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1
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Sol-gel bioactive glass-ceramics Part I: Calcium phosphate silicate/wollastonite glass-ceramics

100%
Radev L., Hristov V., Michailova I., Samuneva B.
Open Chemistry
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2009
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vol. 7
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issue 3
317-321
EN
In this work we present experimental results about synthesis, structure evolution and in vitro bioactivity of new calcium phosphate silicate/wollastonite (CPS/W) glass-ceramics. The samples obtained were synthesized via polystep sol-gel process with different Ca/P+Si molar ratio (R). The structure of the materials obtained was studied by XRD, FTIR spectroscopy and SEM. XRD showed the presence of Ca15(PO4)2(SiO4)6, β-CaSiO3 and α-CaSiO3 for the sample with R=1.89 after thermal treatment at 1200°C/2h. The XRD results are in good agreement with FTIR analysis. SEM denotes that apatite formation can be observed after soaking in simulated body fluid (SBF). [...]
2
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Organic/Inorganic bioactive materials Part II: in vitro bioactivity of Collagen-Calcium Phosphate Silicate/Wollastonite hybrids

100%
Radev L., Hristov V., Samuneva B., Ivanova D.
Open Chemistry
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2009
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vol. 7
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issue 4
711-720
EN
In the present study, novel hybrid materials of Collagen (C) and Calcium Phosphate Silicate/Wollastonite (CPS/W) were synthesized. The CPS/W ceramic was prepared via polystep sol-gel method. The dissolution test of CPS/W ceramic was filled with TRIS-HCl buffer. FTIR depicts that hydroxyl carbonate apatite (OHCO3HA) was observed after 3 days of immersion in TRIS-HCl buffer. Biohybrids of C-CPS/W were produced from diluted hydrochloric acid collagen type I and ceramic powder with different ratios of C and CPS/W equal to 25:75 and 75:25 wt.%. The synthesized hybrids were characterized by FTIR, XRD and SEM. FTIR depicts a “red shift” if amide I could be attributed to the fact that the collagen prefers to chelate Ca2+ from partial dissolution of CPS/W ceramic. The growth of B-type carbonate containing hydroxyapatite (B-CO3HA) on the C-CPS/W hybrids soaked in 1.5SBF was observed. The negatively charged carboxylate groups from the collagen may be responsible for hydroxyapatite (HA) deposition. This fact was confirmed by the “red shift” of carboxylate groups of collagen in FTIR spectra. The formation of HA was observed by FTIR, XRD and SEM.
3
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Organic / inorganic bioactive materials Part I: Synthesis, structure and in vitro assessment of collagen/silicocarnotite biocoatings

100%
Hristov V., Radev L., Samuneva B., Apostolov G.
Open Chemistry
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2009
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vol. 7
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issue 4
702-710
EN
The silicocarnotite, as an inorganic part of the coatings, has been synthesized using a polystep sol-gel method. The chemical composition of the prepared silicocarnotite sol is described as 58.12 CaO, 29.42 P2O5, 12.45 SiO2 (wt%), where Ca/P+Si = 1,67. The acid soluble type I collagen, as an organic part of the obtained coatings, was mixed with silicocarnotite powder in a weight ratio of 25:75 and 75:25 weight ratio without cross-linkage. The acidity of the obtained mixture was readjust with 25% NH4OH to pH = 9.0. The mixture was then dried at 37°C for 12 h. The growth of B-type carbonate containing hydroxyapatite (B-type CO3HA) in which CO3 2+→PO4 3− on the surface of collagen/silicocarnotite coatings soaked in 1.5 simulated body fluid (1.5 SBF) was observed. The nucleation of B-type CO3HA was estimated on the obtained coatings after 3 days immersion in 1.5 SBF. The negatively charged carboxylate groups from the collagen surface may be responsible for the HA deposition. This was confirmed by the “red shift” of carboxylate groups of collagen molecules in the FTIR spectra. After soaking in 1.5 SBF, the morphology of prepared coatings and HA formation was observed by SEM.
4
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Sol-gel bioactive glass-ceramics Part II: Glass-ceramics in the CaO-SiO2-P2O5-MgO system

100%
Radev L., Hristov V., Michailova I., Samuneva B.
Open Chemistry
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2009
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vol. 7
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issue 3
322-327
EN
Ceramics, with basic composition based on the CaO-SiO2-P2O5-MgO system with different Ca+ Mg/P+Si molar ratio (R), were prepared via polystep sol-gel technique. The structure of the obtained ceramic materials has been studied by XRD, FTIR spectroscopy, and SEM. X-ray diffraction showed the presence of akermanite and HA for the sample with R = 1.68 and Mg substituted β-TCP and silicocarnotite for the sample with R = 2.16, after thermal treatment at 1200°C/2 h. The obtained results are in good agreement with FTIR. In vitro test for bioactivity in static condition proved that the carbonate containing hydroxyapatite (CO3HA) can be formed on the surface of the synthesized samples. CO3HA consisted of both A- and B-type CO 32− ions. SEM micrographs depicted different forms of HA particles, precipitated on the surface after soaking in 1.5 simulated body fluid (SBF). [...]
5
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Silica hybrid nanocomposites

88%
Chernev G., Samuneva B., Djambaski P., Salvado I., Fernandes H.
Open Chemistry
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2006
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vol. 4
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issue 1
81-91
EN
In this work we present experimental results about the formation, properties and structure of sol - gel silica based biocomposite containing Calcium alginate as an organic compound. Two different types of silicon precursors have been used in the synthesis: tetramethylortosilicate (TMOS) and ethyltrimethoxysilane (ETMS). The samples have been prepared at room temperature. The hybrids have been synthesized by replacing different quantitis of the inorganic precursor with alginate. The structure of the obtained hybrid materials has been studied by XRD, IR Spectroscopy, EDS, BET and AFM. The results proved that all samples are amorphous possessing a surface area from 70 to 290 m2/g. It has also been established by FT IR spectra that the hybrids containing TMOS display Van der Walls and Hydrogen bonding or electrostatic interactions between the organic and inorganic components. Strong chemical bonds between the inorganic and organic components in the samples with ETMS are present. A self-organized nanostructure has been observed by AFM. In the obtained hybrids the nanobuilding blocks average in size at about 8–14 nm for the particles.
6
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Characterization of superparamagnetic MgxZn1−x Fe2O4 powders

76%
Kassabova-Zhetcheva V., Pavlova L., Samuneva B., Cherkezova-Zheleva Z., Mitov I., Mikhov M.
Open Chemistry
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2007
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vol. 5
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issue 1
107-117
EN
Structural and magnetic properties of Mgx Zn1−x Fe2O4 powders have been studied with respect to the application for thermal cancer therapy (magnetic hyperthermia). Mgx Zn1−x Fe2O4 (x=0.1–0.5) powders with particle sizes between 5 and 8 nm were produced by citrate method. The X-ray diffraction patterns of the samples correspond to a spinel phase. The lattice constant and the volume of the elementary cell increase when x changes from 0.1 to 0.5. The FTIR-spectra ascertain the spinel phase formation. The Mossbauer studies reveal the presence of extremely small particles, which undergo superparamagnetic relaxation at room temperature. The core-shell model has been applied to explain quadruple doublets. The quadruple splitting at “shells” is bigger than those at “cores” whereas the isomer shifts remain close. Magnetic studies confirm the presence of extremely small particles that behave as superparamagnetic ones. [...]
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