scholarly journals Effects of Synthesis Conditions on the Formation of Si-Substituted Alpha Tricalcium Phosphates

2020 ◽  
Vol 21 (23) ◽  
pp. 9164
Author(s):  
Katarzyna Szurkowska ◽  
Łukasz Szeleszczuk ◽  
Joanna Kolmas

Powders of α-TCP containing various amounts of silicon were synthesized by two different methods: Wet chemical precipitation and solid-state synthesis. The obtained powders were then physico–chemically studied using different methods: Scanning and transmission electron microscopy (TEM and SEM), energy-dispersive X-ray spectroscopy (EDS), powder X-ray diffractometry (PXRD), infrared and Raman spectroscopies (FT-IR and R), and solid-state nuclear magnetic resonance (ssNMR). The study showed that the method of synthesis affects the morphology of the obtained particles, the homogeneity of crystalline phase and the efficiency of Si substitution. Solid-state synthesis leads to particles with a low tendency to agglomerate compared to the precipitation method. However, the powders obtained by the solid-state method are less homogeneous and contain a significant amount of other crystalline phase, silicocarnotite (up to 7.33%). Moreover, the microcrystals from this method are more disordered. This might be caused by more efficient substitution of silicate ions: The silicon content of the samples obtained by the solid-state method is almost equal to the nominal values.

Materials ◽  
2019 ◽  
Vol 12 (16) ◽  
pp. 2566 ◽  
Author(s):  
Katarzyna Szurkowska ◽  
Agata Drobniewska ◽  
Joanna Kolmas

Silicated hydroxyapatite powders enriched with small amounts of manganese (Mn2+) cations were synthesized via two different methods: precipitation in aqueous solution and the solid-state method. The source of Mn2+ ions was manganese acetate, while silicon was incorporated using two different reagents: silicon acetate and sodium metasilicate. Powder X-ray diffraction (PXRD) analysis showed that the powders obtained via the precipitation method consisted of single-phase nanocrystalline hydroxyapatite. In contrast, samples obtained via the solid-state method were heterogenous and contaminated with other phases, (i.e., calcium oxide, calcium hydroxide, and silicocarnotite) arising during thermal treatment. The transmission electron microscope (TEM) images showed powders obtained via the precipitation method were nanosized and elongated, while solid-state synthesis produced spherical microcrystals. The phase identification was complemented by Fourier transform infrared spectroscopy (FTIR). An in-depth analysis via solid-state nuclear magnetic resonance (ssNMR) was carried out, using phosphorus 31P single-pulse Bloch decay (BD) (31P BD) and cross-polarization (CP) experiments from protons to silicon-29 nuclei (1H → 29Si CP). The elemental measurements carried out using wavelength-dispersive X-ray fluorescence (WD-XRF) showed that the efficiency of introducing manganese and silicon ions was between 45% and 95%, depending on the synthesis method and the reagents. Preliminary biological tests on the bacteria Allivibrio fisheri (Microtox®) and the protozoan Spirostomum ambiguum (Spirotox) showed no toxic effect in any of the samples. The obtained materials may find potential application in regenerative medicine, bone implantology, and orthopedics as bone substitutes or implant coatings.


2016 ◽  
Vol 703 ◽  
pp. 316-320
Author(s):  
Hai Feng Chen ◽  
Jing Ling Hu ◽  
Bing Xu

Using NH4VO3, Bi (NO3)3•5H2O and Co (NO3)2•6H2O as raw materials, Co doped BiVO4 (Co/BiVO4) photocatalysts were successfully prepared by solid state method. And the photo catalytic properties were test in this work. Crystal structures of these samples were characterized by X-ray diffraction (XRD). The Methyl Orange (MO) was simulated as the sewage under the visible light to explorer the influence of the illumination time and the mass of photocatalyst. The visible-light absorption spectrum of BiVO4 was broadening with doping Co. It was found that the Co/BiVO4 had higher photocatalytic activity than pure BiVO4 .The reason of enhanced catalytic effect also had been analyzed and discussed in the article.


2011 ◽  
Vol 306-307 ◽  
pp. 410-415
Author(s):  
Li Sun ◽  
Fu Tian Liu ◽  
Qi Hui Jiang ◽  
Xiu Xiu Chen ◽  
Ping Yang

Core/shell type nanoparticles with an average diameter of 20nm were synthesized by chemical precipitation method. Firstly, Monodisperse Fe3O4 nanoparticles were synthesized by solvethermal method. FeSO4ž7H2O and NaBH4 were respectively dissolved in distilled water, then moderated Fe3O4 particles and surfactant(PVP) were ultrasonic dispersed into the FeSO4ž7H2O solution. The resulting solution was stirred 2 h at room temperature. Fe could be deposited on the surface of monodispersed Fe3O4 nanoparticles to form core-shell particles. The particles were characterized by using various experimental techniques, such as transmission electron microscopy (TEM), X-ray diffraction (XRD), AGM and DTA. The results suggest that the saturation magnetization of the nanocomposites is 100 emu/g. The composition of the samples show monodisperse and the sides of the core/shell nanoparticles are 20-30nm. It is noted that the formation of Fe3O4/Fe nanocomposites magnetite nanoparticles possess superparamagnetic property.


2011 ◽  
Vol 412 ◽  
pp. 61-64
Author(s):  
Xiao Bo Wu ◽  
Da Zhi Sun ◽  
Dan Yu Jiang ◽  
Hai Fang Xu ◽  
De Xin Huang ◽  
...  

3Y-TZP powder has been successfully synthesized by gel solid-state method. The structural phases of powder particles were analyzed by X-ray diffraction and the morphology was analyzed by scanning electron microscopy. The average size of grains was 230 nm. The sintering behavior, mechanical properties and microstructure of 3Y-TZP ceramics sintered by this powder were investigated. The experiment results showed that the mechanical properties of ceramics were excellent.


2021 ◽  
Vol 854 ◽  
pp. 157204
Author(s):  
Yongxiang Chen ◽  
Shuliang Luo ◽  
Jin Leng ◽  
Shiyi Deng ◽  
Sheng Yan ◽  
...  

2014 ◽  
Vol 2014 ◽  
pp. 1-9
Author(s):  
Hamadi Hamza ◽  
Mohamed Faouzi Zid ◽  
Ahmed Driss

LiNa5K3Mo11As3O45 is a new inorganic compound. It was synthesized by a solid state method. The crystal structure has been studied by single crystal X-ray analysis. The R-values reached 2.8%. The title compound crystallizes in the triclinic system, space group P-1, with a = 10.550 (2) Å, b = 11.723 (2) Å, c = 17.469 (3) Å, α = 102.35 (3)°, β = 87.61 (2)°, and γ = 111.03 (3)°. The anionic unit [Mo11As3O45]9− is formed by nine MoO6 octahedra, two MoO5 trigonal bipyramids, and three AsO4 tetrahedra. The association of [Mo11As3O45]9− units, running along [010], leads to a one-dimensional framework. Li, K, and Na are located in the space surrounding the anionic ribbons. This material was characterized by SEM microscopy, IR spectroscopy, and powder X-ray diffraction. The electrical conductivity was investigated from 528 K to 673 K by impedance complex followed by DSC spectroscopy.


2018 ◽  
Vol 281 ◽  
pp. 716-722
Author(s):  
Xiao Xuan Wang ◽  
Shu Zhen Wang ◽  
Shu Wang Duo ◽  
Xing Yu Jiang ◽  
Wen Li Li ◽  
...  

ZnS:F quantum dots (QDs) capping with and without L-cys were synthesized by a solid-state method at low temperature, and the influence of L-cys on the properties of ZnS:F QDs were investigated. The crystal structure, surface morphology and luminescent properties of the samples were analyzed by X-ray diffractometer (XRD), transmission electron microscope (TEM), fourier transform infrared (FTIR), photoluminescence spectrometer (PL) and ultraviolet-visible spectrometer (UV-Vis). The results showed that all samples had a zinc blende structure with particle size in the range of 2-6 nm. The emission intensity was significantly enhanced after capping with L-cys, and the strongest luminescence was obtained when the ratio of L-cys/ZnS:F was 0.8:1, and was about 2.5 times of that of ZnS:F QDs. The capping of L-cys increased the grain size of ZnS:F QDs and their water solubility.


2012 ◽  
Vol 19 (03) ◽  
pp. 1250024 ◽  
Author(s):  
H. T. WU ◽  
C. H. YANG ◽  
W. B. WU ◽  
Y. L. YUE

Nanosized and highly reactive Mg4Ta2O9 were successfully synthesized by aqueous sol–gel method compared with conventional solid-state method. Ta-Mg-citric acid solution was first formed and then evaporated resulting in a dry gel for calcination in the temperature ranging from 600°C to 800°C for crystallization in oxygen atmosphere. The crystallization process from the gel to crystalline Mg4Ta2O9 was identified by thermal analysis and phase evolution of powders was studied using X-ray diffraction (XRD) technique during calcinations. Particle size and morphology were examined by transmission electron microscopy (TEM) and high resolution scanning electron microscopy (HR-SEM). The results revealed that sol–gel process showed great advantages over conventional solid-state method and Mg4Ta2O9 nanopowders with the size of 20–30 nm were obtained at 800°C.


Materials ◽  
2022 ◽  
Vol 15 (2) ◽  
pp. 569
Author(s):  
Oleg E. Polozhentsev ◽  
Ilia A. Pankin ◽  
Darya V. Khodakova ◽  
Pavel V. Medvedev ◽  
Anna S. Goncharova ◽  
...  

Herein we report the development of a nanocomposite for X-ray-induced photodynamic therapy (X-PDT) and computed tomography (CT) based on PEG-capped GdF3:Tb3+ scintillating nanoparticles conjugated with Rose Bengal photosensitizer via electrostatic interactions. Scintillating GdF3:Tb3+ nanoparticles were synthesized by a facile and cost-effective wet chemical precipitation method. All synthesized nanoparticles had an elongated “spindle-like” clustered morphology with an orthorhombic structure. The structure, particle size, and morphology were determined by transmission electron microscopy (TEM), X-ray diffraction (XRD), and dynamic light scattering (DLS) analysis. The presence of a polyethylene glycol (PEG) coating and Rose Bengal conjugates was proved by Fourier-transform infrared spectroscopy (FTIR), thermogravimetric analysis (TG), and ultraviolet–visible (UV-vis) analysis. Upon X-ray irradiation of the colloidal PEG-capped GdF3:Tb3+–Rose Bengal nanocomposite solution, an efficient fluorescent resonant energy transfer between scintillating nanoparticles and Rose Bengal was detected. The biodistribution of the synthesized nanoparticles in mice after intravenous administration was studied by in vivo CT imaging.


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