Hydrothermal Synthesis and Structure of Fe(NH3)2PO4:  A Novel Monophosphate

Salvadó, Miguel A.; Pertierra, Pilar; Garcı́a-Granda, Santiago; Espina, Aránzazu; Trobajo, Camino; Garcı́a, José R.

doi:10.1021/ic990879n

Cited by 20 publications

(16 citation statements)

References 22 publications

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“…Using this new hydrothermal route, the diamin iron(III) phosphate large crystals were carried out. The scanning electron microscopy (SEM) image of Fe(NH 3 ) 2 PO 4 displayed in Figure 1 suggests the morphology of the sample is constituted by fibres forming compact blocks, unlike polycrystalline phases (hydrogenated and deuterated) [11,13].…”

Section: Morphological and Structural Resultsmentioning

confidence: 99%

“…144.90(10) P(1)-O(3)-Fe (1) 132.56(9) Fe(1)N(1)H (11) 109.3 Fe(1)N(1)H (12) 115.6 H(11)N(1)H (12) 105.1 Fe(1)N(2)H (21) 104.8 Fe(1)N(2)H (22) 124.6 H(21)N(2)H (22) 106.4 Symmetry transformations used to generate equivalent atoms:…”

Section: Bond Lengths (å) Bond Angles (Deg)mentioning

confidence: 99%

“…The polycrystalline diamin iron(III) phosphate, Fe(NH 3 ) 2 PO 4 , and its deuterated phase Fe(ND 3 ) 2 PO 4 had been previously synthesized and structurally characterized in our laboratory [11,12]. The nuclear diagram obtained from the powder neutron diffraction data (PND) of the deuterated sample between 30 and 300 K, complementary to the powder X-ray diffraction (PXRD), allowed us to analyze in depth the structural phase transition: orthorhombic (Pnma space group) crystal structure at room temperature and monoclinic structure (P2 1 /n space group) below 226(5) K [12].…”

Section: Introductionmentioning

confidence: 99%

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Kinetic Analysis of the Thermal Decomposition of Iron(III) Phosphates: Fe(NH3)2PO4 and Fe(ND3)2PO4

Iglesias

Huidobro

Alfonso

et al. 2020

IJMS

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The hydrothermal synthesis and both the chemical and structural characterization of a diamin iron phosphate are reported. A new synthetic route, by using n-butylammonium dihydrogen phosphate as a precursor, leads to the largest crystals described thus far for this compound. Its crystal structure is determined from single-crystal X-ray diffraction data. It crystallizes in the orthorhombic system (Pnma space group, a = 10.1116(2) Å, b = 6.3652(1) Å, c = 7.5691(1) Å, Z = 4) at room temperature and, below 220 K, changes towards the monoclinic system P2 1 /n, space group. The in situ powder X-ray thermo-diffraction monitoring for the compound, between room temperature and 1100 K, is also included. Thermal analysis shows that the solid is stable up to ca. 440 K. The kinetic analysis of thermal decomposition (hydrogenated and deuterated forms) is performed by using the isoconversional methods of Vyazovkin and a modified version of Friedman. Similar values for the kinetic parameters are achieved by both methods and they are checked by comparing experimental and calculated conversion curves.

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Section: Morphological and Structural Resultsmentioning

confidence: 99%

Section: Bond Lengths (å) Bond Angles (Deg)mentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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Kinetic Analysis of the Thermal Decomposition of Iron(III) Phosphates: Fe(NH3)2PO4 and Fe(ND3)2PO4

Iglesias

Huidobro

Alfonso

et al. 2020

IJMS

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“…All have the general formula A 2-x B 2 O 6 (O, OH, F)ÁnH 2 O, where A may belong to a long list of metal ions: lead, iron, calcium, potassium, bismuth, sodium, barium, cerium, caesium, tin, strontium, thorium, uranium, yttrium, zirconium and/or antimony, while B represents an octahedral site in the structure and can be any of the following metal ions: niobium, tungsten, tin, tantalum and/or titanium. In the course of our systematic research, the hydrothermal synthesis has been used to synthesise new materials exhibiting promising ion-exchange properties [3][4][5][6][7][8][9][10], such as ammonium-titanium(IV) phosphate, (NH 4 ) 0.79 (P 1.14 Ti 0.86 )O 3.93 (OH) 2.07 , with a pyrochlore-type structure [11]. Its framework is made up of MO 6 (M = P, Ti) octahedra connected by vertices, where M atoms occupy the 16c site, the 8b site is partially occupied by NH 4 ?…”

Section: Introductionmentioning

confidence: 99%

Morphological study and thermal behaviour of an ammonium-titanium(IV) phosphate with pyrochlore-type structure

García-Glez

Alfonso

Huidobro

et al. 2016

J Therm Anal Calorim

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Polycrystalline ammonium-titanium(IV) phosphate with pyrochlore-type structure has been obtained under hydrothermal conditions and characterised by powder X-ray thermodiffractometry (HT-pXRD), electron microscopy (SEM and TEM) and thermal analysis (TG/ SDTA-MS). Moreover, the activation energy of thermal decomposition has been calculated as a function of the extent of conversion applying the Vyazovkin isoconversional method to the thermogravimetric data. The sample is constituted by nearly spherical plate-like particles (diameter ca. 25 nm) which in an aqueous medium are prone to auto-assembling to originate polycrystalline fibres. Thermogravimetric analysis showed significant differences between the thermal decomposition behaviour in inert (N 2 ) and oxidiser (O 2 ) atmospheres (e.g. the total mass loss), revealing the presence of a fraction of P(III) which oxidises to P(V) when the N 2 atmosphere is replaced at 823 K by O 2 atmosphere.

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“…The mono-dimensional order occurs with the formation of a unusual link between ammonia molecules and zinc atoms. In our knowledge, the process described here constitutes the first example of dimensionality change in solid phase promoted by a solid-gas interaction at room temperature [3][4][5][6]. …”

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confidence: 99%

Old materials in the nanoworld: cases of shape and dimensionality control

García-Granda¹

2013

Acta Cryst Sect A

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The versatility of phosphate materials concerning microscopic dimensionality and nanostructural shape is shown throughout two recent examples. Trialkylammonium-titanium(IV) phosphate nanomaterials with different shape, size and crystallinity are reported. These nanomaterials have been prepared by using microemulsionmediated solvothermal methods. Both morphology and structure are controllable, and this simple synthesis-route will be used to prepare whisker-, rod-, platelet-like and tubular hybrid nanomaterials [1,2]. It was found that the reaction temperature, concentration of reagents and molar ratio of the reactants have significant effect on the structure, shape and size of the nanocrystals formed. Experimental results indicate that the synthesis of TAA/TiP metastable phases can be controlled, and we are making efforts in this way. NH 4 Zn 2 (PO 4 )(HPO 4 ) (1) two-dimensional zinc phosphate, via ammonia vapor interaction at room temperature, transform to NH 4 Zn(NH 3 ) PO4 (2) one-dimensional novel compound. By partial ammonia desorption (outgassing at room temperature or by soft thermal treatment) 2 transform to NH 4 ZnPO 4 (3) with a well-known ABW-zeolitic topology. The crystal structure of 1 was refined using single-crystal neutron diffraction data, while that the crystal structure of 2 was solved ab initio using synchrotron powder X-ray diffraction. The structure of three compounds include extra-framework ammonium cations to the 4-fold coordinated zinc (ZnO 4 tetrahedra for 1 and 3, and ZnO 3 N tetrahedra for 2) and phosphorus (PO 4 tetrahedra) with bi-, mono-or three-dimensional linkages, respectively for 1, 2 or 3. The mono-dimensional order occurs with the formation of a unusual link between ammonia molecules and zinc atoms. In our knowledge, the process described here constitutes the first example of dimensionality change in solid phase promoted by a solid-gas interaction at room temperature [3][4][5][6]. Acknowledgements

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Hydrothermal Synthesis and Structure of Fe(NH₃)₂PO₄: A Novel Monophosphate

Cited by 20 publications

References 22 publications

Kinetic Analysis of the Thermal Decomposition of Iron(III) Phosphates: Fe(NH3)2PO4 and Fe(ND3)2PO4

Kinetic Analysis of the Thermal Decomposition of Iron(III) Phosphates: Fe(NH3)2PO4 and Fe(ND3)2PO4

Morphological study and thermal behaviour of an ammonium-titanium(IV) phosphate with pyrochlore-type structure

Old materials in the nanoworld: cases of shape and dimensionality control

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