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PubMed1997

Apatite layer-coated titanium for use as bone bonding implants.

For development of thin bioactive coatings on metal implants, a dense and uniform apatite layer was coated onto titanium (Ti) implants in situ by using a new biomimetic method, which is composed of apatite nucleation and growth steps in simulated body fluid (SBF). Analysis of the coatings by thin film X-ray diffraction and scanning electron microscopy-energy dispersive X-ray microanalysis (SEM-EMPA) before implantation showed that its characteristics were very similar to those of natural bone. The coated and uncoated rectangular plates were bilaterally implanted into the tibial proximal metaphyses of rabbits. After 6, 10 and 25 weeks post-implantation, the bone bonding and bone formation at the bone-implant interfaces were evaluated by a detachment test and undecalcified histological examination. Mechanical testing in tension showed that the failure load of apatite layer-coated Ti implants was significantly higher than that of uncoated control at each time period (all P < 0.001). Histologically, it was shown that bone was deposited directly onto the apatite coating without any intervening soft tissue, while in the paired controls, interpositional soft tissue was seen at the bone-implant interface. By SEM-EPMA, a uniform calcium- and phosphorus-rich layer was detected between the coated implants and bone, but not in uncoated controls at either earlier or later time periods. The results indicate that the apatite layer deposited on Ti in situ may significantly increase the bone bonding strength by providing a bioactive surface, which allows for an early bone apposition to the implant. In addition, the apatite layer-coated Ti produced by the biomimetic process may fulfil the requirements of favourable thin coatings and strong adhesion at the metal-coating interface.

Analysis of Variance↗

PubMed1998

Heterogeneous fluoridated apatites synthesized with a three-step fluoride supply system.

Two types of heterogeneous fluoridated apatite, H-F-H and F-H-F, were synthesized by supplying fluoride during the middle half (H-F-H) or initial and final quarters (F-H-F) of the experimental period. Although X-ray diffraction patterns and SEM photographs of both H-F-H and F-H-F-type apatites were not significantly different, high-resolution transmission electron microscopy showed quite different features; H-F-H-type apatite crystals were elongated hexagons, while those of F-H-F-type apatite were rather wider hexagons with electron damage in three-quarters of the inner core. These results supported the previous speculations on the two different types of heterogeneous fluoridated hydroxyapatites synthesized with fluoride concentrations stoichiometrically equivalent to that of fluorapatite: hydroxyapatite covered with fluorapatite and fluorapatite covered with hydroxyapatite. F-H-F-type apatite was less soluble than that of H-F-H-type apatite.

Apatites↗

PubMed1992

The role of brushite and octacalcium phosphate in apatite formation.

Studies of apatite mineral formation are complicated by the possibility of forming several calcium phosphate phases. The least soluble, hydroxyapatite (HAP), is preferentially formed under neutral or basic conditions. In more acidic solutions phases such as dicalcium phosphate dihydrate (Brushite, DCPD) and octacalcium phosphate (OCP) are often found. Even under ideal HAP precipitation conditions the precipitates are generally nonstoichiometric, suggesting the formation of calcium-deficient apatites. Both DCPD and OCP have been implicated as possible precursors to the formation of apatite. This may occur by the initial precipitation of DCPD and/or OCP followed by transformation to a more apatitic phase. Although DCPD and OCP are often detected during in vitro crystallization, in vivo studies of bone formation rarely show the presence of these acidic calcium phosphate phases. In the latter case the situation is more complicated, since a large number of ions and molecules are present that can be incorporated into the crystal lattice or adsorbed at the crystallite surfaces. In biological apatite, DCPD and OCP are usually detected only during pathological calcification where the pH is often relatively low. In normal in vivo calcifications these phases have not been found, suggesting the involvement of other precursors or the formation of an initial amorphous calcium phosphate phase (ACP) followed by transformation to apatite.

Apatites↗

PubMedDate not supplied

Apatite and phillipsite as sequestering agents for metals and radionuclides.

Laboratory and greenhouse studies were conducted to quantify apatite and phillipsite (zeolite) sequestration of selected metal contaminants. The laboratory batch study measured the sorption of aqueous Co2+, Ba2+, Pb2+, Eu3+, and UO2(2+). Apatite sorbed more Co2+, Pb2+, Eu3+, and UO2(2+) from the spike solution than phillipsite, resulting in distribution coefficients (Kd values) of >200,000 L kg(-1). Phillipsite was more effective than apatite at sorbing aqueous Ba2+. Results from the laboratory study were used to design the greenhouse study that used a soil affected by a Zn-Pb smelter from Pribram, Czech Republic. Two application rates (25 and 50 g kg(-1)) of phillipsite and apatite and two plant species, maize (Zea mays L.) and oat (Avena sativa L.), were evaluated in this study. There was little (maize) to no (oat) plant growth in the unamended contaminated soil. Apatite and, to a slightly lesser extent, phillipsite additions significantly enhanced plant growth and reduced Cd, Pb, and Zn concentrations in all analyzed tissues (grain, leaves, and roots). The sequestering agents also affected some essential elements (Ca, Fe, and Mg). Phillipsite reduced Fe and apatite reduced P and Fe concentrations in oat tissues; however, the level of these elements in oat leaves and grains remained sufficient. Sequential extractions of the soil indicated that the Cd, Pb, and Zn were much more strongly sorbed onto the amended soil, making the contaminants less phytoavailable.

Adsorption↗

PubMed2002

[The effects of surface morphology of calcium phosphate ceramics on apatite formation in dynamic SBF].

Bone-like apatite formation on the surface of calcium phosphate ceramics has been believed to be the prerequisite of new bone growth on ceramics and to be related to the osteoinductivity of the material. The research of the factors effecting bone-like apatite formation is a great help in understanding the mechanism of osteoinduction. This paper is aimed to a comparative study of in vitro formation of bone-like apatite on the surface of dense and rough calcium phosphate ceramics with SBF flowing at different rates. The results showed that the rough surface was beneficial to the formation of bone-like apatite, and the apatite formed faster in 1.5 SBF than in SBF. Rough surface, namely, larger surface area, increased the dissolution of Ca2+ and HPO4(2-) and higher concentration of Ca2+ and HPO4(2-) ions of SBF and was in turn advantageous to the accumulation of Ca2+, HPO4(2-), PO4(3-) near the ceramic surface. Local supersaturating concentration of Ca2+, HPO4(2-), PO4(3-) near sample surface was essential to nucleation of apatite on the surface of sample.

Apatites↗

PubMed2002

[A study of bone-like apatite formation on porous calcium phosphate ceramics in dynamic SBF].

This study aimed at investigating the influence of the flow rate of simulated body fluid (SBF) (2 ml/100 ml.min) of body fluid in skeletal muscle upon the formation of bone-like apatite on porous calcium phosphate ceramics. The in vitro immersion experiment in SBF flowing at normal physiological rate is referred to as dynamic SBF. The results showed that bone-like apatite could only formed in the pores of porous calcium phosphate when SBF flow at physiological rate (2 ml/100 ml.min) of body fluid in skeletal muscle. At the same time, bone-like apatite could form both in the pores and on the surface of the samples if the flowing physiological solution is 1.5 SBF. When the flowing speed of SBF is higher than normal physiological speed (10 ml/100 ml.min), no bone-like apatite could be detected both on the surface and in the pores of the materials. This result is in concordance with animal experiments. The dynamic SBF simulates the biological environment of bone-like apatite formation in body better than static SBF (SBF does not flow). This method is very useful for the research of the mechanism of bonelike apatite formation, which is the key step of bone growth on biomaterials, and can be used as an effective approach to investigate mechanism of the osteoinduction of calcium phosphate in nonosseous tissues in vivo.

Apatites↗

PubMed2004

Effect of solid/solution ratio on apatite formation from CaSiO3 ceramics in simulated body fluid.

The effect of the solid/solution (S/S) ratio on apatite formation from CaSiO3 ceramics in simulated body fluid (SBF) was investigated. CaSiO3 ceramics with a Ca/Si ratio of 0.91 were prepared by sintering CaSiO3 powder coprecipitated from ethanol solutions of Ca(NO3)2. 4H2O and Si(OC2H5)4 using NH4OH as the precipitant. These ceramics were reacted with SBF at S/S ratios of 1.0, 2.5 and 8.3 mg/ml at 36.5 degrees C for various times. Formation of apatite was observed at all the S/S ratios after soaking for 1 day. The amount and microstructure of the apatite obtained at a S/S ratio of 8.3 mg/ml, however, differed largely from the product formed at the other two S/S ratios. The apatite formed at S/S = 8.3 mg/ml was of smaller particle size, formed in smaller amount and with less preferred orientation of the (001) of apatite crystals compared with those formed at S/S = 1.0 and 2.5 mg/ml. An increase of Ca and decrease of the P components occurred in the soaked SBF at S/S = 8.3 mg/ml, the changes being much more marked than with the other two S/S ratios. These differences in the concentration changes in SBF at different S/S ratios are attributed to the difference in the apatite formation from the CaSiO3 ceramics.

Apatites↗

PubMed2005

Apatite as an interesting seed to remove phosphorus from wastewater in constructed wetlands.

Intensive use of phosphates has resulted in high P levels in surface waters and therefore eutrophication problems. Over the last decade many studies have revealed the advantage of using specific materials with efficient phosphorus retention capacities. Recent studies state that Ca materials are of particular interest for long-term retention of P, but can induce negative effects. To improve P retention and avoid negative counter-effects we tested the potential of natural apatites. Apatite sorption was evaluated using batch and open reactor experiments. Batch experiments identify sorption mechanisms and the influence of the ionic characteristics of the solution; open reactor experiments evaluate sorption capacities in relation to the ionic composition of the solution and biomass development. In parallel, observation of the material by electron microscopy was used to give more precision information about the mechanisms involved. This work reveals the strong chemical affinity between apatites and phosphorus. Compared to other calcareous materials apatite is better able to maintain low outlet P levels. After more than 550 days feeding, sorption was still present and low P outlet levels were still being obtained when sufficient contact time and calcium content in the solution were ensured. This work demonstrates the advantages of using apatites for phosphorus removal in constructed wetlands. The behaviour of apatite in phosphorus retention is explained and its suitability for use in such extensive systems defined.

Adsorption↗

PubMed1989

Recent uses of electron microscopy in the study of physico-chemical processes affecting the reactivity of synthetic and biological apatites.

Studies which used scanning electron microscopy (SEM) to investigate subsurface demineralization of dental enamel have recently been well reviewed. The purpose of the present paper was to review several studies, carried out in our laboratories, which have used electron microscopy to examine physicochemical properties of synthetic and biological apatites, to relate these results to previous studies, and to present new data. Aspects of the ultrastructure of hydroxyapatite and carbonated-apatites have been observed by high resolution transmission electron microscopy, and related to shape and growth of these crystals. Surface morphologies of discs prepared from precipitated carbonated-apatites and from ceramic carbonated-apatites were examined by SEM and the information was used in the interpretation of apatite dissolution studies relevant to dental caries. Improvements in the technique of backscattered electron imaging of demineralized enamel have enabled better interpretation of enamel caries experiments. SEM examination of enamel and dentin treated by low energy lasers of specific wavelengths have shown that lasing conditions can be chosen that produce surface fusion of the apatite which inhibits caries-like lesion progression. SEM examination of crystals formed on and in enamel during high concentration fluoride treatments implies that calcium fluoride-like crystals are formed and they may act as a slow-release fluoride reservoir in the mouth.

Apatites↗

PubMed1982

Preparation, analysis, and characterization of carbonated apatites.

A range of synthetic carbonated apatites were characterized using infrared and Raman spectroscopy, X-ray diffraction, and chemical analysis and compared to stoichiometric hydroxyapatite and dental enamel. Synthetic apatites were prepared by aqueous precipitation and by solid-state reaction at high temperatures. A method is described for the carbonate determination of apatite samples using gas chromatography. This study demonstrates that carbonate exists in two crystallographically distinct sites in the apatite crystal structure and is consistent with a carbonate-for-phosphate substitution mechanism, where four carbonate groups replace three phosphate groups. Sodium and hydroxyl ions are shown to be involved with the substitution of carbonate ions in the apatite structure. Observed sodium/carbonate and calcium/phosphorus molar ratios confirm this mechanism. Substitution of this type may explain the predominant mode of carbonate substitution in biological apatites.

Apatites↗

PubMed1994

Hemolytic activity of phosphorite and apatite dusts in vitro.

An examination was performed to assess the hemolytic activity of phosphorite and apatite dust in vitro by a method used by Potts et al. (1978). After evaluation of dispersion, a certain contents of elements was established, using a spectrometer of X-ray fluorescence. Phosphorite dusts caused 50.4% of hemolyse that is about 5 times more than those caused by dust of apatites. The mean hemolysis index for phosphorite dust was 0.799 and for apatite dust 0.142. Thus, phosphorites are much more toxic to a human being than apatites. A higher level of hemolytical activity in phosphorite dust as compared to apatite one can be explained by significant difference in the contents of certain elements, SiO2, in particular. The mean SiO2 level in samples containing phosphorites was 6.3 +/- 0.1% compared to samples of apatites (3.8 +/- 0.09%).

Apatites↗

PubMed2004

In vitro apatite induction by osteopontin: interfacial energy for hydroxyapatite nucleation on osteopontin.

Noncollagenous phosphoproteins that interact with type I collagen are thought to nucleate the mineral phase to the collagen fibril network of mineralized tissues. We previously reported that a specific dentin phosphoprotein, phosphophoryn, crosslinked to an insoluble substrate such as type I collagen fibrils, was an effective nucleator of apatite. In this study, we investigated the capacity of another phosphoprotein in dentin, osteopontin, for apatite nucleation in vitro. Osteopontin purified from bovine milk was either absorbed to agarose beads or crosslinked to agarose beads. Each preparation was incubated at 37 degrees C in metastable solutions. Apatite was induced by osteopontin that was crosslinked to agarose beads, whereas osteopontin adsorbed to agarose beads failed to induce apatite crystal formation. Using classical nucleation theory, the interfacial energy for hydroxyapatite nucleation on osteopontin crosslinked to agarose beads was determined to be 94.7 ergs/cm(2). This value is larger than that for phosphophoryn, though it is similar to that for hydroxyapatite. The present study indicates that osteopontin, like phosphophoryn, has a high potential to induce apatite formation when it is covalently bound to some substrate in vitro, and suggests the possibility that osteopontin bound to type I collagen may induce apatite formation in vivo.

Animals↗

PubMed1999

Observations on the Apparent Solubility of Carbonate-Apatites.

Previousreports indicating that the apparent solubilities of carbonate-apatites are low appear to conflict with findings that carbonate incorporation into the apatite structure tends to reduce stability. Carbonate-apatites were prepared by a precipitation method and by hydrolysis of monetite and brushite. Apparent solubility profiles were determined by measuring dissolution after exposure for 24 h to acetate buffers with known saturations with respect to hydroxyapatite. All preparations showed a range of apparent solubilities, in agreement with previous work. Precipitated samples had higher apparent solubilities than samples prepared by hydrolysis and this was correlated with differences in crystallinity. Further experiments showed that pyrophosphate ion reduced the apparent solubility, but it was concluded that pyrophosphate occurring naturally in synthetic apatites would be insufficient to cause low apparent solubilities. Microscopical observations showed that precipitated carbonate-apatites were composed of small crystals of uniform size, whereas carbonate-apatites prepared by hydrolysis consisted of both small crystals and very large crystals. The low apparent solubilities observed in the latter preparations are attributed to the large crystals. The surface phenomena possibly involved in apparent solubility behavior are discussed. Copyright 1999 Academic Press.

Journal Article↗

PubMed1998

Surface modification of nano-apatite by grafting organic polymer.

Since surface properties of hydroxyapatite (HA) play an important role in its performance, surface modification of HA has gained much attention from researchers. Silane coupling agents have been the focus of the research. In this study, an effective surface modification method was developed using hexamethylene diisocyanate as a coupling agent. Polyethylene glycol (Mw = 1500) was successfully coupled to the surface of nano-size apatite particles (nano-apatite). Various methods were used to characterize the surface-modified nano-apatite. Infra-red spectra confirmed the existence of a layer of polymer with both urethane and ether linkage on the surface of nano-apatite. The amount of grafted polymer as determined by total organic carbon analysis (TOC) and thermal gravimetric analysis (TGA) was about 20% in weight. Solid 1H MAS NMR spectra indicated that the amount of hydroxyl groups of nano-apatite was decreased by 7.7% after surface grafting reaction. It is concluded that the surface hydroxyl groups of nano-apatite have the reactivity towards isocyanate groups.

Carbon↗

PubMed1999

Functionally graded fluoridated apatites.

Fluoridated hydroxyapatite was synthesized at 80 +/- 1 degree C and pH 7.4 +/- 0.2 using a gradient fluoride supply system. X-ray diffraction analysis showed a typically apatitic pattern, although the (3 0 0) reflection was broader than that of homogeneous fluorapatite. Scanning electron micrographic observation indicated that the apatite was composed of rod-like crystals similarly to fluorapatite. High-resolution transmission electron microscopy showed electron damage in the core of the crystal. When the apatite pellet was prepared, electron spectroscopy for chemical analysis showed a negative gradient of fluoride concentration with depth in the crystals. The apparent solubility in 0.5 mol/l acetate buffer solution (37 degrees C and pH 4.0) was 9.16 +/- 0.39 mmol/l, much less than that of homogeneous hydroxyapatite 32.3 +/- 1.9 mmol/l, and less than that of heterogeneous two-layer fluoridated apatite with an outer fluoride-rich layer 12.5 +/- 0.6 mmol/l, which was synthesized previously by supplying fluoride during the latter half of the experimental period. These results suggest that graded fluoridated apatite may be formed by this process and have higher acid resistance than two-layer fluoridated apatite.

Crystallography, X-Ray↗

PubMed1997

Magnesium-containing carbonate apatites.

Hydroxyapatites precipitated at pH 7.0 and 9.0 with and without carbonate and with different amounts of magnesium were studied. Mg uptake, Ca/P ratios, and lattice constant data indicate that Mg is incorporated into the apatite lattice. IR spectra demonstrate the formation of B-type carbonate apatites with carbonate substituting for phosphate. Decomposition of carbonate-containing apatites at elevated temperatures up to 1000 degrees C is more gradual for apatites prepared at pH 9.0 than for those prepared at pH 7.0 for which an abrupt loss of carbonate occurs after 600 degrees C. Compounds synthesized without added carbonate partially transform to beta Ca3(PO4)2 (TCP) at about 700 degrees C. Greater transformation to TCP occurs as the Mg incorporation is increased, indicating the insertion of Mg into TCP and consequent stabilization of the TCP. SEM micrographs show increases in the size of crystallites when apatites are precipitated with Mg (in the 0.2-1.5% range), providing further evidence for Mg incorporation into the apatite structure.

Calcium↗

PubMed2004

Lattice energies of apatites and the estimation of DeltaH f degrees (PO 4 3-, g).

Experimentally based lattice energies are calculated for the apatite family of double salts M(5)(PO(4))(3)X, where M is a divalent metal cation (Ca, Sr, Ba) and X is hydroxide or a halide. These values are also shown to be estimable, generally to within 4%, using the recently derived Glasser-Jenkins equation, U(POT) = AI(2I/V(m))(1/3), where A = 121.39 kJ mol(-)(1). The apatites exhibiting greater covalent character (e.g., M = Pb, Cd, etc.) are less well reproduced but are within 8% of the experimentally based value. The lattice energy for ionic apatites (having identical lattice ionic strengths, I) takes the particularly simple form U(POT)/kJ mol(-)(1) = 26680/(V(m)/nm(3))(1/3), reproducing cycle values of U(POT) well when V(m) is estimated by ion volume summation and employing a volume for the PO(4)(3)(-) ion (not previously quantified with an associated error) of 0.063 +/- 0.003 nm(3). A value for the enthalpy of formation of the gaseous phosphate ion, DeltaH(f)( ) degrees (PO(4)(3)(-), g), is absent from current thermochemical tabulations. Examination of solution and solid state thermochemical cycles for apatites, however, leads us to a remarkably consistent value of 321.8 +/- 1.2 kJ mol(-)(1). Experimental and estimated lattice energies were used along with other thermodynamic data to determine enthalpies, entropies, and free energies of dissolution for apatites of uncertain stabilities. These dissolution values are compared with the corresponding values for stable apatites and are used to rationalize the relative instability of certain derivatives.

Journal Article↗

PubMed2000

Needle-like apatite-leucite glass-ceramic as a base material for the veneering of metal restorations in dentistry.

A needle-like apatite-leucite glass-ceramic was prepared in the SiO2-Al2O3-Na2O-K2O-P2O5-F system. Nucleation and crystallization processes were studied in bulk and powdered samples. The crystallization of leucite follows the mechanism of surface crystallization. After the precipitation of NaCaPO4 crystals and another unknown crystal phase, the formation of needle-like apatite is based on a volume nucleation and crystallization process. The mechanism of the formation of needle-like apatite differs to those of apatite precipitation in glass-ceramics. The morphology of needle-like apatite is comparable to that of apatite in natural teeth. The properties of the glass-ceramic, especially the good chemical durability, the optical properties, as well as mechanical and thermal properties allow glass-ceramic to be used as a main component in a bio-material for the veneering of metal restorations in dentistry.

Journal Article↗