Direct electrochemical synthesis of zirconium carbide from zirconia/C precursors in molten calcium chloride

Dai, Lei; Wang, Xianyu; Zhou, Huizhu; Yu, Yao; Zhu, Jing; Li, Yuehua

doi:10.1016/j.ceramint.2014.12.101

Cited by 17 publications

(14 citation statements)

References 23 publications

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“…It can be modified for the synthesis of metal carbides by employing a mixture of metal oxide and carbon as the cathode so that the released metal reacts with the carbon in situ. This has been shown for a few pseudo‐unary carbides, but not for any higher systems.…”

Section: Figurementioning

confidence: 89%

Facile Electrochemical Synthesis of Nanoscale (TiNbTaZrHf)C High‐Entropy Carbide Powder

et al. 2020

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High‐entropy alloys and compounds are becoming an important class of new materials due to their outstanding refractory and high‐temperature properties. However, preparation in bulk quantities and in powder form via classical metallurgical methods is challenging. Here, we report the first synthesis of an ultra‐high‐temperature high‐entropy carbide, (TiNbTaZrHf)C, via a facile electrochemical process. In this, a mixture of the individual metal oxides and graphite is deoxidised in a melt of CaCl2 at a temperature of only 1173 K. The (TiNbTaZrHf)C prepared is single‐phase fcc and has a powdery morphology with a particle‐size range of 15–80 nm. Such materials are in demand for modern additive manufacturing techniques, while preliminary tests have also indicated a possible application in supercapacitors. The successful synthesis of (TiNbTaZrHf)C powder may now guide the way towards establishing the electrochemical route for the preparation of many other entropy‐stabilised materials.

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Section: Figurementioning

confidence: 89%

Facile Electrochemical Synthesis of Nanoscale (TiNbTaZrHf)C High‐Entropy Carbide Powder

et al. 2020

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“…Based on the experimental results and the previous studies on the reaction mechanisms of the electrodeoxidation of SiO 2 , TiO 2 , ZrO 2 , and Ta 2 O 5 in CaCl 2based molten salts, [21][22][23][24][25][26][27][28][29][31][32][33][34][35][36][37][44][45][46]48,[52][53][54][55]62 23,35 would thus present in the electrochemical production process. Therefore, the reaction mechanism of the electrodeoxidation of SiO 2 /C to SiC in molten CaCl 2 can be generally summarized as reactions (1)-( 5), as shown in Fig.…”

Section: Reaction Mechanisms Of the Electrodeoxidation Processesmentioning

confidence: 99%

“…[41][42][43][44][45][46][47][48][49] However, in order to produce MCs, the carbon content of the MO x /carbon (MO x /C) precursors used in the graphite-based anode electrodeoxidation process should be generally higher than the stoichiometric ratios of their corresponding MCs. 44,48,49 Therefore, it is difficult to control the carbon content of the MCs products fabricated using the graphite-based anode electrodeoxidation process. 41 In order to produce pure MCs with pre-designed components, the graphite-based anode needs to be improved to avoid the CO/ CO 2 -related anodic side reactions.…”

Section: Introductionmentioning

confidence: 99%

Solid oxide membrane-assisted controllable electrolytic fabrication of metal carbides in molten salt

Zou

Zheng

et al. 2016

Faraday Discuss.

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Silicon carbide (SiC), titanium carbide (TiC), zirconium carbide (ZrC), and tantalum carbide (TaC) have been electrochemically produced directly from their corresponding stoichiometric metal oxides/carbon (MOx/C) precursors by electrodeoxidation in molten calcium chloride (CaCl2). An assembled yttria stabilized zirconia solid oxide membrane (SOM)-based anode was employed to control the electrodeoxidation process. The SOM-assisted controllable electrochemical process was carried out in molten CaCl2 at 1000 °C with a potential of 3.5 to 4.0 V. The reaction mechanism of the electrochemical production process and the characteristics of these produced metal carbides (MCs) were systematically investigated. X-ray diffraction, scanning electron microscopy, and transmission electron microscopy analyses clearly identify that SiC, TiC, ZrC, and TaC carbides can be facilely fabricated. SiC carbide can be controlled to form a homogeneous nanowire structure, while the morphologies of TiC, ZrC, and TaC carbides exhibit porous nodular structures with micro/nanoscale particles. The complex chemical/electrochemical reaction processes including the compounding, electrodeoxidation, dissolution-electrodeposition, and in situ carbonization processes in molten CaCl2 are also discussed. The present results preliminarily demonstrate that the molten salt-based SOM-assisted electrodeoxidation process has the potential to be used for the facile and controllable electrodeoxidation of MOx/C precursors to micro/nanostructured MCs, which can potentially be used for various applications.

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“…However, it remains a challenge to fabricating W-ZrC material with ZrC particle size < 10 nm. For the synthesis of ZrC particles, traditional methods (like carbothermal reduction) is usually carried out at elevated temperatures, which leads to a large ZrC particle size [24][25][26].…”

Section: Introductionmentioning

confidence: 99%

Mechanical properties and thermal shock resistance of tungsten alloys strengthened by laser fragmentation-processed zirconium carbide nanoparticles

Jin

Zhang

et al. 2020

Tungsten

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Direct electrochemical synthesis of zirconium carbide from zirconia/C precursors in molten calcium chloride

Cited by 17 publications

References 23 publications

Facile Electrochemical Synthesis of Nanoscale (TiNbTaZrHf)C High‐Entropy Carbide Powder

Facile Electrochemical Synthesis of Nanoscale (TiNbTaZrHf)C High‐Entropy Carbide Powder

Solid oxide membrane-assisted controllable electrolytic fabrication of metal carbides in molten salt

Mechanical properties and thermal shock resistance of tungsten alloys strengthened by laser fragmentation-processed zirconium carbide nanoparticles

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