Recently, two-dimensional (2D) materials and their heterostructures have attracted considerable attention in gas sensing applications. In this work, we synthesized 2D MoS₂@MoO₃ heterostructures through post-sulfurization of α-MoO₃ nanoribbons grown via vapor phase transport (VPT) and demonstrated highly sensitive NO₂ gas sensors based on the hybrid heterostructures. The morphological, structural, and compositional properties of the MoS₂@MoO₃ hybrids were studied by a combination of advanced characterization techniques revealing a core-shell structure with the coexistence of 2H-MoS₂ multilayers and intermediate molybdenum oxysulfides on the surface of α-MoO₃. The MoS₂@MoO₃ hybrids also exhibit room-temperature ferromagnetism, revealed by vibrating sample magnetometry (VSM), as a result of the sulfurization process. The MoS₂@MoO₃ gas sensors display a p-type-like response towards NO₂ with a detection limit of 0.15 ppm at a working temperature of 125 °C, as well as superb selectivity and reversibility. This p-type-like sensing behavior is attributed to the heterointerface of MoS₂-MoO₃ where interfacial charge transfer leads to a p-type inversion layer in MoS₂, and is enhanced by magnetic dipole interactions between the paramagnetic NO₂ and the ferromagnetic sensing layer. Our study demonstrates the promising application of 2D molybdenum hybrid compounds in gas sensing applications with a unique combination of electronic and magnetic properties.

Crystalline Ni₂B, Ni₃B, and Ni₄B₃ are synthesized by a single-step method using autogenous pressure from the reaction of NaBH₄ and Ni precursors. The effect of reaction temperature, pressure, time, and starting materials on the composition of synthesized products, particle morphologies, and magnetic properties is demonstrated. High yields of Ni₂B (>98%) are achieved at 2.3–3.4 MPa and ~670 °C over five hours. Crystalline Ni₃B or Ni₄B₃ form in conjunction with Ni₂B at higher temperature or higher autogenous pressure in proportions influenced by the ratios of initial reactants. For the same starting ratios of reactants, a longer reaction time or higher pressure shifts equilibria to lower yields of Ni₂B. Using this approach, yields of ~88% Ni₄B₃ (single phase orthorhombic) and ~72% Ni₃B are obtained for conditions 1.9 MPa < P_max < 4.9 MPa and 670 °C < T_max < 725 °C. Gas-solid reaction is the dominant transformation mechanism that results in formation of Ni₂B at lower temperatures than conventional solid-state methods.

Precise compositional analyses at spatial resolution <1 μm, combined with structure determination using bulk (i.e. powder XRD) and individual grain (i.e. EBSD) techniques, show that both β-Fe_xSe and δ-Fe_xSe form as solids in a two-phase field above and below the apparent peritectic temperature of 457 °C. Microstructures show that β-Fe_xSe and δ-Fe_xSe form together via exsolution when cooled from this two-phase field; evident when annealing time and temperature are optimised. Using a facile one-pot method with elemental Fe:Se reactant ratios ranging from 0.95 to 1.14, β-Fe_xSe occurs as the predominant phase in association with hexagonal δ-Fe_xSe in the temperature range 330 °C < T_max < 750 °C, where T_max is the sintering temperature. Maximum yield of β-Fe_xSe occurs after sintering at T_max > 690 °C with annealing at 420 °C for ∼24 h. We define a modified phase diagram that includes this two phase field with β-Fe_xSe and δ-Fe_xSe for 1.02 < x < 0.90 and a second two phase field with β-Fe_xSe and α-Fe for 1.08 < x < 1.02. This revised phase diagram for Fe:Se ∼ 1.0 suggests that the peretectic transition nominally identified at x = 1.04 is not evident.

THz/Far infrared synchrotron absorption experiments on pure and doped MgB₂samples show that the absorption spectral weight at low wavenumber (i.e., <110 cm⁻¹) evolves as the temperature is reduced to 10 K.

We demonstrate synthesis of the ternary intermetallic MgNi₃B₂ using autogenous pressure from the reaction of NaBH₄ with Mg and Ni metal powder. The decomposition of NaBH₄ to H₂ and B₂H₆ commences at low temperatures in the presence of Mg and/or Ni and promotes formation of Ni-borides and MgNi₃B₂ with the increase in temperature. MgNi₃B₂ aggregates with Ni-boride cores are formed when the reaction temperature is >670 °C and autogenous pressure is >1.7 MPa. Morphologies and microstructures suggest that solid–gas and liquid–gas reactions are dominant mechanisms and that Ni-borides form at a lower temperature than MgNi₃B₂. Magnetic measurements of the core-shell MgNi₃B₂ aggregates are consistent with ferromagnetic behaviour in contrast to stoichiometric MgNi₃B₂ which is diamagnetic at room temperature.