Synthesis, crystal structure and spectroscopic properties of the NH4NiPO4·nH2O (n= 1,6) compounds; magnetic behaviour of the monohydrated phase

Goñi, Aintzane; Pizarro, José L.; Lezama, Luis; Barberis, G. E.; Arriortua, Marı́a I.; Rojo, Teófilo

doi:10.1039/jm9960600421

Cited by 46 publications

(27 citation statements)

References 19 publications

(1 reference statement)

Supporting

Mentioning

Contrasting

Order By: Relevance

“…This indicates that the product is crystalline compound with a higher crystallinity. All the diffraction peaks in the pattern are in agreement with that of orthorhombic NH 4 3 Comparing Figure 1a with Figure 1b, NH 4 NiPO 4 • 6H 2 O obtained in the presence of PEG-400 has stronger intensity diffractions than that of no PEG-400, which indicates that the former has higher crystallinity and more perfect crystalline structure than the latter. In other words, the PEG-400 plays an important role in the selfassembly of NH 4 NiPO 4 •6H 2 O crystals.…”

Section: Xrd Analysis Of the Product And Its Calcined Samplessupporting

confidence: 86%

“…3,[12][13][14] The band at 2375 cm -1 (OH mode) reveals that the water molecule in NH 4 NiPO 4 •6H 2 O forms a weak hydrogen bond, which is in agreement with that of NH 4 NiPO 4 •6H 2 O obtained by conventional precipitation method, 3,10 in which OH mode appears at a higher wavenumber by about 21 cm -1 than that of KMnPO 4 • H 2 O obtained by solid-state reaction at room temperature. 15 The deviation cause is not clear.…”

Section: Nhmentioning

confidence: 97%

“…The choice of synthetic method and raw materials is important, as it can lead to the production of several phases with predetermined structure types. 3 Ammonium phosphates of general formula NH 4 M II PO 4 • H 2 O were first described in 1864 by Debray. 4 The series of nickel(II) phosphates MINiPO 4 •H 2 O (M I ＝K, NH 4 ) was reported by Bassett and Bedwell in 1933.…”

Section: Introductionmentioning

confidence: 99%

See 2 more Smart Citations

Novel Method for Preparing NH₄NiPO₄·6H₂O: Hydrogen Bonding Coacervate Selective Self‐assembly

et al. 2010

Chin. J. Chem.

View full text Add to dashboard Cite

The single phase NH 4 NiPO 4 •6H 2 O was synthesized by solid-state reaction at room temperature using NiSO 4 •6H 2 O and (NH 4 ) 3 PO 4 •3H 2 O as raw materials. The NH 4 NiPO 4 •6H 2 O and its calcined products were characterized using X-ray powder diffraction (XRD), thermogravimetry and differential thermal analyses (TG/DTA), Fourier transform IR (FT-IR), ultraviolet-visible (UV-vis) absorption spectroscopy, and scanning electron microscopy (SEM). The results showed that the product dried at 80 ℃ for 3 h was orthorhombic NH 4 NiPO 4 •6H 2 O [space group Pmm2(25)], and surfactant polyethylene glycol (PEG)-400 can direct growth of crystal NH 4 NiPO 4 •6H 2 O. The thermal process of NH 4 NiPO 4 •6H 2 O experienced three steps, which involve the dehydration of the five crystal water molecules at first, and then deamination, dehydration of the one crystal water, intramolecular dehydration of the protonated phosphate groups together, at last crystallization of Ni 2 P 2 O 7 . The product of thermal decomposition at 150 ℃ for 2 h, orthorhombic NH 4 NiPO 4 •H 2 O, is layered compound with an interlayer distance of 0.8370 nm.

show abstract

Section: Xrd Analysis Of the Product And Its Calcined Samplessupporting

confidence: 86%

Section: Nhmentioning

confidence: 97%

Section: Introductionmentioning

confidence: 99%

See 1 more Smart Citation

Novel Method for Preparing NH₄NiPO₄·6H₂O: Hydrogen Bonding Coacervate Selective Self‐assembly

et al. 2010

Chin. J. Chem.

View full text Add to dashboard Cite

show abstract

“…In this compound the Co 2+ ions are coordinated by six O in fairly regular octahedra [18]. Assuming that the position of the six oxygen nearest to the Co 2+ are the same as those of the Nickel compound [18], and taking the average of their positions as the center of the octahedron, we choose two of the O and use them to determine an orthogonal system of axis.…”

Section: The Co 2+ In a Deformed Octahedral Symmetrymentioning

confidence: 99%

“…Assuming that the position of the six oxygen nearest to the Co 2+ are the same as those of the Nickel compound [18], and taking the average of their positions as the center of the octahedron, we choose two of the O and use them to determine an orthogonal system of axis. In the new system the x axis goes through the position of one of those two O, and the z axis is perpendicular to the plane determined by the two O and the center of the octahedron.…”

Section: The Co 2+ In a Deformed Octahedral Symmetrymentioning

confidence: 99%

Study of Co2+ in different crystal field environments

Foglio¹,

Barberis²

2006

Braz. J. Phys.

View full text Add to dashboard Cite

We consider the ESR of Co 2+ in different environments: in an regular octahedron (Co 2+ in a MgO crystal), in a deformed octahedron (Co 2+ in single crystals and powder samples of NH 4 NiPO 4 .6H 2 O) or in a trigonal bipyramid (Co 2+ in powders of Co 2 (OH)PO 4 and Co 2 (OH)AsO 4 ). We study the effect of the non-cubic crystal fields in the ESR of Co 2+ in the deformed octahedron, by employing the normal modes of this structure to simplify the systematic study of the effect of these fields. A similar study was done for the deformed trigonal bipiramid, and it was necessary to derive the normal modes of this complex that are relevant to our problem.

show abstract

Synthesis, X‐ray Powder Structure, and Magnetic Properties of Layered Ni^II Methylphosphonate, [Ni(CH₃PO₃)(H₂O)], and Ni^II Octadecylphosphonate, [Ni{CH₃‐(CH₂)₁₇‐PO₃}(H₂O)]

Bellitto¹,

Bauer²,

Ibrahim³

et al. 2003

Chemistry A European J

View full text Add to dashboard Cite

[Ni(CH(3)PO(3))(H(2)O)] (1) and [Ni(CH(3)-(CH(2))(17)-PO(3))(H(2)O)] (2) were synthesised by reaction of NiCl(2).6 H(2)O and the relevant phosphonic acid in water in presence of urea. The compounds were characterised by elemental and thermogravimetric analyses, UV-visible and IR spectroscopy, and their magnetic properties were studied by using a SQUID magnetometer. The crystal structure of 1 was determined "ab initio" from X-ray powder diffraction data and refined by the Rietveld method. The crystals of 1 are orthorhombic, space group Pmn2(1), with a=5.587(1), b=8.698(1), c=4.731(1) A. The compound has a hybrid, layered structure made up of alternating inorganic and organic layers along the b direction of the unit-cell. The inorganic layers consist of Ni(II) ions octahedrally coordinated by five phosphonate oxygen atoms and one oxygen atom from the water molecule. These layers are separated by bilayers of methyl groups and van der Waals contacts are established between them. A preliminary structure characterisation of compound 2 suggests the crystallisation in the orthorhombic system with the following unit-cell parameters: a=5.478(7), b=42.31(4), c=4.725(3) A. The oxidation state of the Ni ion in both compounds is +2, and the electronic configuration is d(8) (S=1), as determined from static magnetic susceptibility measurements above 50 K. Compound 1 obeys the Curie-Weiss law at temperatures above 50 K; the Curie (C) and Weiss (theta) constants were found to be 1.15 cm(3) K mol(-1) and -32 K, respectively. The negative value of theta indicates an antiferromagnetic exchange coupling between near-neighbouring Ni(II) ions. No sign of 3D antiferromagnetic long-range order is observed down to T=5 K, the lowest measured temperature. Compound 2 is paramagnetic above T=50 K, and the values of C and theta were found to be 1.25 cm(3) K mol(-1) and -24 K, respectively. Below 50 K the magnetic behavior of 2 is different from that of 1. Zero-field cooled (zfc) and field-cooled (fc) magnetisation plots do not overlap below T=21 K. The irreversible magnetisation, DeltaM(fc-zfc), obtained as a difference from fc and zfc plots starts to increase at T=20 K, on lowering the temperature, and it becomes steady at T=5 K. The presence of spontaneous magnetisation below T=20 K indicates a transition to a weak-ferromagnetic state for compound 2.

show abstract

Synthesis, crystal structure and spectroscopic properties of the NH₄NiPO₄·nH₂O (n= 1,6) compounds; magnetic behaviour of the monohydrated phase

Cited by 46 publications

References 19 publications

Novel Method for Preparing NH₄NiPO₄·6H₂O: Hydrogen Bonding Coacervate Selective Self‐assembly

Novel Method for Preparing NH₄NiPO₄·6H₂O: Hydrogen Bonding Coacervate Selective Self‐assembly

Study of Co2+ in different crystal field environments

Synthesis, X‐ray Powder Structure, and Magnetic Properties of Layered Ni^II Methylphosphonate, [Ni(CH₃PO₃)(H₂O)], and Ni^II Octadecylphosphonate, [Ni{CH₃‐(CH₂)₁₇‐PO₃}(H₂O)]

Contact Info

Product

Resources

About

Synthesis, crystal structure and spectroscopic properties of the NH4NiPO4·nH2O (n= 1,6) compounds; magnetic behaviour of the monohydrated phase

Cited by 46 publications

References 19 publications

Novel Method for Preparing NH4NiPO4·6H2O: Hydrogen Bonding Coacervate Selective Self‐assembly

Novel Method for Preparing NH4NiPO4·6H2O: Hydrogen Bonding Coacervate Selective Self‐assembly

Study of Co2+ in different crystal field environments

Synthesis, X‐ray Powder Structure, and Magnetic Properties of Layered NiII Methylphosphonate, [Ni(CH3PO3)(H2O)], and NiII Octadecylphosphonate, [Ni{CH3‐(CH2)17‐PO3}(H2O)]

Contact Info

Product

Resources

About

Synthesis, crystal structure and spectroscopic properties of the NH₄NiPO₄·nH₂O (n= 1,6) compounds; magnetic behaviour of the monohydrated phase

Novel Method for Preparing NH₄NiPO₄·6H₂O: Hydrogen Bonding Coacervate Selective Self‐assembly

Novel Method for Preparing NH₄NiPO₄·6H₂O: Hydrogen Bonding Coacervate Selective Self‐assembly

Synthesis, X‐ray Powder Structure, and Magnetic Properties of Layered Ni^II Methylphosphonate, [Ni(CH₃PO₃)(H₂O)], and Ni^II Octadecylphosphonate, [Ni{CH₃‐(CH₂)₁₇‐PO₃}(H₂O)]