such as electromagnetic window materials, heat sinks, and protective coatings of communication and detection equipment on aircraft. AlN-BN composites are generally prepared by a conventional powder process.11-15 The powder process generally results in substantial anisotropy in their microstructures, however, and, consequently, in their various properties.
11Recently, a few studies have reported the preparation of AlN-BN ceramic-based composites by pyrolytic conversion of precursors. In an approach using metalorganic compounds, the precursors were synthesized by the reaction between (Et 2 AlNH 2 ) 3 and B(NEt) 3 to form homogeneous composites composed of crystalline AlN and turbostatic-BN by pyrolysis.
5In another approach, gels for AlN-BN composites were prepared by the ammonolysis of H 3 BO 3 , AlCl 3 , and (NH 2 ) 2 CO in aqueous solutions. 16 As a one-pot synthesis approach, Dou et al. prepared precursors by reacting metal hydrides (H 3 Al Á NMe 3 and H 3 B Á NH 3 ) with ammonia.17 Although homogeneously dispersed AlN-BN composites were considered to be obtained by this approach, all of these precursors were insoluble in common organic solvents.Here, we report a one-pot synthesis of soluble precursors by the reactions involving lithium tetrahydridoaluminate (LiAlH 4 ), lithium tetrahydroborate (LiBH 4 ), and alkylamine hydrochl...