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The magnetic properties, crystal and magnetic structures of Nd5 SixGe4-x were investigated by ac susceptibility and high resolution neutron powder diffraction. The magnetic and crystalline phase diagrams were derived. Four distinct structures exist in the Nd 5SixGe4-x system: Gd5Ge 4-type [O(II)], Gd5Si2Ge2-type (M), Gd5Si4-type [O(I)], and Zr5Si4-type (T). The refinements of the neutron powder diffraction patterns revealed that the Nd5SixGe4-x compounds exhibit mixed ferro-antiferromagnetic structures. The ac susceptibility measurements showed that the magnetic ordering temperature of Nd5SixGe 4-x increases slightly with increasing silicon content, except that it increases by a factor of 2 in the orthorhombic Gd5Si 4-type [O(I)] phase region. The abrupt change of the magnetic ordering temperature between x = 2.25 and x = 2.5, where the monoclinic Gd5Si 2Ge2-type (M) structure changes to the orthorhombic Gd 5Si4-type [O(I)] structure, suggested that a first order magnetostructural transition likely takes place in this narrow composition range (2.25 < x < 2.5). The investigation of Nd5Si2.335 Ge1.665 revealed that Nd5Si2.335Ge 1.665 adopts the Gd5Si2Ge2-type (M) structure and undergoes a first order magnetostructural transition from the paramagnetic-monoclinic Gd5Si2Ge2-type (M) structure to the orthorhombic Gd5Si4-type [O(I)] structure upon cooling. The T1-T1 bonds increases by ∼1 A when the the Gd 5Si4-type [O(I)] structure (10 K) transforms to the Gd 5Si2Ge2-type (M) structure (140 K). The giant magnetocaloric effect is not observed in Nd5Si2.335Ge 1.665 probably due to the co-existence of the M phase and the O(I) phase. The maximum magnetic entropy change in Nd5Si2.335Ge 1.665 is 7.3 J/kg K for magnetic field change from 0 to 7 Tesla, which is similar to that obtained in Nd5Si1.5Ge2.5, the neighboring phase O(I).

The thermal decompositions of a series of amide complexes of nickel(II) chloride have been studied. Thermochemical, kinetic, structure and solid-state stability correlations have been investigated. Complexes containing homologous amide ligands (L) of the form NiLCℓ₂, Ni₃L₂Cℓ₆, Ni₃LCℓ₆, NiL₂Cℓ₂(2H₂0) and ML₂Cℓ₂ (where M = Ni(II), Co(II) or Cu(II)) have been prepared. Chemical analysis, spectral and thermogravimetric measurements were used to characterize the complexes and their decomposition stoichiometries. Three sets of reactions were identified as yielding stable products in a single step: (i) NiLCℓ₂ (s) → NiCℓ₂ (s) + L (g) (ii) Ni₃LCℓ₆ (s) → 3NiCℓ₂ (s) + 2L (g) (iii) Ni₃LCℓ₆ (s) → 3NiCℓ₂ (s) + L (g) Characterization of the processes in the ML₂Cℓ₂ and NiL₂Cℓ₂(2H₂0) complexes was not straightforward. Reaction enthalpies (ΔH) were determined using DSC. The orders of the reaction onset temperatures (Tc), peak temperatures (Tmax) and ΔHL values for the NiCℓ₂ system were: N-methylacetamide < acetamide < N-methylformamide, suggesting the importance of steric hindrance of the methyl-substituent groups in the amide skeleton. In the Ni₃LCℓ₆, NiL₂Cℓ₂(2H₂0) and ML₂Cℓ₂ systems no simple orders could be deduced. The Te and Tmax sequences obtained from analogous metal(II) chloride complexes indicated that the copper(II) complexes were the least stable. The kinetics of the loss of L from NiLCℓ₂ complexes were investigated using isothermal TG, non-isothermal TG and DSC measurements. The contracting geometry models described the course of the decompositions in the most satisfactory manner. Apparent activation energies ( Ea) were estimated from Arrhenius plots of rate coefficients from: (i) an approximate zero-order relationship, (ii) the contracting-area (R2) and contracting-volume (R3) equations, (iii) a new empirical (B2) expression, (iv) the half-life ( 1/t₀.₅) and (v) the characteristic feature of the rate-time curve ( 1/tmax/2 ). The non-dependence of Ea on the rate equation used supports the reliability of the kinetic parameters. Non-isothermal experiments were analyzed by the Coats-Redfern, the modified BorchardtDaniels and the Kissinger methods. Arrhenius parameters were in keeping with results from the isothermal kinetic measurements. The values of Ea obtained for the NiLCℓ₂ system increased with an increase in basicity of the amide ligands. No straightforward correlation was found between Ea and Te, Tmax, ΔHL or spectral properties.

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M.S. / Materials Science and Engineering / The most fundamental step in the development of a predictive model for microstructure and residual stress distribution in steels is the accurate representation of the transient temperature field. Three constituents of a database of thermophysical properties, namely the thermal conductivity, volumetric specific heat capacity and convective heat transfer coefficient, were isolated and their effects quantified on the accuracy of temperature field predictions using finite element analysis (FEA). The most critical parameter in the heat transfer process was ultimately identified to be the temperature dependent convective heat transfer coefficient. It was determined using an inverse heat transfer method, which was successfully applied to accurately establish the thermal boundary conditions for an arbitrary 3D steel geometry. The temperature dependency of the volumetric specific heat capacity in the transformation range of temperatures has to be known a priori, for which a reliable model describing alloy dependent reaction kinetics has to be developed first. Thermal conductivity and its dependency on temperature have secondary effects on the accuracy of FEA predictions. The impact of the outcome of this study lies in its relevance to the heat treatment industry.

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