Synthesis of Biopolymer‐Derived Zirconium Carbide Powder by Facile One‐Pot Reaction

Abstract

Zirconium carbide (ZrC) was synthesized by polycondensation and carbothermal reduction reactions from an organic-inorganic hybrid complex. A natural biopolymer Gum Karaya (GK) and zirconyl oxychloride octahydrate (ZOO) were used as the sources of carbon and zirconium, respectively. FTIR of as-synthesized dried complexes revealed formation of Zr-O. Pyrolysis of the complexes at 1200°C/1 h under argon resulted in tetragonal and monoclinic zirconia which after heat treatment at 1400°C-1550°C transformed to zirconium carbide. Thermal analysis shows that the GK-ZOO complexes lost less mass than the pristine GK to 600°C. The intensity of exothermic decomposition decreases and shifted to higher temperature for the hybrid complexes indicating that zirconia induced thermal stability. A maximum ZrC yield of~60 wt% is obtained for the intermediate GK-ZOO ratio of 1:2. Particles pyrolyzed for 1 h at 1550°C were coarser (5-10 lm) with flakes for lower GK-ZOO weight ratio, but were spheroidal with narrow size distribution (~1 lm) with increasing GK-ZOO weight ratio.

Low Temperature Carbothermal Reduction Synthesis of ZrC Nanofibers via Cyclized Electrospun PVP/Zr(OPr)4 Hybrid

“…Two flattened endothermic peaks at ~60 and 130°C in DSC curve are attributed to the removal of trapped water and glass transition of PVP polymeric network owing to a quick temperature change rate in comparison with the molecular rearrangement along with the effects of sorbed moisture due to the hygroscopic nature of the material . Two broad exothermic peaks at 400–470°C and 1250–1330°C can be most probably ascribed to the phase transformation from t‐ZrO 2 to m‐ZrO 2 and carbothermal reduction to form ZrC . The TG analysis exhibits that the specimen undergoes a significant weight loss of ~58% between room temperature and ~550°C.…”

Low-temperature solution synthesis of nanosized hafnium carbide using pectin

“…The peak at about 660 cm -1 ν(Hf-O) appears due to ring distortion in FTIR. Thermogravimetric analysis has been used to investigate the decomposition, stability, purity and yield by various investigators [17,[19][20][21][22][23]. 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60 61 62 63 64 HfO, which is more stable at higher temperatures [27].…”

“…The present study focused on synthesis of hafnium carbide using pectin as the source of carbon and chelation followed by carbothermic reduction. This technique offers some advantages compared to conventional powder processing techniques, such as lower reaction temperatures and shorter reaction times which is due to the intimate contact of the polymer with the organometallic salt [17]. This process reduces the kinetic barriers between the formed metal oxide and the carbon particles created in pyrolysis of metal alkoxide polymer due to the atomic level mixing of reactants in the precursor material.…”

Deacetylation-induced changes in thermal properties of Sterculia urens gum

“…From Fig. 3a, b, the degree of deacetylation is calculated for both deacetylation by Thermogravimetric analysis has been used as an excellent tool to investigate the decomposition, stability and purity of materials by many investigators [8,[11][12][13][14][15][16][17]. Figure 4 shows the TG and DTG curve along with the insets of zoomed DTG curve of the major degradation step of pristine, and deacetylated sterculia at different temperature in nitrogen atmosphere is presented.…”

“…Tree wound exudates gum of natural acid polysaccharide which has attracted huge attention among researcher because of their immense potential application in food industry, biomedical as well as material science [1][2][3][4][5][6][7][8]. Natural anionic acid polysaccharides are inexpensive, easily available, non-toxic, biodegradable materials which exhibit peculiar physicochemical properties and applications [6,9,10].…”