Towards a mechanistic understanding of the sol–gel syntheses of ternary carbides

Siebert, J. Paul; Juelsholt, Mikkel; Günzing, Damian; Wende, Heiko; Ollefs, Katharina; Birkel, Christina S.

doi:10.1039/d2qi00053a

Cited by 5 publications

(15 citation statements)

References 42 publications

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“…The latter can be attributed to the final carbothermic reduction toward the Mn 3 GaC phase and confirms the reaction temperature of 1050 °C within the tube furnace. Considering the obtained data, all observations follow recent extensive studies of our group to propose a general reaction mechanism to obtain ternary carbides via sol–gel chemistry transitioning through intermediate oxide phases via a carbothermic reduction reaction …”

Section: Resultssupporting

confidence: 74%

“…Considering the obtained data, all observations follow recent extensive studies of our group to propose a general reaction mechanism to obtain ternary carbides via sol−gel chemistry transitioning through intermediate oxide phases via a carbothermic reduction reaction. 40 Magnetic Properties. While all samples are essentially phase-pure as revealed by X-ray diffraction and Rietveld refinement, the magnetic response gives further information on the phase quality and especially on deviations from the stoichiometric occupancy of the respective lattice sites.…”

Section: ■ Introductionmentioning

confidence: 99%

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Rapid Sol–Gel Synthesis Approach for the Preparation of the Magnetocaloric Antiperovskite Mn₃GaC

Kubitza,

Babaei,

Wiedwald

et al. 2023

Chem. Mater.

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Magnetocaloric materials form highly promising candidates to fundamentally change the current vapor compression-based refrigeration technology, with the benefits of bypassing the use of greenhouse gas emissions and improving the energy efficiency. One member within this group of materials is the antiperovskite phase Mn 3 GaC. However, despite the big potential that lies in its materials properties, the synthesis of this phase and antiperovskites in general is still mainly achieved by conventional energy-consuming solid-state methods, resulting in long reaction times (>7 days) and challenges in influencing the microstructure or morphology. Here, we report a rapid sol−gel approach using citric acid as a gelling agent, which allows us to obtain a highly phase-pure, crystalline Mn 3 GaC phase after only 5 h of annealing. Ex situ X-ray powder diffraction data, combined with DSC/ TGA measurements, elucidate the reaction mechanism, which involves carbothermal reduction of intermediate oxides. Vibrating sample magnetometry of the annealed products demonstrates the ability to alternate the magnetic properties of Mn 3 GaC simply based on the variation of the gelling agent amount in the reaction mixture. Overall, this offers a facile alternative and energy-and time-efficient approach for the synthesis of antiperovskite carbide phases with the power to specifically influence materials properties by only slight adjustments of parameters within this wet chemical-based synthesis procedure.

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Section: Resultssupporting

confidence: 74%

Section: ■ Introductionmentioning

confidence: 99%

Rapid Sol–Gel Synthesis Approach for the Preparation of the Magnetocaloric Antiperovskite Mn₃GaC

Kubitza,

Babaei,

Wiedwald

et al. 2023

Chem. Mater.

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“…Unlike the conventional sintering process for MAX phases, the integration of the sol–gel method and electrospinning process would effectively shrink the average size of the MAX phase by restricting the diffusion distance of ions. The main reactions are the following equations (Me = Cr or Ga) − …”

Section: Resultsmentioning

confidence: 99%

Fabrication of Nano-sized Cr₂GaC with a Bottom-Up Approach for Lithium Storage

Xie,

Zhang,

et al. 2023

ACS Appl. Nano Mater.

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Lithium-ion batteries (LIBs) that balance cycling stability and specific capacity are crucial for the development of green energy systems. MAX phases, with high theoretical specific capacities and robust layered structures, have the potential to be excellent anode materials for LIBs. However, the large particle size of MAX phases makes the metallic atoms in them difficult to utilize, which results in poor specific capacities and long electrochemical activation cycles. Therefore, constructing nanosized MAX phases is an effective strategy to achieve a satisfactory electrochemical performance. Herein, for the first time, we obtain Cr 2 GaC nanoparticles (Cr 2 GaC NPs, ∼100 nm) in situ anchored on carbonaceous nanofibers (NanoMAX-CF for short) via electrospinning. The bottom-up synthesis process results in the uniform size of Cr 2 GaC particles and guarantees their homogeneous distribution within the carbonaceous nanofibers. The asprepared NanoMAX-CF composites not only exhibit high specific surface area and suitable pore distributions but also have great structural stability, resulting in superior rate capability (133 mA h g −1 at 10 A g −1 ) and excellent cyclic performance (534 mA h g −1 at 0.1 A g −1 after 300 cycles and 156.5 mA h g −1 at 10 A g −1 after 8000 cycles). This work paves the way to prepare nanosized MAX phases and provides perspectives to leverage MAX phases for lithium storage.

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“…In a detailed analysis, the reaction mechanism was unraveled, which involves the carbothermal reduction of amorphous oxide species followed by subsequent reaction with graphitic carbon to form the carbide and carbonitride product. [248] Besides, gel-builders can be used, as shown for the synthesis of V 2 PC (Figure 5). [151] One of the perks of starting with a gel is that it can be processed into different morphologies and shapes, which is not easily possible when working with solids/powders.…”

Section: Conventional Heatingmentioning

confidence: 99%

“…Despite the perfectly mixed reactants, quite high reaction temperatures (around 1000 °C) are still necessary for the MAX phases to form. In a detailed analysis, the reaction mechanism was unraveled, which involves the carbothermal reduction of amorphous oxide species followed by subsequent reaction with graphitic carbon to form the carbide and carbonitride product [248] . Besides, gel‐builders can be used, as shown for the synthesis of V 2 PC (Figure 5).…”

Section: Synthesis Strategiesmentioning

confidence: 99%

Extending the Chemistry of Layered Solids and Nanosheets: Chemistry and Structure of MAX Phases, MAB Phases and MXenes

et al. 2023

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MAX phases are layered solids with unique properties combining characteristics of ceramics and metals. MXenes are their two‐dimensional siblings that can be synthesized as van der Waals stacked and multi‐/single‐layer nanosheets, which possess chemical and physical properties that make them interesting for a plethora of applications. Both families of materials are highly versatile in terms of their chemical composition and theoretical studies suggest that many more members are stable and can be synthesized. This is very intriguing because new combinations of elements, and potentially new structures, can lead to further (tunable) properties. In this review, we focus on the synthesis science (including non‐conventional approaches) and structure of members less investigated, namely compounds with more exotic M‐, A‐, and X‐elements, for example nitrides and (carbo)nitrides, and the related family of MAB phases.

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Towards a mechanistic understanding of the sol–gel syntheses of ternary carbides

Abstract: TSol-gel chemistry, while being extremely established, is to this day not fully understood, and much of the underlaying chemistry and mechanisms are yet to be unraveled. Here, we elaborate on...

Cited by 5 publications

References 42 publications

Rapid Sol–Gel Synthesis Approach for the Preparation of the Magnetocaloric Antiperovskite Mn₃GaC

Rapid Sol–Gel Synthesis Approach for the Preparation of the Magnetocaloric Antiperovskite Mn₃GaC

Fabrication of Nano-sized Cr₂GaC with a Bottom-Up Approach for Lithium Storage

Extending the Chemistry of Layered Solids and Nanosheets: Chemistry and Structure of MAX Phases, MAB Phases and MXenes

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Towards a mechanistic understanding of the sol–gel syntheses of ternary carbides

Abstract: TSol-gel chemistry, while being extremely established, is to this day not fully understood, and much of the underlaying chemistry and mechanisms are yet to be unraveled. Here, we elaborate on...

Cited by 5 publications

References 42 publications

Rapid Sol–Gel Synthesis Approach for the Preparation of the Magnetocaloric Antiperovskite Mn3GaC

Rapid Sol–Gel Synthesis Approach for the Preparation of the Magnetocaloric Antiperovskite Mn3GaC

Fabrication of Nano-sized Cr2GaC with a Bottom-Up Approach for Lithium Storage

Extending the Chemistry of Layered Solids and Nanosheets: Chemistry and Structure of MAX Phases, MAB Phases and MXenes

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Product

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Rapid Sol–Gel Synthesis Approach for the Preparation of the Magnetocaloric Antiperovskite Mn₃GaC

Rapid Sol–Gel Synthesis Approach for the Preparation of the Magnetocaloric Antiperovskite Mn₃GaC

Fabrication of Nano-sized Cr₂GaC with a Bottom-Up Approach for Lithium Storage