Hydrothermal synthesis of (Zr0.33 Ti0.67) O2–srilankite in the system ZrO2TiO2H2OMF; (M = Na, K)

Buhl, Josef‐Christian; Willgallis, A.

doi:10.1002/crat.2170240305

Cited by 12 publications

(3 citation statements)

References 4 publications

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“…For the Zr-O bond coming from ZrO 2 , the zirconium second nearest neighbour is another zirconium atom and we get a Zr-O-Zr like bonding. For the Zr-O bond which peak is located at 33.0eV, the second nearest neighbour is a titanium atom and we get a Zr-O-Ti bonding (11). The O-1s spectrum at θ = 0° is plotted on Figure 3b.…”

Section: Resultsmentioning

confidence: 94%

PEALD ZrO₂ Films Deposition on TiN and Si Substrates

et al. 2009

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The substrate influence on the structure of 60nm-thick ZrO2 films deposited by Plasma Enhanced Atomic Layer Deposition (PEALD) is reported. Films were grown either on TiN/Si(100) or on Si(100) substrates. TiN layers (45nm thick) were PVD-deposited. High Resolution Transmission Electron Microscopy (HRTEM) micrographs show that ZrO2 films display a microstructure made of columnar grains with a diameter of 15-20 nm and extended throughout the whole film thickness. An interfacial layer between ZrO2 films and TiN substrates was detected by Synchrotron Radiation X-Ray Photoelectron Spectroscopy and HRTEM. According to thermodynamics simulations, this interfacial layer should be a ternary Zr-Ti-O compound.

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Section: Resultsmentioning

confidence: 94%

PEALD ZrO₂ Films Deposition on TiN and Si Substrates

et al. 2009

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“…It is found in Sri Lanka, the Indian Ocean, and Arizona. Willgallis and coworkers [52][53][54][55] observed Zr atoms to be randomly substituted for Ti in the orthorhombic crystal structure. Aita and coworkers 56 reported observation of terminal phases corresponding to srilankite.…”

Section: Introductionmentioning

confidence: 99%

Synthesis and Characterization of Srilankite Nanowires

Germain¹,

Fraundorf²,

Lin³

et al. 2008

j nanosci nanotechnol

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We describe the synthesis and characterization of srilankite (Ti2ZrO6) nanowires. The nanowires are produced via hydrothermal synthesis with a TiO2/ZrO2 mixture under alkaline conditions. The zirconium titanate nanowires have median diameters of 60 nm and median lengths of 800 nm with the (022) axis along the length of the nanowire. Electron microscopy, energy dispersive X-ray spectroscopy, powder X-ray diffraction, and electron diffraction are used to characterize the phases and compare nanowires produced with varying molar ratios of Ti and Zr. Electron diffraction patterns produced from single nanowires show highly crystalline nanowires displaying a compositional-ordering superlattice structure with Zr concentrated in bands within the crystal structure. This is in contrast to naturally occurring bulk srilankite where Zr and Ti are randomly substituted within the crystal lattice. Streaking is observed in the electron diffraction patterns suggesting short-range ordering within the superlattice structure.

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“…For example, disordered (Zr,Ti) 2 O 4 with X Ti ϭ 0.67 crystallized by the sol-gel method at temperatures as low as 300°, far outside the stability field of the disordered phase. 6,20,21 The high state of disorder in the low-temperature sample was possibly inherited from the perfectly random starting powder, the energetics being too sluggish, or reaction rates too small to actually induce ordering of the atoms. 15 The scarcity and ambiguity of experimental equilibrium data for the ZrO 2 -TiO 2 system led to bold studies quantifying the thermodynamics at lower temperatures based on limited experimental evidence.…”

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confidence: 99%

Synthesis of Ordered Zirconium Titanate (Zr,Ti)₂O₄ from the Oxides Using Fluxes

Troitzsch

Christy

Ellis

2004

Journal of the American Ceramic Society

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The crystallization of ordered (Zr,Ti) 2 O 4 from the oxides succeeded for the first time, at 800°-1200°C and 13-20 kbar, using either ammonium carbonate or copper oxide as flux. The composition of the ordered phase, coexisting with either zirconia or rutile, is pressure-temperature dependent, ranging from X Ti ‫؍‬ 0.60 to 0.68. Its reproducibility and reversibility suggest the ordered compound crystallized at/near thermodynamic equilibrium. The presence of flux permits the equilibration of phase assemblages well below 1200°C, a region previously inaccessible for equilibrium experiments in the ZrO 2 -TiO 2 system due to sluggish kinetics. Thus we were able to determine the ZrO 2 -TiO 2 phase diagram at 20 kbar at temperatures as low as 800°C. In contrast, room-pressure experiments did not result in the spontaneous nucleation of ordered (Zr,Ti) 2 O 4 from the oxides, and seeds were required to initiate growth. The flux-aided synthesis of ordered (Zr,Ti) 2 O 4 from the oxides, at constant temperature and in its stability field, has the following advantages over previous crystallization attempts, which consisted of slow cooling of the disordered polymorph through the ordering transition. The ordered compound forms at equilibrium, therefore permitting phase equilibrium studies and thermodynamic interpretation. Large grain sizes facilitate quantitative analysis of the composition with electron microscopy. Microcracks and ZrO 2 exsolution, reported from samples cooled through the transition, can be avoided. The composition and the ordering state of the ordered compound can be controlled with pressure and temperature. Using the flux-based synthesis method, well-crystallized samples can now be obtained for future crystal structure refinements, calorimetric and dielectric measurements, or investigations into the phase transition. Synthesis of Ordered Zirconium Titanate 2060

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Hydrothermal synthesis of (Zr_0.33 Ti_0.67) O₂–srilankite in the system ZrO₂TiO₂H₂OMF; (M = Na, K)

Cited by 12 publications

References 4 publications

PEALD ZrO₂ Films Deposition on TiN and Si Substrates

PEALD ZrO₂ Films Deposition on TiN and Si Substrates

Synthesis and Characterization of Srilankite Nanowires

Synthesis of Ordered Zirconium Titanate (Zr,Ti)₂O₄ from the Oxides Using Fluxes

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Hydrothermal synthesis of (Zr0.33 Ti0.67) O2–srilankite in the system ZrO2TiO2H2OMF; (M = Na, K)

Cited by 12 publications

References 4 publications

PEALD ZrO2 Films Deposition on TiN and Si Substrates

PEALD ZrO2 Films Deposition on TiN and Si Substrates

Synthesis and Characterization of Srilankite Nanowires

Synthesis of Ordered Zirconium Titanate (Zr,Ti)2O4 from the Oxides Using Fluxes

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Hydrothermal synthesis of (Zr_0.33 Ti_0.67) O₂–srilankite in the system ZrO₂TiO₂H₂OMF; (M = Na, K)

PEALD ZrO₂ Films Deposition on TiN and Si Substrates

PEALD ZrO₂ Films Deposition on TiN and Si Substrates

Synthesis of Ordered Zirconium Titanate (Zr,Ti)₂O₄ from the Oxides Using Fluxes