Wet chemistry and combustion synthesis of nanoparticles of TiB2

Axelbaum, Richard L.; Bates, S.E.; Buhroi, W.E.; Frey, Claire A.; Kelton, K. F.; Lawton, S. A.; Rosen, Lee; Sastry, Srikanth

doi:10.1016/0965-9773(93)90018-7

Cited by 14 publications

(5 citation statements)

References 4 publications

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“…Thermodynamic analyses of reactions of this type are given in Calcote and Felder, [6] Glassman et al, [7] and Axelbaum and co-workers. [8,11] A key finding of these studies is that nearly 100 pct yields can be obtained when reaction temperatures are sufficiently low. Calcote and Felder optimized their yields by passing the products of their reactor through a supersonic nozzle.…”

Section: Thermodynamics Of the Sodium/halide Flamementioning

confidence: 98%

“…Glassman et al [7] developed a thermodynamic criterion for the reactive-metal/halide system and showed, experimentally, that a number of refractory materials, including titanium diboride, can be produced by burning droplets of a sodium-potassium eutectic in various halide atmospheres. To develop this technology for nanostructured materials, Axelbaum and co-workers [8][9][10][11] demonstrated the production of nanocrystalline powders of titanium diboride in three different reactors: a low-pressure, low-temperature reactor, a high-temperature flow reactor, and a coflow diffusion flame.…”

Section: B Sodium/halide Flamementioning

confidence: 99%

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A flame process for synthesis of unagglomerated, low-oxygen nanoparticles: Application to Ti and TiB2

Axelbaum

Sastry

DuFaux

et al. 1997

Metall Mater Trans B

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A gas-phase flame process for synthesizing unagglomerated nanoparticles of metals, intermetallics, ceramics, and composites is described. Employing this process, titanium and titanium boride have been synthesized by the vapor-phase reaction of sodium with titanium tetrachloride and a 1:2 mixture of titanium tetrachloride and boron trichloride, respectively. To minimize agglomeration and protect the particles from postflame oxidation, the NaCl by-product is allowed to condense onto the particles in situ, yielding NaCl-encapsulated particles. In this way, stable, unagglomerated Ti and TiB 2 nanoparticles have been produced and the encapsulated powders have been handled in air without oxidation. Particle size has also been varied with the encapsulation process, and titanium particles with mean sizes of 10 and 60 nm have been produced by varying operating conditions. The NaCl has been removed by water washing as well as vacuum annealing. Thermodynamic results show that the sodium/halide process is applicable for synthesis of many materials, with yields approaching 100 pct under a wide range of operating conditions. Similarly, the encapsulation process is generally applicable, making the sodium/halide flame and encapsulation process a viable one for large-scale synthesis of environmentally insensitive nanopowders.

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Section: Thermodynamics Of the Sodium/halide Flamementioning

confidence: 98%

Section: B Sodium/halide Flamementioning

confidence: 99%

A flame process for synthesis of unagglomerated, low-oxygen nanoparticles: Application to Ti and TiB2

Axelbaum

Sastry

DuFaux

et al. 1997

Metall Mater Trans B

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“…In this connection, advanced scientific organizations, world manufacturers of refractories and metals in the last 10-15 years are conducting intensive research studies on the methods of synthesis of refractory materials based on oxides and borides of titanium with the aim of reducing their cost [4][5][6][7][8][9]. Some progress has been made, but commercial technologies for the production and use of these materials on a large scale have not been reported.…”

Section: Introductionmentioning

confidence: 99%

Carbothermic Synthesis of Titanium Diboride: Upgrade

Gorlanov¹,

Bazhin²,

Fedorov³

et al. 2018

J. Sib. Fed. Univ. Chem.

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The technology of carbothermic reduction of titanium and boron oxides in the TiО 2-B 2 О 3-C reaction mixture at temperatures up to 1070 °C is presented. The temperature and atmospheric regimes of lowtemperature reduction of TiO 2 are determined. In the Ti-B-O-C system, successive phase formation of TiО 2 →Ti n O 2n-1 →TiBО 3 →TiC x O 1-x →TiB 2 at 1030 ÷ 1050 °C was realized, which was recorded by X-ray phase analysis of the samples after synthesis. The conditions for the realization of low-temperature synthesis are established, which consist in observing the prescriptions and special regimes for preparing the reaction mixture, the conditions for heating and holding the samples in a controlled atmosphere. For discussion, the mechanism of oxycarboboride phases formation at each of the stages of reduction of activated titanium oxide is presented. The principal possibility of low-temperature synthesis of TiB 2 in the composition of carbon-graphite products by free pitch technology in the conditions of existing kilns is shown.

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“…This can be achieved by using highly refined synthesis conditions that allow sufficient crystallization and a high control of purity. TiB 2 nanoparticles have been prepared by wet‐chemical‐synthesis methods that provide insufficient crystallization, which complicates a proper characterization of the microstructure , . Gas‐phase combustion synthesis, as well as more expensive approaches including mechanochemical methods with high‐energy ball‐milling, and pressurized vessels often lead to contaminated products.…”

Section: Introductionmentioning

confidence: 99%

A Size‐Dependent Analysis of the Structural, Surface, Colloidal, and Thermal Properties of Ti_1–xB₂ (x = 0.03–0.08) Nanoparticles

et al. 2016

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We report the size-dependent structural, surface, colloidal, and thermal properties of the well-known refractory material titanium diboride prepared at the nanoscale by a sizecontrolled inorganic molten-salt technique. A combined analysis of the powder X-ray diffraction data through a modified Williamson-Hall plot, a size-strain plot, and Rietveld fitting methods indicates that TiB 2 nanocrystals with average crystallite sizes smaller than D ≈ 22 nm prefer to form defects at the titanium site rather than experience strain. The resulting composition is Ti 1-x B 2 [x = 0.03(1)-0.08 (1)]. The size-induced defect formation is accompanied by anisotropic lattice contraction that decreases primarily the cell parameter c. Transmission electron microscopy revealed that the nanocrystals are embedded [a] Physical Chemistry,

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Wet chemistry and combustion synthesis of nanoparticles of TiB2

Cited by 14 publications

References 4 publications

A flame process for synthesis of unagglomerated, low-oxygen nanoparticles: Application to Ti and TiB2

A flame process for synthesis of unagglomerated, low-oxygen nanoparticles: Application to Ti and TiB2

Carbothermic Synthesis of Titanium Diboride: Upgrade

A Size‐Dependent Analysis of the Structural, Surface, Colloidal, and Thermal Properties of Ti_1–xB₂ (x = 0.03–0.08) Nanoparticles

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Wet chemistry and combustion synthesis of nanoparticles of TiB2

Cited by 14 publications

References 4 publications

A flame process for synthesis of unagglomerated, low-oxygen nanoparticles: Application to Ti and TiB2

A flame process for synthesis of unagglomerated, low-oxygen nanoparticles: Application to Ti and TiB2

Carbothermic Synthesis of Titanium Diboride: Upgrade

A Size‐Dependent Analysis of the Structural, Surface, Colloidal, and Thermal Properties of Ti1–xB2 (x = 0.03–0.08) Nanoparticles

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A Size‐Dependent Analysis of the Structural, Surface, Colloidal, and Thermal Properties of Ti_1–xB₂ (x = 0.03–0.08) Nanoparticles