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1.
《Ceramics International》2023,49(6):9219-9230
The use of liquid phase additives is a strategy to improve the physicochemical, mechanical, and biological properties of calcium phosphate cements. In this study, TTCP and α-TCP particles were synthesized using the solid-state reaction method. Apatite cements were prepared by mixing TTCP/DCPD/α-TCP powders and liquid phases containing chondroitin sulfate with various additives of carboxylic acids and phosphate salts. The formation of hydroxyapatite and consumption of raw materials as well as the acceleration and deceleration periods through cementation process were investigated by XRD and DSC experiments, respectively. In addition, the morphology, setting time, porosity, compressive strength, degradation, in-vitro bioactivity and cytotoxicity were studied. The results showed that the approximate amount of hydroxyapatite resulting from the cementation process was divergent in the presence of liquid phase additives. The use of phosphate salt additives presented better results compared to carboxylic acid ones regarding hydroxyapatite cement product formation, compressive strength, hardening, setting, and cytotoxicity. All cements showed, generally a similar tendency to form dense hydroxyapatite on their outer surfaces through immersion in the simulated body fluid. The cement containing Na2HPO4 salt exhibited the lowest cytotoxicity and highest strength. The ALP assay and the morphological behavior of MG63 cells indicated the good activity and proper cell adhesion of this cement.  相似文献   

2.
Recently, premixed calcium phosphate cement pastes have been proposed as biomaterials for bone tissue repair and regeneration. Use of premixed pastes saves the time and removes an extra step during a medical operation. α-Tricalcium phosphate (α-TCP) based cements set to form calcium deficient hydroxyapatite which has a moderate bioresorbtion speed. α-TCP cements require a setting aid, usually a sodium or potassium phosphate salt, to speed up the setting process. Within the current research we investigated which setting aid has significant advantage, if α-TCP is used in form of non-aqueous premixed paste. This approach offers the application of simple ingredients to produce a premixed calcium phosphate cement. The following properties of cement formulations were evaluated: cohesion, phase composition, microstructure, pH value of the liquid surrounding the cement, and compressive strength.Compositions using mixture of basic and acidic potassium phosphate salts (KH2PO4 and K2HPO4) in sufficient amounts give the best overall results (adequate cohesion and pH of the surrounding liquid, hydrolysis of starting materials within 48 h, and compressive strength of 12 ± 3 MPa). Cement prepared with basic sodium phosphate salt (Na2HPO4) as setting aid had considerably higher compressive strength 22 ± 1 MPa, but the pH of the surrounding liquid was basic (9.0).  相似文献   

3.
Tetracalcium phosphate/monetite biocement was modified with the addition of 30 wt% highly porous silicon nitride/α-tricalcium phosphate (α-TCP) microgranules. The volume ratio of Si3N4 and α-TCP in microgranules was 1:1 and showed good in vitro simulated body fluid bioactivity with precipitation of hydroxyapatite particles. The intention of addition of microgranules to the biocement was to have a carrier of drug, which can be released into the body in due time. Granules prepared by the freeze granulation of starting mixture of silicon nitride and calcium phosphate and subsequent sintering at 1100°C have a suitable pore structure for the foreseen use. The pore volume was almost 1000 mm3/g with the open porosity of 77 vol%. This porosity and the biocompatible composition of silicon nitride–based granules gave a chance to fabricate a suitable composite cement for dexamethasone (DMZ) drug release into the human body. An accelerated release of dexamethasone from composite cement was observed and the full amount of DMZ was released from the composite biocement after 10 days. The presented results are a good base to adjust the total drug release time by the mixing of an appropriate amount of drug infiltrated ceramic granules with the tetracalcium phosphate/monetite cement.  相似文献   

4.
《Ceramics International》2022,48(11):15390-15404
The standard preparation routine of a calcium phosphate cement includes mixing a solid and a liquid component (reactive cement powder and mixing liquid) in an open bowl at the operating theatre. This poses the risk of preparation-related deviations of the resulting properties when the cements are mixed by different persons. Hence, facilitating this mixing procedure is highly desirable. It can be achieved by application of premixed cement pastes: The mixing liquid and a stable suspension of the cement powder are assembled and mixed in a special syringe, minimizing the impact of these preparation-related effects.In this study, a suspension of reactive α-tricalcium phosphate powder in water was stabilized by sodium pyrophosphate decahydrate (PP). Controlled activation of these premixed pastes was then accomplished by adding a concentrated Na2HPO4/NaH2PO4 (Na2/Na) solution. Systematic assessment of the activation mechanism, including the effect of the PP concentration and the amount of Na2/Na added, was performed by isothermal calorimetry, quantitative in-situ X-ray diffraction, rheological characterization and automated Gillmore needle measurements at 37 °C.Premixed pastes with addition of at least 0.05 wt% PP were successfully stabilized for up to 2 weeks at 25 °C, and even 4 weeks at 4 °C. This pre-storage had no significant impact on the setting performance of the pastes. Increasing the PP concentration at constant Na2/Na amount systematically retarded the setting reaction, while an elevated quantity of Na2/Na addition at constant PP concentration resulted in an acceleration.Based on these results, a composition stabilized with 0.05 wt% PP and activated with 20.8 vol% Na2/Na related to the amount of liquid in the premixed pastes appears ideal with respect to the desired setting performance.  相似文献   

5.
Calcium phosphate powders, β-TCP and biphasic HA/β-TCP, were synthesized by calcining the powders obtained from the co-precipitation method using Ca(NO3)2·4H2O and (NH4)2HPO4. The effects of the initial Ca/P ratio and pH of the solution on the phase evolution and in vitro dissolution behavior of the powders in a Ringer's solution were investigated. The Ca/P ratio of the resulting powders was strongly dependent on the pH of the solution and weakly dependent on the initial Ca/P ratio. Single phase TCP powder was obtained at pH=7.4 and the initial Ca/P ratio had a little effect on the resulting Ca/P ratio. Biphasic composite powders were prepared at pH=8.0 and the Ca/P ratio of resulting powder was controllable by adjusting the initial Ca/P ratio. TCP powder showed the highest dissolution rate in the Ringer's solution and biphasic composite powder exhibited an intermediate dissolution behavior between that of HA and TCP.  相似文献   

6.
In this research, biphasic β-tricalcium phosphate/carbonate apatite (β-TCP/CO3Ap) scaffolds incorporated with alginate were fabricated. Sodium alginate was extracted from local brown seaweed, Sargassum polycystum via calcium alginate process. Biphasic β-TCP/CO3Ap scaffolds were fabricated by polymer reticulate method. β-TCP slurry was infiltrated into the polyurethane foam (PU) foam, then sintered up to 1300?°C, soaked for 4?h and immediately quenched in still air to form biphasic β-TCP/α-TCP scaffold. Biphasic β-TCP/α-TCP scaffold was then transformed to biphasic β-TCP/CO3Ap scaffold by dissolution-precipitation reaction with 1?M of NaHCO3 at 170?°C for 1, 3 and 5 days. Biphasic β-TCP/CO3Ap scaffold from 5 days dissolution-precipitation reaction was chosen to incorporate with 1%, 3% and 5% of sodium alginate, respectively, as it has the highest composition of CO3Ap phase. FTIR and FESEM analysis confirmed the presence of characteristic functional groups of sodium alginate. Mechanical strength of biphasic β-TCP/CO3Ap scaffold improved by increasing the concentration of sodium alginate. The highest mechanical strength achieved was 26.38 kPa for biphasic β-TCP/CO3Ap scaffold with 5% sodium alginate coating and it was chosen to further study with the addition of 1%, 3% and 5% microspheres. FESEM analysis confirmed the attachment of microspheres on the surface of alginate/biphasic β-TCP/CO3Ap scaffold was successful.  相似文献   

7.
The Pechini based liquid-mix technique has been applied to prepare either single phases of hydroxyapatite –Ca10(PO4)6OH2– (OHAp), α and β-tricalcium phosphate –Ca3(PO4)2–, (α-TCP, β-TCP) or biphasic calcium phosphates (BCP). Compositions with a Ca/P molar ratio between 1.5 and 1.667 were synthesized and subjected to a thermal treatment up to 1400 °C. α and β-TCP were both prepared from a Ca/P ratio of 1.5, but while β-TCP is isolated at 900 °C and remains stable up to 1100 °C, it is necessary to anneal at 1400 °C for 72 h to obtain pure α-TCP. OHAp is obtained as a single phase from a 1.667 Ca/P ratio after annealing at 1000 °C for 24 h and starts to decompose at 1400 °C. Between these two extremes a whole range of biphasic calcium phosphates can be prepared by using this technique with an accurate control of the starting reactants. These materials have been characterized by FTIR, XRF, BET, XRD and, based on this technique, a phase quantification determination (QXRD). The solubility of these products was tested in a buffered solution at 37 °C and pH=7.4.  相似文献   

8.
Calcium phosphate cements are used as synthetic bone grafts with several advantages such as biocompatibility, osteoconductivity, and moldability. In this study, the synthesis of a biocement starting from calcium hydroxide (Ca(OH)2) and Monocalcium Phosphate Monohydrate (MCPM) was investigated. A 6?wt% Na2HPO4 aqueous solution along with a modified polymeric resin (RIVA(SDI)®) were adopted as the variable liquid phase in self- and light-cure cement groups. XRD analysis and FTIR spectroscopy were used to study the phase composition. The composite microstructure was characterized by scanning electron microscopy (SEM) and the degradation rates were measured by atomic absorption spectroscopy (AAS) analysis. In addition, the effect of soaking time of the cement in simulated body fluid (SBF) on the final phase and morphology was studied. The results showed that soaking the composite in SBF has a significant influence in phase transformation into hydroxyapatite, but following a slower kinetic in light-cured composite cements. Evidences of crosslinking reactions in light-cured cements were observable, which at the same time can legitimize slower apatite formation and faster biodegradation of these composite cements.  相似文献   

9.
In the present study, a bioactive silicate-phosphate glass-ceramic scaffold was fabricated via the polymer-derived ceramics (PDC) method. K2HPO4 phosphate salt was used as the P2O5 precursor in this method. The effect of K2HPO4 wt% and heat treatment temperatures (900–1100 °C) was evaluated. It was observed that although increasing the wt% of K2HPO4 led to the formation of scaffolds with higher densities and strengths, it could also increase the formation of the calcium phase, which could result in improper release behavior of scaffolds. On the other hand, higher heat treatment temperatures enhanced the strength of the scaffolds but eliminated the bioactive octacalcium phosphate (OCP) phase. X-ray diffraction (XRD) analysis showed that the dissolution of the OCP phase in simulated body fluid (SBF) resulted in precipitation of hydroxyapatite (HA) on the scaffold surface which enhanced the bioactivity. Furthermore, based on microstructural studies by Scanning Electron Microscopy (SEM), the fabricated scaffold possessed a wide range of pore sizes, appropriate for osteointegration and bone formation. The optimum wt% of phosphate salt was less than 6 wt% and the optimum heat treatment temperature was 1000 °C. After the optimization of compositions and processing, Alamar Blue Assay was used to evaluate HOb cell cultures, showing a continuous proliferation for the optimized samples.  相似文献   

10.
《Ceramics International》2016,42(14):15376-15382
Porous β-tricalcium phosphate (β-TCP) was successfully prepared from starfish-derived calcium carbonate (sf-bone) under several hydrothermal conditions. The sf-bone, obtained from Patiria Pectinifera by bleaching to remove organic substances, was Mg-containing calcite granules with an interconnected microporous structure of approximately 10−50 µm of pore, and was hydrothermally treated with ammonium phosphate aqueous solutions at various pHs and temperatures. The sf-bone was converted to Mg-containing β-TCP with maintaining its microporous structure by the hydrothermal treatment for 1 day or longer in (NH4)2HPO4 aqueous solution at 200 °C. This conversion was based on dissolution-reprecipitation process of Mg-containing calcite in the phosphate salt aqueous solution. Thus, conditions during the conversion, pH and temperature, affected the morphologies and crystal phases of sf-bone after the treatment depended upon both calcite dissolution and calcium phosphate-formation rates.  相似文献   

11.
《应用陶瓷进展》2013,112(2):79-82
Abstract

In the present study, β tricalcium phosphate (β-TCP) was prepared by precipitation from aqueous solutions. Calcium nitrate tetrahydrate Ca(NO3)2.4H2O and diammonium hydrogen phosphate (NH4)2HPO4 salts with an initial Ca/P molar ratio of 1·5 were dissolved in distilled water and mixed at 20°C and pH 10. Phase evolution of the as received precipitate was studied by X-ray diffraction and infrared spectroscopy before and after calcination in a dry air atmosphere at temperatures in the range 200-1400°C for 1 h. Thermal behaviour was investigated by simultaneous thermal analysis (DTA-TG). Calcium and phosphorus contents of the as received precipitate were determined by the inductively coupled plasma technique, and a Ca/P molar ratio of 1·49 ± 0·01 was found. The densities of the as received precipitate and of powder calcined at 800°C were determined by picnometery to be 2·43 and 3·01 ± 0·05 g cm-3 respectively. The experimental data suggest the formation of an amorphous phase corresponding to a TCP-like composition, which is calcium deficient and contains a very small amount of HPO42- groups.  相似文献   

12.
This study evaluated the phase transformation of calcium phosphate cement (CPC) using a mixture of monocalcium phosphate monohydrate (MCPM) and CaCO3 as the solid phase and either water or a sodium phosphate buffer (SPB) solution (pH=7.0) as the liquid phase. The synthetic CPC was characterized by X-ray diffraction (XRD) analysis and transmission electron microscopy (TEM). The setting reaction in the SPB solution involved three phase transformations. Firstly, MCPM and CaCO3 reacted with sodium phosphate immediately to form dicalcium phosphate dehydrate (DCPD) which continued to dissolve. Secondly, meanwhile, an intermediate amorphous calcium phosphate (ACP) was formed. Finally, ACP transformed into calcium-deficient hydroxyapatite (CDHA). In contrast, the reaction stopped at the first stage in water. Consequently, the SPB solution not only caused the dissolution of DCPD but also provided the buffering capacity to induce the conversion of the starting materials to CDHA.  相似文献   

13.
Macromolecularly imprinted calcium phosphate/alginate hybrid polymer microspheres surface imprinted with bovine serum albumin were prepared in inverse‐phase suspension by introducing the intermixture solutions of bovine serum albumin (BSA) and CaCl2 in sodium alginate aqueous solution where (NH4)2HPO4 was added beforehand. Morphology of the imprinted microspheres was observed by optical microscopy. Rebinding dynamic and thermodynamic behaviors of surface molecularly imprinted calcium phosphate/alginate polymer microspheres (CP/A SMIPMs) and embedding molecularly imprinted calcium phosphate/alginate polymer microspheres (CP/A EMIPMs) were evaluated. CP/A SMIPMs exhibited significant improvement in equilibrium rebinding capacity (Qe) and imprinting efficiency (IE), compared to CP/A EMIPMs. The surface of CP/A SMIPMs was more competent to facilitate the migration and re‐assembling of proteins. Surface specific peak and interior specific peak were proposed to describe the characteristics of surface and interior specific rebinding behaviors in rebinding dynamics. The effects of (NH4)2HPO4 addition were investigated in detail, along with the concentration of sodium alginate and CaCl2 solutions to the rebinding and imprinting property of imprinted microspheres. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2008  相似文献   

14.
Nano-sized calcium hydroxyapatite, [Ca10(PO4)6(OH)2] has been synthesized by the sol–gel combustion method using calcium nitrate and di-ammonium hydrogen phosphate as precursors in the aqueous medium. Triethyl phosphite was used as a phosphate precursor for alcohol mediated combustion. The aqueous and alcohol media were employed for the investigation of combustion synthesis in the presence of various fuels such as urea, glycine, alanine, hydrazine and hexamine. The metal-to-fuel ratio in the synthesis was maintained at 1 to facilitate complete combustion and the Ca/P ratio was maintained at 1.67 to aid the stoichiometric formation of hydroxyapatite. The combustion products were calcined at 800 °C for 10 h and were characterized by powder XRD, FT-IR, HR-SEM and HR-TEM techniques. All the five fuels used under the alcohol mediated combustion, resulted in forming phase pure hydroxyapatite; whereas the aqueous mediated combustion method yielded biphasic calcium phosphate containing Ca10(PO4)6(OH)2 and β-TCP depending on the nature of the fuel.  相似文献   

15.
Effects of zirconium oxide (ZrO2) nanoparticles additive on the microstructure and physical properties of hydroxyapatite (HA) were investigated. The HA powder was derived from natural bovine bone by a sequence of thermal processes. The composites containing nanoparticles of ZrO2 (0.2–1.0 vol%) were fabricated by a solid-state reaction mixed oxide method. All samples showed traces of HA, beta-tricalcium phosphate (β-TCP) and alpha-tricalcium phosphate (α-TCP) phases while the x≥0.1 samples also showed ZrO2 phase. Amount of β-TCP and α-TCP phases tend to decrease with ZrO2. The additive inhibited grain growth as a result of a decrease in grain size. However, the x=0.2 sample exhibited higher hardness value which is consistent with the density data. In addition, bioactivity test suggested that the additive promoted an apatite forming with the values of Ca/P close to the value obtained from HA.  相似文献   

16.
Derived Hench’s bioglasses with specific ionic dopants Ag+, Cu2+, or Zn2+ have been prepared. The bone-boding ability or bioactivity behavior for the prepared glasses and their glass-ceramic derivatives has been investigated after immersion in phosphate solution for two weeks. Collective Fourier transform infrared absorption spectra (FTIR) and scanning electron microscopic (SEM) studies were conducted in order to study the in-vitro bioactivity behavior. X-ray diffraction (XRD) analysis was carried out to identify the crystallized phases upon thermal heat treatment through a two-step regime. The glasses and their glass-ceramic derivatives were tested to study their antibacterial or antifungal efficiency responding to the doped metal ions. FTIR spectra revealed the generation of two split peaks at about 560 and 605 cm?1, after immersion in (0.2 M) sodium phosphate solution (Na3PO4), signifying the formation of a crystalline calcium phosphate phase, leading to hydroxyapatite formation. SEM examinations show characteristic rounded or nodular microcrystals for hydroxyapatite which support the FTIR data. X-ray diffraction analysis indicated crystallization of the main soda-lime silicate phase (1Na2O.2CaO.3SiO2) besides a secondary silicon phosphate phase (SiO2.P2O5) in the studied glass ceramics. The route of crystallization is discussed on the basis of the presence of 6% P2O5; which facilitates the formation of phase separation and voluminous bulk crystallization of the main soda-lime silicate phase. The introduction of dopants is identified to cause no changes in the precipitated phases, with only minor changes in the percent of the crystalline phases. Experimental data indicate that the glass-ceramic samples are effective in bioactivity and antimicrobial efficiency.  相似文献   

17.
《Ceramics International》2016,42(9):10638-10644
In this study, ceramics containing mixed phases of hydroxyapatite/beta-tricalcium phosphate (HA/β-TCP) were fabricated by a solid-state reaction technique. The HA powder was synthesized from cockle shells while the β-TCP powder was synthesized from egg shells. Pure HA and β-TCP fine powders were successfully obtained. The HA and β-TCP were mixed and subjected to a thermal treatment up to 1100 °C. To form the mixed phase ceramics, the resulting powders were sintered at 1350 °C. Effects of HA concentration on the properties of the studied ceramic were investigated. X-ray diffraction analysis revealed that all samples presented multiphase of calcium phosphate compounds. Average grain size of the ceramics decreased with the HA additive content. The 75 wt% HA ceramic showed the maximum hardness value (5.5 GPa) which is high when compared with many calcium phosphate ceramics. In vitro bioactivity test indicated that apatite forming increased with the HA additive content. To increase antibacterial activity, selected ceramics were coated with AgNO3. Antibacterial test suggested that an Ag compound coating on the ceramics could improve the antibacterial ability of the studied ceramics. In addition, the antibacterial ability for the Ag coated ceramics depended on the porosity of the ceramics.  相似文献   

18.
Soda lime phosphate bioglass–ceramics with incorporation of small additions of TiO2 were prepared in the metaphosphate and pyrophosphate region, using an appropriate two-step heat treatment of controlled crystallization defined by differential thermal analysis results. Identification and quantification of crystalline phases precipitated from the soda lime phosphate glasses were performed using X-ray diffraction analysis. Calcium pyrophosphate (β-Ca2P2O7), sodium metaphosphate (NaPO3), calcium metaphosphate (β-Ca(PO3)2), sodium pyrophosphate (Na4P2O7), sodium calcium phosphate (Na4Ca(PO3)6) and sodium titanium phosphate (Na5Ti(PO4)3) phases were detected in the prepared glass–ceramics. The degradation of the prepared glass–ceramics was carried out for different periods of time in simulated body fluid at 37 °C using granules in the range 0.300–0.600 mm. The released ions were estimated by atomic absorption spectroscopy and the surface textures were measured by scanning electron microscopy. Investigation of in vitro bioactivity of the prepared glass–ceramics was done by the measurement of the infrared reflection spectra for the samples after immersion in the simulated body fluid for different periods at 37 °C. The result showed that no apatite layer was formed on the surface of the samples and the dominant phase remained on the surface was β-Ca2P2O7, which is known for its bioactivity.  相似文献   

19.
The influence of the slag powder's fineness, the amounts of activator, type and contents of modification addition on the dry-shrinkage and strength of the high-strength slag cement material was investigated. The experimental data showed that adding 9% Na2SiO3 activator and 10% Portland cement (PC) made the ratios of drying-shrinkage of high-strength slag cement material similar to the ratios of Portland cement and the compressive strengths as higher. The main hydration products are calcium alumina-silicate gels and a little CH; the gel ratio of CaO/SiO2 is close to 1 and includes a little Na2O and MgO for high-strength slag cement material, as shown by means of scanning electron microscope (SEM) and energy-dispersive X-ray analyzer (EDXA).  相似文献   

20.
Nano SiO2 and MgO particles were incorporated into β-tricalcium phosphate (β-TCP) scaffolds to improve the mechanical and biological properties. The porous cylindrical β-TCP scaffolds doped with 0.5 wt % SiO2, 1.0 wt % MgO, 0.5 wt % SiO2 + 1.0 wt % MgO were fabricated via selective laser sintering respectively and undoped β-TCP scaffold was also prepared as control. The phase composition and mechanical strength of the scaffolds were evaluated. X-ray diffraction analysis indicated that the phase transformation from β-TCP to α-TCP was inhibited after the addition of MgO. The compressive strength of scaffold was improved from 3.12 ± 0.36 MPa (β-TCP) to 5.74 ± 0.62 MPa (β-TCP/SiO2), 9.02 ± 0.55 MPa (β-TCP/MgO) and 10.43 ± 0.28 MPa (β-TCP/SiO2/MgO), respectively. The weight loss and apatite-forming ability of the scaffolds were evaluated by soaking them in simulated body fluid. The results demonstrated that both SiO2 and MgO dopings slowed down the degradation rate and improved the bioactivity of β-TCP scaffolds. In vitro cell culture studies indicated that SiO2 and MgO dopings facilitated cell attachment and proliferation. Combined addition of SiO2 and MgO were found optimal in enhancing both the mechanical and biological properties of β-TCP scaffold.  相似文献   

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