Metastable Intermediate Phase during Phase Transformation of Calcium Phosphates

Author(s):  
Kazuo Onuma ◽  
Yuki Sugiura
2018 ◽  
Vol 283 ◽  
pp. 23-36 ◽  
Author(s):  
Yothin Chimupala ◽  
Rik Drummond-Brydson

Titanium dioxide (B phase) with 1-D structures was successfully fabricated via a hydrothermal method with a subsequent ion-exchange process and calcination. P25, titanium isopropoxide (TTIP), rutile and also anatase were used as Ti precursors in the alkali hydrothermal system. TTIP promoted an elongation of nanorod morphology whereas the other precursors produced short nanorod structures. The different types of titanium precursors did not have any influence on the phase transformation during the fabrication process. Na2Ti6O13 was the primary intermediate product after washing the hydrothermal sample. H2Ti3O7 was the secondary intermediate phase obtained following proton-exchange of Na2Ti6O13 in HNO3 solution. Finally, the TiO2(B) phase was the product of calcination of the secondary intermediate product at 400°C for 5 hr. A phase transformation mechanism is presented based on an investigation of products at each of the steps. The effects of the synthesis conditions on tailoring of the crystal morphology are discussed. The growth direction of the TiO2(B) nanorods was investigated by HR-TEM and SADP. Finally, the metastable phase of TiO2(B) was shown to be transformed to anatase during thermal treatment at temperatures higher than 400°C.


2010 ◽  
Vol 1256 ◽  
Author(s):  
Sujata Mazumder ◽  
Jiten Ghosh

AbstractThe detailed structure of nanocrystalline BaTiO3 powder during ball milling has been studied using XRD & TEM. The study illustrates important advances in understanding atomic scale properties of this material. Ferroelectric BaTiO3 powder undergoes phase transformation along the sequence Cubic(Pm3m)-tetragonal(P4mm)-orthohombic (Amm2)-rhombohedral(R3m) structure when pressureless sintered samples are cooled from high temperature to low temperature. The high to low symmetry phases are not related to group subgroup symmetry as transformation is discontinuous and first order in nature and the twin relationship in the low symmetry is forbidden by Landau theory. In case of ball milled BaTiO3 powder a continuous and diffusionless phase transition occur via second order to and from a metastable intermediate phase. In this pathway crystallites in the aggregation are twinned and the twin structure is related to crystal point group m3m which in the present case is illustrated as having 6mm symmetry formed under low driving force. The unit cell evolution due to phase transition and the crystallographic relationship are established. The phase transformation, coalescence and twin structure of thermally annealed BaTiO3 nanocrystals under high vacuum has been investigated using in situ high temperature XRD. The structure analysis is performed with the use of the method of computer modelling of disorder structure and simulation of corresponding diffraction pattern.


2013 ◽  
Vol 365-366 ◽  
pp. 1095-1099
Author(s):  
Tao Jiang ◽  
Lu Zhang ◽  
Yi Tang ◽  
Yi Xia ◽  
Xiang Xin Xue

This paper focuses on the influence of temperature and holding time on synthesizing MgAlON-SiAlON powders applying CRN method. The results were analyzed by chemical and XRD analysis technology. The experimental results revealed that β-SiAlON, as an intermediate phase, appeared in the synthesized products at 1200°C. With the increase of synthesis temperature, β-SiAlON was translated into Mg-SiAlON polytypoid (Mg1.25Si1.25Al2.5O3N3) and reached the maximum at 1450°C. Increasing synthesis temperature was beneficial to generate MgAlON, and the optimal condition of temperature for powders synthesis was 1500°C. β-SiAlON disappeared with the increase of holding time. MgAlON and Mg-SiAlON polytypoid became the main crystalline phases with a holding time of 4h. Whats more, the phase compositions had no evident change with longer holding time. Flaky MgAlON grains and elongated Mg-SiAlON grains were observed in synthesized powders.


2011 ◽  
Vol 89 (7) ◽  
pp. 885-891 ◽  
Author(s):  
Tim W. T. Tsai ◽  
Wei-Ya Chen ◽  
Yao-Hung Tseng ◽  
Jerry C. C. Chan

This work describes a phase-transformation pathway of calcium phosphate in the presence of glutamic acid. The route follows the order starting from amorphous calcium phosphate and brushite, then octacalcium phosphate (OCP), and finally hydroxyapatite (HAp). The preferred growth direction of the intermediate OCP and the final HAp phases lies along the c axis. On the basis of our scanning electron microscopy, X-ray powder diffraction, and 31P solid-state NMR data, we suggest that the transformation is via the dissolution–reprecipitation process, which is facilitated in the presence of glutamic acid. The effect on the transformation kinetics is rationalized by the disruption of the water layer bound on the crystal surface.


1976 ◽  
Vol 61 (0) ◽  
pp. 184-193 ◽  
Author(s):  
Helga Füredi-Milhofer ◽  
Ljerka Brečević ◽  
Branislav Purgarić

2014 ◽  
Vol 631 ◽  
pp. 99-103 ◽  
Author(s):  
Agnese Brangule ◽  
Kārlis Gross

Amorphous calcium phosphate (ACP) plays an important role in the body and can be used as an intermediate phase for forming calcium phosphates. All ACPs are thermodynamically unstable compounds, unless stored in dry conditions or at low temperature (-18oC), and spontaneously undergo transformation to crystalline calcium phosphates (CaP). This work will investigate the influence of drying on the stability of ACP. ACPs powders were prepared by wet synthesis; mixing solution made of Ca (NO3)2∙4H2O and 30% ammonia with (NH4)2HPO4 and (NH4)2CO3 solution at room temperature. The suspension was stirred, filtered and washed several times with deionized water containing ammonia. ACP samples were dried at different conditions and with different drying agents (DA). XRD and FTIR spectra showed poorly crystallinity powders after drying. Some FTIR spectra indicated residual organic compounds from drying. The Rietveld’s method and Schrrer’s relationship estimated the particle size (0.5 – 20 nm) of ACP. Thermogravimetry (TG) revealed that the moisture (7% – 25%) is released upon drying, and the drying agents have no significant effect on. The drying methods are ordered to show which the most effective for removing moisture. By changing the drying conditions, it is a possible to obtain poorly crystalline ACPs with different particle size and moisture content.


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