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PubMed1982

Crystallinity, solubility, and dissolution rate behavior of fluoridated CO3 apatites.

To study the effect of fluoride on the physicochemical properties of carbonate-containing apatites, two series of fluoridated CO3 apatites with various fluoride contents were synthesized at 80 degrees C and pH 7.4. The alpha-axis dimensions of these apatites decreased with the increase of both fluoride and carbonate contents. The crystallinity of the apatites showed similar patterns of variation with the degree of fluoridation irrespective of carbonate content. These patterns appear analogous to the complex pattern of the fluoridated hydroxyapatites previously reported. In contrast to this unexpected crystallinity phenomena, the apparent solubility of fluoridated CO3 apatites in acetate buffer solutions at pH 4.0 and 6.0 and 37 degrees C decreased monotonically with increasing degree of fluoridation and approached that of fluoridated hydroxyapatites at high fluoride content. Dissolution rate of fluoridated CO3 apatite pellets at pH 4.0 also showed a simple decrease with increasing degree of fluoridation and was extremely sensitive to acid at low fluoride content.

Apatites↗

PubMed1995

Apatite coated on organic polymers by biomimetic process: improvement in its adhesion to substrate by glow-discharge treatment.

A dense, uniform, and highly biologically active bone-like apatite layer can be formed in arbitrary thickness on any kind and shape of solid substrate surface by the following biomimetic method at ordinary temperature and pressure: First, a substrate is set in contact with particles of bioactive CaO-SiO2-based glass soaked in a simulated body fluid (SBF) with inorganic ion concentrations nearly equal to those of human blood plasma so that a number of apatite nuclei are formed on the substrate. Second, the substrate is soaked in another solution with ion concentrations 1.5 times those of SBF (1.5SBF) so that the apatite nuclei grow in situ. In the present study, organic polymer substrates were treated with glow-discharge in O2 gas atmosphere, then subjected to the above-mentioned biomimetic process. The induction periods for the apatite nucleation on all the examined organic polymers were reduced from 24 to 6 h, with glow-discharge treatment. The adhesive strengths of the formed apatite layer to the substrates increased from about 4 to 10 MPa for poly(ethylene terephthalate) and poly-ether sulfone, and from 1 approximately 2 to 6 approximately 7 MPa even for poly(methyl methacrylate), polyamide 6 and polyethylene. It is supposed that highly polar groups such as carbonyl, ester, hydroxyl, and carboxyl ones formed by glow-discharge treatment increased the affinity of a silicate ion with the substrates to decrease the induction period, and also increased the affinity of the apatite with the substrate to increase the adhesive strength.(ABSTRACT TRUNCATED AT 250 WORDS)

Adhesiveness↗

PubMed2003

Structural dependence of apatite formation on titania gels in a simulated body fluid.

The apatite-forming ability of titania gels with different structures has been investigated in a simulated body fluid with ion concentrations nearly equal to those of human blood plasma. Titania gels with an amorphous structure or with an anatase or rutile structure were prepared by the sol-gel process with a subsequent heat treatment at various temperatures. The titania gels with an amorphous structure did not induce apatite formation on their surfaces in the simulated body fluid, whereas gels with an anatase or rutile structure induced apatite formation on their surfaces. The deposition of apatite was more pronounced on the anatase gels than on the rutile gels. This indicates that a specific structure of titania is effective in inducing apatite formation in a body environment. Such a specific structure was assumed in this study to be the crystalline planar arrangement in the anatase structure, which facilitates epitaxy of the apatite crystal.

Apatites↗

PubMed2003

Effect of calcium salt content in the poly(epsilon-caprolactone)/silica nanocomposite on the nucleation and growth behavior of apatite layer.

The effect of calcium salt content in the poly(epsilon-caprolactone) (PCL)/silica nanocomposite on the nucleation and growth behavior of apatite layer in simulated body fluid (SBF) was investigated. The specimens were prepared with low (L) and high (H) concentrations of calcium nitrate tetrahydrate through a sol-gel method. After soaking in the SBF at 36.5 degrees C for 1 week, a densely packed apatite layer that had a smooth surface and a Ca/P ratio similar to bone was formed on specimens containing a low concentration of calcium salt while a loosely packed apatite layer with a rugged surface and a higher Ca/P ratio than that of bone occurred on specimens containing a high concentration of calcium salt. The results are explained in terms of the degree of supersaturation of apatite in the SBF, as determined by the concentrations of constituent ions of apatite and pH. The practical implication of the results is that a dense and bone-like apatite layer on the PCL/silica nanocomposite in vitro, and perhaps in vivo, can be achieved by adopting an appropriate calcium salt content.

Apatites↗

PubMed2005

Formation of apatite on poly(alpha-hydroxy acid) in an accelerated biomimetic process.

Bonelike apatite coating was formed on poly(L-lactic acid) films and poly(glycolic acid) scaffolds within 24 h through an accelerated biomimetic process. The ion concentrations in the simulated body fluid (SBF) were nearly 5 times of those in the human blood plasma. The apatite formed was characterized by using scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD), and Fourier transform infrared spectroscopy (FTIR). The apatite formed in 5SBFs was similar in morphology and composition to that formed in the classical biomimetic process using SBF or 1.5SBF and similar to that of natural bone. This indicated that the biomimetic apatite-coating process could be accelerated by using concentrated simulated body fluid at 37 degrees C. Besides saving time, the accelerated biomimetic process is particularly significant to biodegradable polymers. Some polymers that degrade too fast to be coated with apatite by a classical biomimetic process (e.g., PGA) could be coated with bonelike apatite in an accelerated biomimetic process.

Apatites↗

PubMed1982

Blood:bone disequilibrium. VI. Studies of the solubility characteristics of brushite: apatite mixtures and their stabilization by noncollagenous proteins of bone.

Recent evidence of the occurrence of brushite in newly formed bone mineral prompted a study of the solubility properties of brushite:apatite mixtures under physiological conditions and the influence on them of pH, lactate, pyruvate, and, particularly, noncollagenous bone proteins (NCBPs). Brushite alone was surprisingly stable in solution at pH 7.4, 37 degrees C. In the presence of increasing amounts of apatite, hydrolysis of brushite to an insoluble phase occurred. A decrease of 0.1 pH unit or the addition of 1.5 mM pyruvate or 10 mM lactate increased the ion activity product (Ca2+ x HPO4(2-) 3 or more times. However, within the loose envelope of bone such conditions so different from those in the circulation might be only local or temporary. NCBPs, on the other hand, stabilized brushite in solution alone as well as in the presence of apatite for days. They probably act by adsorbing strongly to the crystal surface and preventing nucleation by apatite. This brushite-apatite-bone protein system exhibits solubility characteristics that can resolve the old problems presented by the participation of the skeleton in extracellular calcium homeostasis on the one hand, and by the apparent insolubility of the apatite mineral of bone on the other.

Animals↗

PubMed1976

The interaction of supersaturated calcium phosphate solutions with apatitic substrates.

The in vitro formation of calcium phosphates from supersaturated solutions seeded with apatite was examined. Reaction kinetics were followed by monitoring solution Ca, Mg, and PO4. Seeds and reaction products were examined chemically and by X-ray diffraction and electron microscopy. Under conditions where amorphous calcium phosphate (ACP) normally precipitates spontaneously, apatite reduced the amount of free ACP formed with a considerable fraction of the Ca and PO4 initially removed from solution depositing directly onto the seeds. At sufficiently great seed concentrations all initial solution losses occurred by this latter route with no free ACP precipitating. These initial events were followed by seed-induced formation of new apatite crystals accompanied by further losses in solution Ca and PO4. Supersaturated solutions stable to spontaneous ACP formation underwent similar losses in solution Ca and PO4 when seeded with apatite. Initial decrease in these ions was instantaneous and proportional to the seed concentration. Subsequent ion removal exponentially decreased with time and correlated with the formation of new apatite crystals overlaying the original seeds. In seeding experiments using physiologically-balanced salt solutions, the initial deposit formed on the seed surface was a magnesium stabilized calcium carbonate phosphate phase. This stable surface phase did not prevent the secondary crystallization of apatite from occurring.

Apatites↗

PubMed1990

Orientation of apatite and organic matrix in Lingula unguis shell.

The orientation relationship between apatite and organic matrix in shell of Lingula unguis (inarticulate brachiopod) was studied. The organic layers, mineralized layers, and decalcified mineralized layers were examined layer by layer using microbeam X-ray diffraction technique. Both organic layer and decalcified mineralized layer showed the diffraction pattern of beta-chitin. The degree of orientation of apatite showed correlation to that of beta-chitin: Well oriented diffraction patterns of apatite crystal and organic matrix were observed in the central part. In this part, the fiber axis of beta-chitin was parallel to the c-axis of apatite. A close relationship of unit cell dimension between apatite and chitin was indicated. These strongly suggest that the fibrous structure of organic matrix assists the orientation of apatite crystals in Lingula unguis shell.

Animals↗

PubMed1991

Carbonate ions in apatites: infrared investigations in the upsilon 4 CO3 domain.

Fourier transform infrared (IR) spectroscopic investigations of precipitated carbonate apatites in the upsilon 4 CO3 domain reveal the existence of five bands at 757, 740, 718, 692, 670 cm-1 which can be assigned to several distinct environments of the carbonate ion in the apatite structure. In order to identify these environments precisely, fluoridated and pure type A carbonate apatites (i.e., with carbonate ions in monovalent anionic sites) were examined. The bands at 670 and 757 cm-1 were attributed to type A carbonate and their relative intensity was found to increase when the carbonate content of the apatite diminished or when samples were heated at 400 degrees C. Fluoridated apatites show only two bands, close to 718 and 692 cm-1, corresponding to type B carbonate ions (carbonate in trivalent anionic sites). The band at 740 cm-1 was revealed by heating the samples to 400 degrees C. This is due to OH ions' hydrogen bonded to fluoride and to carbonate ions in an undetermined apatite site. Despite the low intensity of IR bands, investigations in the upsilon 4 CO3 domain appear complementary to those in other carbonate vibrational domains and could be useful for a more precise identification of bone mineral.

Apatites↗

PubMed1998

EPR properties of synthetic apatites, deorganified dentine, and enamel.

Electron paramagnetic resonance spectroscopy (EPR) was used to study synthetic hydroxyapatite and approximately 1, 2, and 6% synthetic carbonated apatites, deorganified dentine, and enamel. The carbonated apatites were synthesized by hydrolysis of dicalcium phosphate. Comparisons were made with spectra from enamel and deorganified dentine. Microwave power saturation and dose responses were determined for the synthetic materials. The Marquardt version of the Levenberg decomposition method was used to extract individual signals from the apatite data. Two samples of dentine were irradiated with 25 and 100 Gy, respectively, from a 60Co source. The first sample was then deorganified at 200 degreesC using the Soxhlet extraction technique. A third sample was irradiated with 100 Gy after deorganification. The resulting EPR spectra were then compared. It was determined that the dosimetric signal of 2% synthetic carbonated apatite was approximately the same as that of enamel. It was also verified that the dosimetric signal saturates at about 2% in synthetic carbonated apatites. The study established that the precenters responsible for the dosimetric signal (g perpendicular = 2.0018, g parallel = 1.9985) are preferentially concentrated in the surface-accessible region of the mineral component, as shown by the approximately 80% attenuation of the dosimetric signal in dentine following deorganification. The precenters responsible are not destroyed by the deorganification since the magnitude of the dosimetric signal from the dentine specimen irradiated following deorganification was approximately twice that of the comparable untreated, irradiated sample. Finally, the dose response of 2 and 6% synthetic carbonated apatites was determined.

Apatites↗

PubMed2005

Comparative study of apatite formation on CaSiO3 ceramics in simulated body fluids with different carbonate concentrations.

Apatite formation on CaSiO3 ceramics was investigated using two different simulated body fluids (SBF) proposed by Kokubo (1990) and Tas (2000) and three sample/SBF (S/S) ratios (1.0, 2.5 and 8.3 mg/ml) at 36.5 degrees C for 1-25 days. The CaSiO3 ceramic was prepared by firing coprecipitated gel with Ca/Si = 0.91 at 1400 degrees C. The bulk density was 2.14 g/cm3 and the relative density about 76%. The two SBF solutions contain different concentrations of HCO3- and Cl- ions, the concentrations of which are closer to human blood plasma in the Tas SBF formulation than in the Kokubo formulation. The pH values in the former solution are also more realistic. The CaSiO3 ceramics show apatite formation in SBF (Kokubo) after soaking for only 1 day at all S/S ratios whereas different phases were formed at each S/S ratio in SBF (Tas). The crystalline phases formed were mainly apatite at S/S = 1.0 mg/ml, carbonate-type apatite at 2.5 mg/ml and calcite at 8.3 mg/ml. At higher S/S ratios the increase in the Ca concentration became higher while the P concentration became lower in the reacted SBF. These changes in SBF concentrations and increasing pH occurred at higher S/S ratios, producing more favorable conditions in the SBF for the formation of carbonate bearing phases, finally leading to the formation of calcite instead of apatite in the higher HCO3- ion concentration SBF (Tas). Apatite is, however, formed in the lower HCO3- ion concentration SBF (Kokubo) even though the Ca and P concentrations change in a similar manner to SBF (Tas).

Apatites↗

PubMed2005

The influence of calcium fluoride (CaF2) on biaxial flexural strength of apatite-mullite glass-ceramic materials.

OBJECTIVE: The aim of this study was to evaluate the effect of varying the molar percentage of calcium fluoride (CaF2) on the biaxial flexural strength (BFS) of apatite-mullite glass-ceramics. METHODS: Three apatite-mullite glass-ceramic materials were produced based on a formula of 4.5SiO(2)-3Al2O(3)-1.5P2O(5)-3CaO-XCaF2, where X=0.5, 1 and 3 and called HG 1-3, respectively. These materials were used to produce discs of 2 mm thickness and 12 mm diameter using the lost-wax casting process. 30 discs per material were produced, 10 discs per material were cast and then left to bench cool (glass state), 10 discs per material were given a heat treatment at 765, 679 and 629 degrees C for 1h and then heat treated at 890, 860 and 824 degrees C for the HG 1-3, respectively, for another hour to form apatite. Ten discs per material were heat treated as previously described (765, 679 and 629 degrees C) then heat treated for 1h at 1022, 987 and 892 degrees C for the HG 1-3, respectively, to form apatite-mullite. The heat treatment temperatures were obtained from differential thermal analysis data. A lithium disilicate glass-ceramic was used as a control. Biaxial flexural strength (BFS) was determined using a LIoyd 2000R tester. RESULTS: Data showed that the BFS increased as the fluoride content increased, and the apatite-mullite samples had significantly higher BFS values than the as cast glass or apatite samples (p<0.05), with the control having significantly higher BFS values than all the HG glass-ceramic materials for every condition (p<0.05). The fictive glass transition temperature (Tg) was observed to drop with increasing fluoride content. SIGNIFICANCE: Increasing the CaF2 content increased the BFS and decreased the Tg of the glass-ceramic materials tested.

Aluminum Silicates↗

PubMed2002

Apatite formation on zirconium metal treated with aqueous NaOH.

Previous studies by the authors have shown that titanium metal, titanium alloys and tantalum metal which were subjected to aqueous NaOH solution and subsequent heat treatments form an apatite surface layer upon immersion in a simulated body fluid (SBF) with ion concentrations nearly equal to those in human blood plasma. These metals form the apatite surface layer even in living body, and bond to living bone through the apatite layer. In the present study, the apatite-forming ability of NaOH-treated zirconium metal in SBF has been investigated. A hydrated zirconia gel layer was formed on the surface of the zirconium metal on exposure to 1-15 M NaOH aqueous solutions at 95 degrees C for 24h. It was observed that the metals treated in NaOH aqueous solutions with concentrations above 5 M form an apatite layer on their surface in SBF. This indicates that the Zr-OH group of the zirconia gel induces apatite nucleation. The present study points to the possibility of obtaining bioactive zirconium after treatment by NaOH.

Apatites↗

PubMed2002

Morphological regulation and crystal growth of hydrothermal-electrochemically deposited apatite.

Apatite was deposited on commercially pure titanium plates using a hydrothermal-electrochemical method in an electrolyte containing calcium and phosphate ions. Needle-like apatites were synthesized in 43 kinds of condition with different electrolyte temperatures (90-200 degrees C), current densities (5.0-25.0 mA/cm2), and current loading times (10-120 min). The length of one side of the hexagonal apatite and longitudinal length of them were determined through field-emission-type scanning electron microscopic photographs. The size of needle-like apatites remarkably increased with the electrolyte temperature and current loading time, and slightly changed with current density. Multivariate analysis revealed that both size and shape of apatite needle on titanium substrate can be regulated accurately by systematic control of the electrolyte temperature, current density, and current loading time. These results revealed that hydrothermal-electrochemical deposition of apatite consists of two processes: nucleation and crystal growth, which strongly depend on the electrolyte temperature and current density.

Apatites↗

PubMed2004

Lack of OH in nanocrystalline apatite as a function of degree of atomic order: implications for bone and biomaterials.

Using laser Raman microprobe spectroscopy, we have characterized the degree of hydroxylation and the state of atomic order of several natural and synthetic calcium phosphate phases, including apatite of biological (human bone, heated human bone, mouse bone, human and boar dentin, and human and boar enamel), geological, and synthetic origin. Common belief holds that all the studied phases are hydroxylapatite, i.e., an OH-containing mineral with the composition Ca10(PO4)6(OH)2. We observe, however, that OH-incorporation into the apatite crystal lattice is reduced for nanocrystalline samples. Among the biological samples, no OH-band was detected in the Raman spectrum of bone (the most nanocrystalline biological apatite), whereas a weak OH-band occurs in dentin and a strong OH-band in tooth enamel. We agree with others, who used NMR, IR spectroscopy, and inelastic neutron scattering, that-contrary to the general medical nomenclature-bone apatite is not hydroxylated and therefore not hydroxylapatite. Crystallographically, this observation is unexpected; it therefore remains unclear what atom(s) occupy the OH-site and how charge balance is maintained within the crystal. For non-bone apatites that do show an OH-band in their Raman spectra, there is a strong correlation between the concentration of hydroxyl groups (based on the ratio of the areas of the 3572 deltacm(-1) OH-peak to the 960 deltacm(-1) P-O phosphate peak) and the crystallographic degree of atomic order (based on the relative width of the 960 deltacm(-1) P-O phosphate peak) of the samples. We hypothesize that the body biochemically imposes a specific state of atomic order and crystallinity (and, thus, concentration of hydroxyl) on its different apatite precipitates (bone, dentin, enamel) in order to enhance their ability to carry out tissue-specific functions.

Animals↗

PubMed2004

Prediction of apatite lattice constants from their constituent elemental radii and artificial intelligence methods.

Lattice constants (LCs) of all possible 96 apatite compounds, A(5)(BO(4))(3)C, constituted by A[double bond]Ba(2+), Ca(2+), Cd(2+), Pb(2+), Sr(2+), Mn(2+); B[double bond]As(5+), Cr(5+), P(5+), V(5+); and C[double bond]F(1-), Cl(1-), Br(1-), OH(1-), are predicted from their elemental ionic radii, using pattern recognition (PR) and artificial neural networks (ANN) techniques. In particular, by a PR study it is demonstrated that ionic radii predominantly govern the LCs of apatites. Furthermore, by using ANN techniques, prediction models of LCs a and c are developed, which reproduce well the measured LCs (R(2)=0.98). All the literature reported on 30 pure and 22 mixed apatite compounds are collected and used in the present work. LCs of all possible 66 new apatites (assuming they exist) are estimated by the developed ANN models. These proposed new apatites may be of interest to biomedical research especially in the design of new apatite biomaterials for bone remodeling. Similarly these techniques may also be applied in the study of interface growth behaviors involving other biomaterials.

Algorithms↗

PubMed1997

Formation and characteristics of the apatite layer on plasma-sprayed hydroxyapatite coatings in simulated body fluid.

Plasma-sprayed hydroxyapatite (HA) coatings were incubated in simulated body fluids (SBFs) for different periods of time to investigate the nucleation and growth of apatite on their surface. The layer that formed was recognized as having similarities to bone apatite because it is poorly crystallized, non-stoichiometric or calcium deficient, and contains carbonate and magnesium. Scanning electron microscopy (SEM) and infrared spectroscopy (IR) were employed to investigate the morphological changes of the coating surface and the structure of the grown layer respectively. In the first few hours, calcium and phosphate ions dissolved from the coatings so as to increase their local supersaturation to a higher degree, thereafter followed by the nucleation and growth of apatite. The nucleation occurred firstly on the recessed regions, inside pores and cracks where the higher supersaturation was readily maintained. Only after 24 h incubation was a complete layer formed on the surface of the coating. There is no obvious interface between the grown layer and the underlying coating. Heat treatment in the air made the apatite transform into biphasic calcium phosphate of HA and tricalcium phosphate, with a blue colour because of trace manganese ions. The heat-treated HA coating showed no dissolution by SEM observation. This resulted in no precipitation on the surface. When SBF was used with two-fold higher ion concentrations, the apatite layer formed slowly in 72 h without dissolution of the coating surface. This may mean that the microenvironment with a sufficiently high degree of supersaturation of calcium and phosphate ions is crucial for apatite to nucleate and grow in SBF, while the HA crystalline structure is not critical in the nucleation process, as expected.

Apatites↗

PubMed1997

Apatite deposition on titanium surfaces--the role of albumin adsorption.

Titanium implant surfaces are known to spontaneously nucleate apatite layers when in contact with simulated body fluids. However, adsorption of proteins may influence the process of apatite layer formation. In this study the role of bovine serum albumin (BSA) adsorption in the process of apatite deposition on titanium substrates is investigated. Deposition of calcium phosphate was induced by immersing titanium substrates in a Hank's balanced salt solution (HBSS) for times ranging from 1 to 23 days. The resulting substrates were studied by scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS), wettability measurements and electrochemical impedance determinations. All these methods indicate the presence of a calcium phosphate layer. The same procedure was repeated substituting HBSS with a solution of BSA in HBSS. Although SEM, EDS and electrochemical impedance spectra do not reveal the presence of an apatite layer, XPS analysis strongly indicates that the inhibition of apatite formation by BSA is only partial. The competition between BSA adsorption and apatite deposition seems to lead to a mixed film where the protein co-exists with calcium phosphate. Wettability studies suggest that this surface film is heterogeneous and porous, similar to the thicker films formed in albumin-free HBSS.

Adsorption↗