Tantalum as a High‐Temperature Container Material for Reduced Halides

Corbett, John D.; Simon, Arndt

doi:10.1002/9780470132531.ch3

Cited by 75 publications

(5 citation statements)

References 7 publications

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“…Reactions were carried out in Nb tubes, which were welded closed under a partial pressure of Ar and sealed in evacuated silica jackets. GdI 3 was synthesized by reaction of Gd metal turnings with HgI 2 , as described in the literature, and sublimed at least three times. , The transition metal iodides were synthesized from the elements and sublimedFeI 2 under dynamic vacuum and MnI 2 and CoI 2 under static vacuum. CsI (Aesar 99%) was sublimed under dynamic vacuum and stored in ampules until use.…”

Section: Methodsmentioning

confidence: 99%

Ferromagnetic Coupling in Hexanuclear Gadolinium Clusters

et al. 2006

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The magnetic susceptibilities of hexanuclear gadolinium clusters in the compounds Gd(Gd6ZI12) (Z = Co, Fe, or Mn) and CsGd(Gd6CoI12)2 are reported and subjected to theoretical analysis with the help of density functional theory (DFT) computations. The single-crystal structure of Gd(Gd6CoI12) is reported here as well. We find that the compound with a closed shell of cluster bonding electrons, Gd(Gd6CoI12), exhibits the effects of antiferromagnetic coupling over the entire range of temperatures measured (4-300 K). Clusters with unpaired, delocalized cluster bonding electrons (CBEs) exhibit enhanced susceptibilities consistent with strong ferromagnetic coupling, except at lower temperatures (less than 30 K) where intercluster antiferromagnetic coupling suppresses the susceptibilities. The presence of two unpaired CBEs, as in [Gd6MnI12]3-, yields stronger coupling than when just one unpaired CBE is present, as in [Gd6FeI12]3- or [Gd6CoI12]2-. DFT calculations on model molecular systems, [Gd6CoI12](OPH3)6 and [Gd6CoI12]2(OPH3)10, indicate that the delocalized cluster bonding electrons are highly effective at mediating intracluster ferromagnetic exchange coupling between the Gd atom 4f7 moments and that intercluster coupling is expected to be antiferromagnetic. The DFT calculations were used to calculate the relative energies of various 4f7 spin patterns and form the basis for construction of a simple spin Hamiltonian describing the coupling within the [Gd6CoI12] cluster.

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Section: Methodsmentioning

confidence: 99%

Ferromagnetic Coupling in Hexanuclear Gadolinium Clusters

et al. 2006

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“…The title compounds were synthesized in welded Nb tubes sealed in evacuated fused silica jackets. The rare earth triiodides were prepared by oxidation of the rare earth elements with HgI 2 , as described in the literature, and purified in at least three vacuum sublimations. , Transition metal iodides were prepared from the elements and sublimed under static vacuum. CsI (Aesar 99%) and KI (Fisher Scientific 99.95%) were sublimed under dynamic vacuum and stored in ampules before use.…”

Section: Methodsmentioning

confidence: 99%

CsR(R₆CoI₁₂)₂(R = Gd, Er) and (CeI)_0.26(Ce₆MnI₉)₂: Two New Structure Types Featuring R₆Z Clusters

Sweet

Hughbanks

2006

Inorg. Chem.

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Compounds adopting two new structure types containing discrete lanthanide clusters have been found, CsR(R6CoI12)2 (R = Gd or Er) and (CeI)0.26(Ce6MnI9)2. CsEr(Er6CoI12)2 and CsGd(Gd6CoI12)2 were synthesized in reactions of CsI, RI3, CoI2, and R metals (3:19:6:23) heated to 750 degrees C for 500 h followed by slow cooling (0.1 degrees C/min). The X-ray crystal structure of CsEr(Er6CoI12)2 was solved in the Pa3 space group with a = 18.063(2) A at 250 K (Z = 4, R1 [I > 2sigma(I)] = 0.0459). (CeI)0.26(Ce6MnI9) was synthesized by combining KI, CeI3, MnI2, and Ce metal and heating to 850 degrees C for 500 h. The single-crystal X-ray structure for (CeI)0.26(Ce6MnI9)2 was solved in the trigonal, P3 (147) space group with lattice parameters of a = 11.695(1) A and c = 10.8591(2) A (Z = 2, R1 [I > 2sigma(I)] = 0.0895). Elemental analyses (X-ray photoelectron spectroscopy (XPS) and atomic absorption spectroscopy (AAS)) were performed and show the absence of potassium in the structure. A disorder model was refined for the atoms in the large cavity. The magnetic susceptibility data for CsGd(Gd6CoI12)2 is consistent with strong intracluster ferromagnetic coupling, but intercluster antiferromagnetic coupling suppresses the susceptibility below 70 K.

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“…Better results can be obtained with the more inert container materials niobium and tantalum. Information on the self-fabrication of niobium and tantalum ampoules can be found in Corbett and Simon (1983) and Pöttgen et al (1999). The metal containers are usually enclosed in quartz Schlenk tubes or sealed evacuated silica tubes for oxidation protection.…”

Section: Synthesis Conditions Binary Lithium Pnictidesmentioning

confidence: 98%

Lithium transition metal pnictides – structural chemistry, electrochemistry, and function

Winter

Pöttgen

Greiwe

et al. 2014

Reviews in Inorganic Chemistry

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Lithium-transition metal (T)-pnictides (Pn = P, As, Sb, Bi) are an interesting class of materials with greatly differing crystal structures. The transition metal and pnictide atoms build up covalently bonded networks that leave cavities or channels for the lithium atoms. Depending on the bonding of lithium to the polyanionic network, one observes mobility of the lithium atoms. The crystal chemistry, chemical bonding, 7 Li solid-state NMR, and the electrochemical behavior of the pnictides are reviewed. The structural chemistry is compared with related tetrelides.

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Tantalum as a High‐Temperature Container Material for Reduced Halides

Cited by 75 publications

References 7 publications

Ferromagnetic Coupling in Hexanuclear Gadolinium Clusters

Ferromagnetic Coupling in Hexanuclear Gadolinium Clusters

CsR(R₆CoI₁₂)₂(R = Gd, Er) and (CeI)_0.26(Ce₆MnI₉)₂: Two New Structure Types Featuring R₆Z Clusters

Lithium transition metal pnictides – structural chemistry, electrochemistry, and function

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Tantalum as a High‐Temperature Container Material for Reduced Halides

Cited by 75 publications

References 7 publications

Ferromagnetic Coupling in Hexanuclear Gadolinium Clusters

Ferromagnetic Coupling in Hexanuclear Gadolinium Clusters

CsR(R6CoI12)2(R = Gd, Er) and (CeI)0.26(Ce6MnI9)2: Two New Structure Types Featuring R6Z Clusters

Lithium transition metal pnictides – structural chemistry, electrochemistry, and function

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CsR(R₆CoI₁₂)₂(R = Gd, Er) and (CeI)_0.26(Ce₆MnI₉)₂: Two New Structure Types Featuring R₆Z Clusters