Low-temperature CVD of η-Mn3N2−x from bis[di(tert-butyl)amido]manganese(II) and ammonia

Abstract

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A Molecular Approach to Manganese Nitride Acting as a High Performance Electrocatalyst in the Oxygen Evolution Reaction

“…Up to now only af ew procedures forming manganese nitrides have been reported using am olecular approach, but they gave merely air-sensitive materials. [17,18] Herein we present the novel molecular route to air-stable, reliably scalable,a nd phase-pure crystalline manganese nitride (Mn 3 N 2 ), which displayed an excellent performance as pre-catalyst in OER with outstanding durability in alkaline media. Mn 3 N 2 was successfully prepared in astraightforward route through ammonolysis of manganocene [(C 5 H 5 ) 2 Mn] as amolecular precursor at 700 8 8Cfor 12 husing atube furnace (Scheme 1; see also the Supporting Information).…”

“…[20,21] TheN1s spectrum exhibited ap eak at 396.3 eV for all catalysts (as-prepared, after CV and CP) that can be assigned to elemental nitrogen (Supporting Information , Figure S21). [17] TheO1s XPS spectra of OER CV and OER CP displayed two peaks,one at about 529.7 eV corresponding to formation of metal-oxygen bonds (MnO x )o nt he surface owing to corrosion, whereas the second peak at 531.1 eV is largely related to oxyhydroxide/hydroxides( Supporting Information, Figure S21). [30] Incidentally,s imilar modifications can also be observed for Mn 2 O 3 with the formation of amorphous MnO x layers on the surface and no drastic increase in the oxidation state of Mn 2 O 3 occurred after electrochemical OER in comparison to the as-prepared material.…”

Plasma-Enhanced Atomic Layer Deposition of Low Resistivity and Ultrathin Manganese Oxynitride Films with Excellent Resistance to Copper Diffusion

“…Only one diffraction peak located at 2θ = 42.9°appears in all of the films, which should be associated with Mn 3 N 2 (006) orientation. 31 Moreover, as the growth temperature increases from 225 to 300 °C, the peak intensity increases gradually, and the calculated average grain size increases from 4.9 to 6.5 nm according to the Sherrer formula. This indicates that a higher growth temperature is in favor of the growth of the Mn 3 N 2 (006) plane, which is not perpendicular to the substrate.…”

Convenient synthesis of nanocrystalline powders of phase-pure manganese nitride η-Mn3N2

“…In the related area, numerous metal (trimethylsilyl)amides M[N(Si(CH 3 ) 3 ) 2 ] n , M = metal, upon reactions with ammonia have been useful precursors to metal nitride nanoparticles via thermal decomposition/ deamination of the postulated metal amides M(NH 2 ) n as outlined in a recent review [32]. Analogous chemistry was also successfully explored by some of us to prepare nanocrystalline powders of gallium nitride GaN [33][34][35], aluminum nitride AlN [36,37], and titanium nitride TiN [38,39] 2 ] 2 , in the system with ammonia was successfully used to make thin films of mixed-phase manganese nitrides, possibly, via transamination and subsequent deamination reactions of the transient manganese amide/imide [23]. The Mn[N(Si(CH 3 ) 3 ) 2 ] 2 itself was applied as a volatile precursor for deposition of thin films of metallic manganese [40][41][42].…”

“…Reactive sputtering of the Mn-disc in the Ar/N 2 mixture produced MnN that decomposed to Mn 3 N 2 at 758 K [22]. Low-temperature CVD processing in the system bis[di(tert-butyl)amido]manganese(II) and ammonia afforded thin films of mixedphase manganese polytypes including g-Mn 3 N 2 [23]. Mn 3 N 2 was also synthesized by high-pressure (10 GPa) and high-temperature (1800 K) reactions of elemental Mn and N 2 [24].…”