The calcium phosphate spherical material with a hierarchical structure has been used as a bone implantation material. To improve the properties of the implant material, the compositions of calcium phosphate, silicon, and titanium are crucial. The presence of silicon on the surface of the phosphate–calcium material accelerates the bonding of the implant with the bone (osseointegration). The aim of this work was to develop a sol–gel method to prepare spherical calcium-phosphate@TiO 2 –SiO 2 biomaterials for bone implantation. The CaO@TiO 2 –SiO 2 biomaterial with a core–shell structure was synthesized by the sol–gel method. The biological properties of the materials were studied with a simulated body fluid (SBF). The sample had a spherical shape. The sample exhibited bioactive properties because an increase in the content of calcium and phosphorus ions in the shell and the presence of precipitated ions from the solution were detected on the surface. The TiO 2 –SiO 2 framework was uniformly fixed on the CaO core. Heat treatment of the hybrid mesostructure led to the formation of mesoporous materials with a specific regular structure in the nanometer size in the shell, which is necessary for the fixation of biological cells when the sample is introduced into the biological medium. The formation of a calcium–phosphate layer on the materials and the release of soluble silicon and calcium ions into the SBF are the key factors for the rapid connection of these materials with tissue. The results demonstrate that the CaO@TiO 2 –SiO 2 biomaterial with a core–shell structure is a good candidate for bone implantation.
Abstract. Thin films were synthesized by sol-gel method from alcohol film forming solutions (FFS) based on tetraethoxysilane, phosphoric acid, calcium chloride. Concentration of tetrabutoxytitanium was 0.4 and 0.3 M. Thin films were produced on substrates of single crystal silicon (model substrate) by spin-coating with a centrifuge speed of 3000 rev/min, followed by heat treatment at 60 °С for 20 minutes and at 600 °С for 1 h. During the experiment it was found that film with uniform surface may be got on the fifth day after preparation of the solution with a concentration of Ti 4+ 0.3 M. For homogeneous material requires heat treatment at 800 °С. The highest bioactivity was observed in the films based on film-forming solution with a concentration of Ti 4+ 0.3 M.
A calcium–phosphate system was obtained by sol–gel method from 0.4 M solutions based on ethyl alcohol, tetraethoxysilane, phosphoric acid, calcium nitrate, and magnesium nitrate, sodium chloride. Compositions with different contents of CaO, Na 2 O, and MgO were prepared. After maturation of the solutions, heat treatments were applied at 60 °C for 30 min; and followed by 600 °C and 800 °C for 1 h. Solution with 20 wt% MgO was found suitable for film production. The physicochemical processes of the formation of materials were studied, including the main stages: removal of physically bound and chemically bound water, combustion of alcohol and the products of thermo-oxidative destruction of ethoxy groups, and crystallization processes. The phase composition and structure of the films obtained were established at 600 °C and above when crystalline forms of SiO 2 , CaSiO 3 , Ca 2 P 2 O 7 , and complex phosphates were fixed. In the system with the addition of magnesium ions, β-cristobalite SiO 2 and stenfieldt Mg 3 Ca 3 (PO 4 ) 4 were detected; however, a crystalline sample could only be obtained at 800 °C. In the system with sodium ions, chemical compounds Ca 5 (PO 4 ) 3 Cl, NaCl, and SiO 2 were determined. A uniform film coating was formed on the surface of the substrate. The introduction of sodium oxide into the SiO 2 –P 2 O 5 –CaO system increased the bioactivity of the materials obtained.
Синтез и свойства материалов на основе системы SiO2-P2O5-CaO-MgO Золь-гель методом получена кальций-фосфатная система из растворов на основе тетраэтоксисилана, фосфорной кислоты, нитратов кальция и магния. С помощью методов термического анализа и ИК-спектроскопии установлены стадии процесса формирования оксидных систем. Установлены оптимальные режимы термической обработки образцов. Методом рентгенофазового анализа изучено фазообразование в полученных образцах. Растровой электронной микроскопией исследована морфология поверхности образцов. Ключевые слова: золь-гель метод; кальций-фосфатные материалы; силикатная система; биоактивный материал; пленкообразующий раствор; дисперсные материалы.
The authors obtained spherical biomaterials of TiO2 – SiO2 – P2O5/MgO composition by sol-gel method. TOKEM-200, a weakly acid porous cation exchanger based on acryl-divinylbenzene was used as organic matrices. The cation exchangers were saturated with Mg2+ ions. Sol based on titanium butoxide, tetraethoxysilane and phosphoric acid was deposited on them. The temperature condition for producing spherical materials TiO2–SiO2– P2O5 / MgO were proposed. To obtain a spherical material, the treated cation exchangers were subjected to stepwise heat treatment in the temperature range from 60 to 600 °C. To study the biologically active properties of the material, the samples were immersed in simulation body fluid (SBF).
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