Synthesis of Boron Carbide Powder via Rapid Carbothermal Reduction Using Boric Acid and Carbonizing Binder

Raw material is one of the most decisive factors for the quality of sintered boron carbide (B4C) products, in the past, there were relatively successful efforts for the synthesis of B4C powders via carbothermal reduction approaches. To prepare high-quality powder, a deeper understanding of the relationship between technological manufacturing parameters and resulting powder properties is required. In this paper, pure B4C powders were synthesized by rapid carbothermal reduction (RCR) under B2O3 excess conditions using boric acid and a carbonizing binder as B2O3 and carbon source, respectively. The molar ratio of B2O3/C of starting mixtures was varied from 0.75:1 to 4:1. The effects of heat-treating temperature and starting composition on phase constitution, morphology as well as stoichiometry of the prepared powders were investigated. The studies show that the starting composition has no effect on the stoichiometry of the powders, all boron carbides synthesized at 1900 °C have a stoichiometric composition of B4C. With increasing heating temperature and B2O3 content in the starting composition, the particle size of B4C was reduced. Uniform B4C powders with an average grain size of 300 nm were synthesized at 1900 °C from a starting powder mixture with a molar ratio of B2O3/C = 4. A formation mechanism is proposed under large B2O3 excess conditions. For the starting powder mixtures with a molar ratio of B2O3/C < 2, the formation of boron carbide occurs through both liquid–solid reaction and gas–solid reaction. Accordingly, the synthesized powders exhibit a morphology with mixed elongated platelets and small polyhedral particles. For the starting powder mixtures with a molar ratio of B2O3/C ≥ 2, fine-sized B4C particles were formed by a liquid–solid reaction.

[1]  H. Hadadzadeh,et al.  Effects of boron oxide composition, structure, and morphology on B4C formation via the SHS process in the B2O3–Mg – C ternary system , 2020 .

[2]  R. Haber,et al.  Modification of commercial boron carbide powder using Rapid Carbothermal Reduction , 2018, International Journal of Applied Ceramic Technology.

[3]  R. Haber,et al.  Densification and characterization of rapid carbothermal synthesized boron carbide , 2017 .

[4]  Zhe Cheng,et al.  Understanding the morphological variation in the formation of B4C via carbothermal reduction reaction , 2016 .

[5]  A. Domínguez-Rodríguez,et al.  Grain size dependence of hardness and fracture toughness in pure near fully-dense boron carbide ceramics , 2016 .

[6]  A. Michaelis,et al.  Reactive sintering process and thermoelectric properties of boron rich boron carbides , 2014 .

[7]  A. Michaelis,et al.  In Situ Preparation and Thermoelectric Properties of B4C1−x–TiB2 Composites , 2013, Journal of Electronic Materials.

[8]  R. Haber,et al.  Submicron Boron Carbide Synthesis through Rapid Carbothermal Reduction , 2012 .

[9]  O. Yucel,et al.  Effect of initial composition on boron carbide production by SHS process followed by acid leaching , 2012 .

[10]  R. Haber,et al.  Boron Carbide: Structure, Properties, and Stability under Stress , 2011 .

[11]  I. Yanase,et al.  Synthesis of boron carbide powder from polyvinyl borate precursor , 2009 .

[12]  N. Seiler,et al.  Investigations on boron carbide oxidation for nuclear reactors safety : General modelling for ICARE/CATHARE code applications , 2008 .

[13]  K. Balasubramanian,et al.  Multiphase formation of boron carbide in B2O3–Mg–C based micropyretic process , 2007 .

[14]  S. Anthonysamy,et al.  Vapour pressure and standard enthalpy of sublimation of H3BO3 , 2007 .

[15]  A. Khanra Production of boron carbide powder by carbothermal synthesis of gel material , 2007 .

[16]  M. Karaman,et al.  Kinetic investigation of chemical vapor deposition of B4C on tungsten substrate , 2006 .

[17]  A. S. Ramos,et al.  High-energy ball milling of powder B–C mixtures , 2006 .

[18]  B. Morosin,et al.  Structures of the Boron-Rich Boron Carbides from Neutron Powder Diffraction: Implications for the Nature of the Inter-Icosahedral Chains , 1996 .

[19]  S. Pratsinis,et al.  Kinetics of Carbothermal Reduction Synthesis of Boron Carbide , 1992 .

[20]  T. Aselage,et al.  Lattice Constants of Boron Carbides , 1992 .

[21]  A. Weimer,et al.  Rapid carbothermal reduction of boron oxide in a graphite transport reactor , 1991 .

[22]  Y. Tumanov The synthesis of boron carbide in a high frequency electromagnetic field , 1979 .

[23]  P. N. Walsh,et al.  THE REACTION BETWEEN B2O3(l) AND C(s): HEAT OF FORMATION OF B2O2(g)* , 1960 .