2014
DOI: 10.1002/zaac.201300676
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Formation and Decomposition of Iron Nitrides Observed by in situ Powder Neutron Diffraction and Thermal Analysis

Abstract: Abstract. In order to gain more information on the formation and decomposition behavior of various iron nitrides from different starting materials in situ neutron diffraction and thermal analysis under application of different gas atmospheres and heating rates were carried out. The following phases were observed during these investigations: crystalline α-Fe, γ-FeN z , γЈ-Fe 4 N y , ε-Fe 3 N 1+x , ζ-Fe 2 N, FeCl 2 , [Fe(NH 3 ) 6 ]Cl 2 , Fe(NH 3 ) 2 Cl 2 , and amorphous Fe(NH 3 )Cl 2 . In situ neutron diffractio… Show more

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Cited by 42 publications
(59 citation statements)
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“…Other synthesis methods leading to metal ammoniates are reaction of metal halides with gaseous ammonia or reaction of metals with ammonia donors (e.g., NH 4 [94][95][96] and [B(NH 3 ) 5 Cl]Cl 2 with B = Al [84], Cr [97], Co [97,98], Rh [97,99], Ru [97], Os [97]. Further ammoniates may be obtained by thermal decomposition of higher ammoniates.…”
Section: Ammoniates Of Metal Halidesmentioning
confidence: 99%
“…Other synthesis methods leading to metal ammoniates are reaction of metal halides with gaseous ammonia or reaction of metals with ammonia donors (e.g., NH 4 [94][95][96] and [B(NH 3 ) 5 Cl]Cl 2 with B = Al [84], Cr [97], Co [97,98], Rh [97,99], Ru [97], Os [97]. Further ammoniates may be obtained by thermal decomposition of higher ammoniates.…”
Section: Ammoniates Of Metal Halidesmentioning
confidence: 99%
“…In contrast, bulk Fe 4 Nb egins to decompose at 600 8C, which arises from the cohesion energy of iron given the larger fraction of Fe-Fe bonds that have to be broken and the solid-state diffusion of Na toms towards the surface. [21,22] As can be seen in Figure 7b,t he existence of at least two types of nitrides is further supported by changes observed in the traces obtainedd uring NH 3 -TPD after the catalytic reaction. First of all, the onset of both H 2 and N 2 evolution is located at as imilar temperature of around 400 8C.…”
Section: Surface Analysis By Nh 3 -Tpdmentioning
confidence: 63%
“…It is well known that iron forms varioust ypes of nitrides. [20] As has been shown by in situ neutron diffraction experiments during the sequential thermal decomposition of z-Fe 2 N, [21] formation NH 3 -TPD experiments were additionally carried out after the reduced samples were subjected to at emperature programmed ammonia decomposition cycle up to 515 8C. Figure S2 shows the qualitative NH 3 ,H 2 ,a nd N 2 traces obtained during the catalytic reaction.…”
Section: Surface Analysis By Nh 3 -Tpdmentioning
confidence: 95%
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“…Chromium powder was reacted in a silica glass tube [42,43] in the high temperature resistive furnace (HTF) of the SPODI diffractometer (FRM-II, Garching) with flowing ammonia (60 cm 3 ·min -1 ). During the reaction powder neutron diffraction was recorded with an effective time resolution of 90 min and an angular resolution of Δ(2Θ) = 0.1° (Figure 1).…”
Section: Synthesis Of Chromium Nitride From Chromium and Ammoniamentioning
confidence: 99%