| 1. |
- Hemamala, U. L. C., et al.
(författare)
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High-pressure Raman and infrared study of ZrV2O7
- 2007
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Ingår i: Solid State Communications. - : Elsevier BV. - 0038-1098 .- 1879-2766. ; 141:12, s. 680-684
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Tidskriftsartikel (refereegranskat)abstract
- The room-temperature Raman and infrared spectra of zirconium vanadate (ZrV2O7) were observed up to pressures of 12 GPa and 5.7 GPa, respectively. The frequencies of the optically active modes at ambient pressure were calculated using direct methods and compared with experimental values. Average mode Gruneisen parameters were calculated for the Raman and infrared active modes. Changes in the spectra under pressure indicate a phase transition at similar to 1.6 GPa, which is consistent with the previously observed a (cubic) to (pseudo-tetragonal) phase transition, and changes in the spectra at similar to 4 GPa are consistent with an irreversible transformation to an amorphous structure.
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| 2. |
- Krogh Andersen, A.M., et al.
(författare)
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Ab Initio Structure Determination and Rietveld Refinement of a High-Temperature Phase of Zirconium Hydrogen Phosphate and a New Polymorph of Zirconium Pyrophosphate from In-Situ Temperature-Resolved Powder Diffraction Data.
- 2000
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Ingår i: Acta Crystallographica Section B. - : Wiley. - 0108-7681. ; 56:4, s. 618-625
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Tidskriftsartikel (refereegranskat)abstract
- The collected in situ temperature-resolved synchrotron powder data revealed that the transformation of the recently reported three-dimensional τ-Zr(HPO4)2 to cubic ZrP2O7 goes through two intermediate phases. The first intermediate phase, ρ-Zr(HPO4)2, is formed in a reversible phase transition at 598 K, which involves both rearrangement and disordering of the hydrogen phosphate groups of τ-Zr(HPO4)2. At 688 K condensation of the hydrogen phosphate groups leads to the formation of the second intermediate, a new polymorph of zirconium pyrophosphate (β-ZrP2O7). Heating above 973 K results in the gradual transformation of β-ZrP2O7 to cubic zirconium pyrophosphate (α-ZrP2O7). The crystal structures of the two intermediate phases were solved from the in situ powder diffraction data using direct methods and refined using the Rietveld method. Both phases are orthorhombic, space group Pnnm and Z = 2. The lattice parameters for the two phases are: ρ-Zr(HPO4)2: a = 8.1935 (2), b = 7.7090 (2), c = 5.4080 (1) Å; β-ZrP2O7: a = 8.3127 (5), b = 6.6389 (4), c = 5.3407 (3) Å. The formation mechanism for the new zirconium pyrophosphate polymorph, β-ZrP2O7, is discussed in relation to structurally restricted soft chemistry
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| 3. |
- Krogh Andersen, A.M., et al.
(författare)
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Determination of the Formation Regions of Titanium Phosphates. Determination of the Crystal Structure of β-Titanium Phosphate, Ti(PO4)(H2PO4), from Neutron Powder Data.
- 1998
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Ingår i: Journal of solid state chemistry. - : Elsevier. - 1095-726X .- 0022-4596. ; 140:2, s. 266-271
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Tidskriftsartikel (refereegranskat)abstract
- The formation region of the various types of layered titanium hydrogen phosphate hydrates was investigated. The materials were prepared by hydrothermal methods, treating amorphous titanium phosphate with phosphoric acid (8 to 16M) in the temperature range 175 to 250°C. The materials obtained were:α-Ti(HPO4)2·H2O,γ-Ti(PO4)(H2PO4)·2H2O, and its anhydrous formβ-Ti(PO4)(H2PO4). The structure ofβ-Ti(PO4)(H2PO4) has been determined by Rietveld powder refinement of high resolution neutron diffraction data. The structure is refined in the monoclinic space groupP21/n(No. 14). The unit cell parameters are:a=18.9503(4) Å,b=6.3127(1) Å,c=5.1391(1) Å,β=105.366(2)°;Z=4. The final agreement factors were:Rp=2.9% andRwp=3.8%. The structure ofβ-Ti(PO4)(H2PO4) is built from TiO6octahedra linked together by tertiary phosphate (PO4) and dihydrogen phosphate ((OH)2PO2) tetrahedra. The layers are held together by hydrogen bonds.
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| 4. |
- Krogh Andersen, A.M., et al.
(författare)
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High-pressure properties of TiP2O7, ZrP2O7 and ZrV2O7
- 2001
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Ingår i: Journal of Applied Crystallography. - : Wiley. - 0021-8898. ; 34:1, s. 7-12
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Tidskriftsartikel (refereegranskat)abstract
- High-pressure synchrotron X-ray powder diffraction studies of TiP2O7, ZrP2O7 and ZrV2O7 have been performed. The ZrV2O7 structure undergoes a reversible transition at 1.38–1.58 GPa from cubic α- to pseudo-tetragonal β-ZrV2O7 that displays an orthorhombic 2 × 3 × 3 supercell. At pressures above 4 GPa, ZrV2O7 becomes irreversibly X-ray amorphous. No such transformations are observed for TiP2O7 and ZrP2O7, which compress smoothly up to the highest investigated pressures (40.3 and 20.5 GPa, respectively). These differences in high-pressure properties are discussed in terms of the negative thermal expansion of ZrV2O7. The bulk moduli at ambient pressure (B0) for TiP2O7, ZrP2O7, α-ZrV2O7 and β-ZrV2O7 were estimated to be 42 (3), 39 (1), 17.0 (7) and 20.8 (10) GPa, respectively.
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| 5. |
- Krogh Andersen, A.M., et al.
(författare)
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High-Pressure Structures of α- and δ-ZrMo2O8
- 2001
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Ingår i: Acta Crystallographica Section B Structural science. - : Wiley. - 0108-7681. ; 57:1, s. 20-26
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Tidskriftsartikel (refereegranskat)abstract
- In situ high-pressure synchrotron X-ray powder diffraction studies of trigonal α-ZrMo2O8, zirconium molybdate, have been performed from ambient conditions to 1.9 GPa, over the α–δ phase transition at 1.06–1.11 GPa. The monoclinic structure of δ-ZrMo2O8, stable between 1.1 and 2.5 GPa at 298 K, has been solved by direct methods and refined using the Rietveld method. Significant distortions of the ZrO6 and MoO4 polyhedral elements are observed for δ-ZrMo2O8, as compared to the ambient conditions of the α-phase, while the packing of anions becomes more symmetric at high pressure.
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| 6. |
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| 7. |
- Krogh Andersen, A.M., et al.
(författare)
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Preparation and Characterization of a New 3-Dimensional Zirconium Hydrogen Phosphate, τ-Zr(HPO4)2; Determination of the Complete Crystal Structure Combining Synchrotron X-ray Single Crystal Diffraction and Neutron Powder Diffraction.
- 1998
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Ingår i: Inorganic chemistry. - : American Chemical Society. - 1520-510X .- 0020-1669. ; 37:5, s. 876-881
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Tidskriftsartikel (refereegranskat)abstract
- A new 3-dimensional zirconium hydrogen phosphate, τ-Zr(HPO4)2, was prepared by hydrothermal syntheses. The preparation, characterization, and determination of the crystal structure of this new material are reported. The structure was solved from single-crystal synchrotron diffraction on a 25 × 25 × 50 μm crystal. The position of the hydrogen atom was found using high-resolution neutron powder diffraction data. The unit cell is tetragonal, space group I41cd (No. 110), with lattice parameters a = 11.259(1) Å, c = 10.764(1) Å, and Z = 8. The structure can be described as a 3-dimensional framework built from ZrO6 octahedra bound together by hydrogen phosphate groups (PO3(OH)). The OH groups form a hydrogen-bonded spiral along the 41 axes, with each hydrogen phosphate both donating and accepting hydrogen bonds. The thermal transformations of τ-Zr(HPO4)2 were studied using in-situ temperature-resolved powder diffraction experiments. Hereby the existence of two new phases was discovered. The new phases have been indexed and the unit cell parameters are as follows. Intermediate I: a = 8.172(1), b = 7.691(1), and c = 10.794(2) Å. Intermediate II: a = 8.283(2), b = 6.620(2), and c = 10.643(2) Å.
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| 8. |
- Krogh Andersen, A.M., et al.
(författare)
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Structural Aspects of the Dehydration and Dehydroxylation of Layered γ-Titanium Phosphate, γ-Ti(PO4)(H2PO4)⋅2H2O.
- 1998
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Ingår i: Inorganic chemistry. - : American Chemical Society. - 1520-510X .- 0020-1669. ; 37:17, s. 4313-4320
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Tidskriftsartikel (refereegranskat)abstract
- The thermal transformations of γ-titanium phosphate, γ-Ti(PO4)(H2PO4)·2H2O, have been studied using thermogravimetric analysis, differential scanning calorimetry, X-ray powder diffraction, and temperature-resolved in-situ powder diffraction. The transformation sequence goes from γ-Ti(PO4)(H2PO4)·2H2O over a new partially dehydrated form γ‘-Ti(PO4)(H2PO4)·(2−x)H2O (x 1) to the anhydrous form β-Ti(PO4)(H2PO4) and then through a two-step condensation process where layered titanium pyrophosphate, Ti(PO4)(H2P2O7)0.5, is formed first and finally cubic titanium pyrophosphate TiP2O7. The dehydration of γ-Ti(PO4)(H2PO4)·2H2O and the dehydroxylation/condensation process from β-Ti(PO4)(H2PO4) to layered titanium pyrophosphate,Ti(PO4)(H2P2O7)0.5, was followed in-situ. A new partially dehydrated phase, γ‘-Ti(PO4)(H2PO4)·(2−x)H2O (x 1), which forms at approximately 50 °C has been detected and characterized. The unit cell is monoclinic with the lattice parameters a = 23.670(1) Å, b = 6.264(1) Å, c = 5.036(1) Å, β = 102.41(1)°, and Z = 4. Layered titanium pyrophosphate, Ti(PO4)(H2P2O7)0.5, which forms at 375 °C has been characterized. The unit cell is monoclinic with lattice parameters a = 16.271(3) Å, b = 6.319(1) Å, c = 5.122(1) Å, β = 90.59(2)°, and Z = 4.
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| 9. |
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| 10. |
- Muthu, D. V S, et al.
(författare)
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Pressure-induced phase transitions in α-ZrMo2O8
- 2002
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Ingår i: Physical Review B (Condensed Matter). - 0163-1829. ; 65:6, s. 641011-641015
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Tidskriftsartikel (refereegranskat)abstract
- We report high-pressure Raman, infrared (IR), and optical-absorption spectra of α-ZrMo2O8 (trigonal) up to 38 GPa at room temperature. The spectroscopic studies are consistent with diffraction results that show that α-ZrMo2O8 transforms into δ-ZrMo2O8 (monoclinic) at about 1 GPa and the δ phase converts to the ε phase (triclinic) at about 2.0 GPa. Optical-absorption measurements give an estimate of the band gap of about 0.6 eV at the lowest pressure. Band-gap changes with pressure are confirmed with visual observations. ZrMo2O8 changes from transparent at 5 GPa to yellow at 10 GPa, red at 18 GPa, and at about 30 GPa it becomes opaque.
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