Apatite Particles Research Articles

Synthesis of Dense Collagen/Apatite Composites Using a Biomimetic Method

In this article we describe a simple but effective biomimetic method to prepare dense apatite/collagen nanocomposites. Collagen-containing simulated body fluid was used to mimic the natural bone formation environment. The apatite/collagen films were formed at the air–solution interface under physiological conditions (40°C and pH=6.3). Transmission electron microscopy, scanning electron microscopy, thermal gravimetric analysis, X-ray diffraction, western blot analysis, and energy-dispersive X-ray were used to characterize the apatite/collagen composites. It was revealed that the nanosized apatite particles formed into a platelet shape with 100 nm in width and length and <10 nm in thickness. The collagen existed around the apatite platelets and acted as a glue to bind these platelets together. The collagen and apatite were strongly adhered to each other and formed into dense composite.

Tribological properties of polyvinyl alcohol hydrogel reinforced with nanometer hydroxy apatite

As a potential artificial cartilage material, the friction and wear properties of nano-hydroxy apatite (HA) particles filled poly (vinyl alcohol) hydrogel (PVA-H) composites sliding against stainless steel disk under water lubrication condition were studied by using a four ball tester. The worn surfaces were investigated by using a scanning electron microscope (SEM) to determine the wear mechanisms. Experimental results show that filling HA to PVA-H will slightly increase the friction coefficient of composites with the increasing of HA content under water lubrication condition. Meanwhile, HA particles can greatly reduce the wear mass loss of the PVA-H composites and enhance the load carrying capacity, the wear loss of the 1 wt% HA reinforced PVA-H composites can be decreased by 30 percent under 2.0 MPa to 50 percent under 0.5 MPa contact pressure. We also found that 2 wt% HA content of composites increase the wear mass loss under the same condition. SEM examination shows that the worn surface of low HA containing (1 wt%) composites are much smoother than that of pure PVA-H or high HA containing (2 wt%) composites under 1.5 MPa contact pressure. It is also found that there are big hole and big reunited HA particles in the surface of 2 wt% HA containing composites, which leads to deterioration of the surface of samples under higher loads in water lubrication. These results may be useful in the tribological design of artificial articular cartilage material.

Potential environmental impact of dissolution of raw phosphate in sea water of the Gulf of Aqaba

Dissolution of raw phosphate (apatite) in sea water of the Gulf of Aqaba was investigated through lab incubation experiments. Three types from three different sources (Al-Hasa, Al-Abyad and Esh-Shydiya) have been used for these experiments. Impact of quantity, grain size, and source (type) of raw phosphate on dissolution rate were studied. Statistical analysis shows significant differences between the results obtained from comparing each two weights; as weight of apatite increased, dissolved inorganic phosphate-phosphorus (DIP) and fluoride in sea water solution increased. The differences between the dissolution rates of raw phosphate from the three sites were not significant while the differences between the different grain size fractions were significant. Dissolution rates were inversely related to particle size. Using a worst-case scenario, a conservative estimate of the maximum increase in DIP in seawater of the Gulf of Aqaba due to the apatite particles lost to the sea during ship loading resulted in DIP concentrations of 0.03 μM per year. As the residence time of the water in the Gulf of Aqaba is about one year, the DIP concentration will not increase by more than 0.03 μM under the estimated annual quantity of exported phosphate. Fluoride will not increase by more than 0.03 mg/l under the same conditions.

Mechanism of apatite formation on silicon suboxide film prepared by pulsed metal vacuum arc deposition

Pulsed metal vacuum arc deposition technology was employed to fabricate SiO x ( x ≤ 2) film at the oxygen partial pressure at 0.6 × 10 −2 Pa. Surface characteristics of the as-deposited SiO x film were studied by X-ray photoelectron spectroscopy (XPS) and atomic force microscopy (AFM). Results show that the film is substoichiometric and abundant oxygen vacancies exist in the film. The as-deposited film was immersed in simulated body fluid (SBF) for evaluation of in vitro bioactivity. After incubation in SBF, ball-like apatite particles were found on the film surfaces by scanning electron microscopy (SEM), X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR). The mechanism of apatite deposition on the SiO x film was explained in terms of the silanol functional groups formed on the surface of the film after immersion in SBF. There are abundant active oxygen vacancies in the SiO x film that were attacked by the water molecules in the solution and then formed silanol groups in the film. The silanol groups adsorbed calcium and phosphate ions from the solution to the hydrated surface to form critical apatite cluster. Once the apatite nuclei are formed, they spontaneously grow by consuming calcium and phosphate ions in the surrounding fluid.

Enhancement of in vitro apatite-forming ability of thermally oxidized titanium surfaces by ultraviolet irradiation

Ultraviolet (UV) light was irradiated in air for 1 h on titania (rutile) films prepared by thermal oxidation of titanium substrates from 300°C up to 800°C, coded as HT300UV, HT400UV, HT500UV, HT600UV, HT700UV, and HT800UV, respectively. All samples were then soaked in a simulated body fluid (SBF, Kokubo solution) and their in vitro apatite-forming ability was evaluated. It was found that bone-like apatite particles were deposited on HT500UV, HT600UV, and HT700UV within 7 d whereas that was not the case with others during the same period. Moreover, the apatite particles were deposited more on HT500UV than on the others. Therefore, the ultraviolet light irradiation enhanced the in vitro apatite-forming ability of the thermally oxidized titanium.

Sintering behavior and mechanical properties of the mica–diopside machinable glass-ceramics

The machinability of fluor-mica glass-ceramics is an attractive characteristic of these materials. However, the poor mechanical strength and hardness has limited their applications. In this research, to overcome this problem, a glass frit in the system CaO–SiO 2–P 2O 5–MgO was gradually added to a mica-based frit. After sintering of compacted mixtures, simultaneous crystallization of diopside and mica occurred that led to improved mechanical properties. The sinterability of various samples was investigated and their microstructure and crystallinity were evaluated by electron microscopy (SEM) and X-ray diffraction (XRD). The presence of plate-like crystals of mica, spherical particles of apatite and fibrous inclusions of diopside was the microstructural specification of the optimum composition. The four-point bending strength and the Vickers microhardness of samples were also determined.

Effects of calcination temperature on the drug delivery behaviour of Ibuprofen from hydroxyapatite powders

The effects of heat treatment time and temperature on the delivery behaviour of Ibuprofen from hydroxyapatite particles were investigated in this study. The drug release was seen to follow Fickian diffusion for the initial period of release for all heat treatment conditions. The gradient of Fickian release increased with (1) increasing crystallite size, attributed to the decreasing amount of boundary area, and (2) with decreasing surface area, due to the reduction in porosity and hence tortuosity within the apatite particles. This study has shown that altering the heat treatment conditions used to calcine hydroxyapatite may alter its drug delivery abilities, whereby calcination temperature was noted to influence the drug release behaviour to a greater extent than calcination time.

Preparation and properties of a novel bone repair composite: nano-hydroxyapatite/chitosan/carboxymethyl cellulose

Nano-hydroxyapatite/chitosan/carboxymethyl cellulose (n-HA/CS/CMC) composites with weight ratios of 70/10/20, 70/15/15 and 70/20/10 were prepared through a co-solution method. The properties of the composites were characterized by means of burn-out test, IR, XRD, TEM and universal material testing machine. The degradation and bioactivity were also investigated by in vitro test in a simulated body fluid (SBF) for 8 weeks. The results showed that n-HA particles were dispersed uniformly in organic phase, and strong chemical interactions formed among the three phases. Moreover, the composites were similar to natural bone in morphology and size. In addition, the compressive strength was improved compared with n-HA/CS composite. The biodegradation rate was controllable by altering weight ratio of the CS/CMC. Meanwhile, the composites could induce apatite particles to deposit in SBF. All the above results indicate that the novel composites of n-HA/CS/CMC have a promising prospect used for bone repair materials in view of the good mechanical property, adjustable biodegradation rate and bioactivity in SBF. Additionally, the study would provide a good guide to exploit clinical application of natural cellulose.

A mesoporous bioactive glass/polycaprolactone composite scaffold and its bioactivity behavior

Composite scaffolds of mesoporous bioactive glass (MBG)/polycaprolactone (PCL) and conventional bioactive glass (BG)/PCL were fabricated by a solvent casting-particulate leaching method, and the structure and properties of the composite scaffolds were characterized. The measurements of the water contact angles suggest that the incorporation of either MBG or BG into PCL can improve the hydrophilicity of the composites, and the former is more effective than the later. The bioactivity of the composite scaffold is evaluated by soaking the scaffolds in a simulated body fluid (SBF) and the results show that the MBG/PCL composite scaffolds can induce a dense and continuous layer of apatite after soaking in SBF for 3 weeks, as compared with the scattered and discrete apatite particles on the BG/PCL composite scaffolds. Such improvements (improvements of the hydrophilicity and apatite forming ability) should be helpful for the extensive applications of PCL scaffold in tissue engineering.

An electrospun triphasic nanofibrous scaffold for bone tissue engineering

A nanofibrous triphasic scaffold was electrospun from a mixture of polycaprolactone (PCL), type-I collagen and hydroxyapatite nanoparticles (nano-HA) with a mixture dry weight ratio of 50/30/20, respectively. Scaffolds were characterized by evaluating fiber morphology and chemical composition, dispersion of HA particles and nanoindentation. Scanning electron microscopy revealed fibers with an average diameter of 180 ± 50 nm, which coincides well with the collagen fiber bundle diameter characteristic of the native extracellular matrix of bone. The triphasic fibers, stained with calcein and imaged with confocal microscopy, show a uniform dispersion of apatite particles throughout their length with minor agglomeration. Scaffold fibers of triphasic (50/30/20), collagen/nano-HA (80/20), PCL/nano-HA (80/20), pure PCL and pure collagen were each pressure consolidated into non-porous pellets for evaluation by transmission electron microscopy and nanoindentation. While the majority of apatite particles are uniformly dispersed having an average size of 30 nm, agglomerated particles as large as a few microns are sparsely distributed. Nanoindentation of the pressure-consolidated scaffolds showed a range of Young's modulus (0.50–3.9 GPa), with increasing average modulus in the order of (PCL < PCL/nano-HA < collagen < triphasic < collagen/nano-HA). The modulus data emphasize the importance of collagen and its interaction with other components in affecting mechanical properties of osteoconductive scaffolds.

Anatase/rutile dual layer deposition due to hydrolysis of titanium oxysulfate with hydrogen peroxide solution at low temperature

Anatase/rutile dual layers were deposited on titanium and polyethylene substrates when they were soaked in TiOSO4/H2O2 solution and aged in hot water: The dense bottom layer predominantly consisted of rutile, while the upper layer consisted of loosely packed aggregation of anatase particles. The titania deposition was the results of compromise among three conflicting processes: (1) hydrolysis of TiOSO4 to yield either soluble titania-H2O2 complexes or titania, (2) dissolution of the titania layer under the presence of H2O2, and (3) corrosive reactions between titanium substrates and H2O2 to yield similar complexes or compounds. The dissolution–deposition equilibrium was found associated with pH of the sulfate solution and changed with soaking time. Thus, proper pH value and soaking time in the treating solution were the two key factors to control the formation of dense titania layers. The resulted titania layers were easily covered with fine apatite particles when soaked in a solution supersaturated with its component ions.

Formation of Apatite within Biodegradable Scaffolds by an Accelerated Biomimetic Process in the Shaking Condition and Flow Condition

Bonelike apatite coating was formed on poly(L-lactic acid) (PLLA) scaffolds and poly(glycolic acid) (PGA) scaffolds in 24 hours through an accelerated biomimetic process. The ion concentrations in the simulated body fluid (SBF) were nearly 5 times of those in human blood plasma. The apatite formed in 5SBF was similar in morphology and composition to that formed in the classical biomimetic process employing SBF or 1.5SBF, and similar to that of natural bone. To facilitate coating into scaffolds, the flowing condition was introduced into the accelerated biomimetic process. It was found that the accelerated biomimetic process performed in the flowing condition yielded more uniform spatial distribution of apatite particles than that in the regular shaking condition.

In Vitro Apatite-Forming Ability of Titania Films Depends on Their Substrates

Titania films were coated by means of sol-gel method on various substrates such as titanium, titanium alloy, silicon wafer, stainless-steel, alumina, and glass slide where they coded as C5Ti, C5Ti6Al4V, C5Si, C5SUS, C5Al2O3 and C5GS, respectively. Their in vitro apatite-forming ability was examined with the Kokubo’s simulated body fluid (SBF; pH 7.4, 36.5°C). C5Ti, C5Ti6Al4V and C5Si deposited apatite particles on their surface within 7 days, whereas, C5SUS, C5Al2O3 and C5GS did not. These results implied that the in vitro apatite-forming ability of the titania films indirectly depended on the chemical or physical properties of the substrates.

Biocompatibility and Mechanical Performance of Ni-Ti

Biomimetic apatite deposition behaviors and mechanical performance for as-rolled and annealed Ni-Ti plates were investigated. Apatite nucleation and growth on Ni-Ti in SBF (simulated body fluid) was not appreciably influenced by heat treatment. But, the apatite deposition rate increased slightly by NaOH surface treatment. The nodular apatite on the deposited layer is favored on a macro-scale since the surface energy of polycrystalline apatite particles can be reduced by forming nodules. The weight gain after apatite deposition for Ni-Ti (0.004 g/cm2) after 10 days were found to be smaller that that of NaOH treated Ti-6Al-4V, but it was comparable to that of non- NaOH-treated Ti-6Al-4V (0.004 g/cm2). The stress-strain responses of annealed Ni-Ti displayed the pseudoelastic behavior associated with stress-induced martensite formation with the transition stress for the martensite formation equal to 320 MPa. On the other hand the cold worked Ni-Ti displayed no appreciable pseudoelastic region and the yield stress was ~500MPa. A good biomimetic apatite formation and excellent mechanical performance of Ni-Ti suggests that Ni-Ti can be an excellent candidate material for orthopedic implants.

Cooperative deformation of mineral and collagen in bone at the nanoscale

In biomineralized tissues such as bone, the recurring structural motif at the supramolecular level is an anisotropic stiff inorganic component reinforcing the soft organic matrix. The high toughness and defect tolerance of natural biomineralized composites is believed to arise from these nanometer scale structural motifs. Specifically, load transfer in bone has been proposed to occur by a transfer of tensile strains between the stiff inorganic (mineral apatite) particles via shearing in the intervening soft organic (collagen) layers. This raises the question as to how and to what extent do the mineral particles and fibrils deform concurrently in response to tissue deformation. Here we show that both mineral nanoparticles and the enclosing mineralized fibril deform initially elastically, but to different degrees. Using in situ tensile testing with combined high brilliance synchrotron X-ray diffraction and scattering on the same sample, we show that tissue, fibrils, and mineral particles take up successively lower levels of strain, in a ratio of 12:5:2. The maximum strain seen in mineral nanoparticles (approximately 0.15-0.20%) can reach up to twice the fracture strain calculated for bulk apatite. The results are consistent with a staggered model of load transfer in bone matrix, exemplifying the hierarchical nature of bone deformation. We believe this process results in a mechanism of fibril-matrix decoupling for protecting the brittle mineral phase in bone, while effectively redistributing the strain energy within the bone tissue.

Wet Powder Processing of Sol–Gel Derived Mesoporous Silica-Hydroxyapatite Hybrid Powders

This paper describes a method by which a porous silica coating layer can be obtained on different apatite particles through a simple sol-gel synthesis route. Sol-gel derived powders of hydroxyapatite (HAP) and beta tricalciumphosphate (beta-TCP) were coated with a mesoporous silica using C16TAB (hexadecyltrimethylammonium bromide) as a template in order to induce mesophase formation. Further calcination of the material removes the template from the mesophase and leaves a highly ordered hexagonal arranged mesoporous silica structure with a core of HAP/beta-TCP. The phase purity of the SiO2/apatite composites has been thoroughly investigated by the means of FT-IR, XRD, and solid state 31P MAS NMR. The phase purity of these materials is shown to be dependent on the solubility properties of the used apatites. The hybrid materials are suitable as a multifunctional biomaterial where osteoconductive properties can be combined with drug delivery.

γ‐Radiation‐induced changes in structure and properties of tetracalcium phosphate and its derived calcium phosphate cement

The purpose of the present study was to investigate the gamma-radiation effect on the structure and properties of the single-phase tetracalcium phosphate (TTCP) powder and its derived calcium phosphate cement (CPC). Experimental results show that low-dosed (0-30 kGy) CPC has a setting time of 10-12 min, while high-dosed (40-120 kGy) CPC has a setting time of 8-10 min. The low dose gamma-radiation does not significantly change porosity volume fraction or compressive strength of the CPC. The pH values of all CPC samples fell in a relatively narrow band, with a band width of 8.5-9.1 (in terms of pH value). With a dose of 10 or 20 kGy gamma-radiation, the TTCP-apatite conversion ratio does not change much. With 30 kGy the conversion ratio significantly increases and reaches a maximum value. With further increases in dose, the conversion ratio quickly declines. With increasing gamma-ray dose, the CPC morphology becomes more porous/loose and apatite particles become larger in size. When exposed to a high dose (120 kGy) of gamma-radiation, TTCP structure is radiation-damaged, and gamma-ray-induced formation of apatite is confirmed by transmission electron microscopic/selected-area diffraction/lattice imaging analyses.

Biocompatibility of CaSiO&lt;sub&gt;3&lt;/sub&gt; /High-Density Polyethylene Composites Prepared by Hot-Pressing

We have reported that CaSiO3 ceramics show very fast bone-like apatite formation in simulated body fluid (SBF). However, CaSiO3 ceramics have disadvantages in their mechanical properties and shapability. It is therefore more effective to develop composites of CaSiO3 particles dispersed in a matrix of polymer or metal. Such composites are usually prepared by homogeneously blending the ceramic powder with the matrix component. This method is, however, ineffective for the preparation of biocompatible polymers or metals because only the surfaces containing accidentally-exposed ceramic particles play a role in generating apatite in SBF. It is therefore necessary to add a large volume of ceramic powder and also to abrade the surface to expose more of the ceramic particles. In this study, CaSiO3/high-density polyethylene (HDPE) composites were prepared by hot-pressing to introduce surface CaSiO3 particles and their biocompatibilities were evaluated under in vitro conditions using SBF. CaSiO3 powders were spread on a HDPE plate and hot-pressed at 140oC and 4.9-14.7 MPa for 2 min. The composite sample (about 10×10×1 mm3 in size) was immersed in 30ml SBF (sample/solution ratio of 2.5 g/l) at 36.5oC. After 14 days soaking, the apatite product particles covered most of the composite surface and formed apatite layers. Bone-like apatite particles were formed only on the surface regions containing exposed CaSiO3 particles but no apatite was formed on the CaSiO3 particles buried in the HDPE matrix. The results show that this surface deposition method is very effective in developing biocompatibility in the composites using very small amounts of CaSiO3 powder (about &lt;1 %v) compared with results reported for hydroxyapatite and AW glass-ceramic powders (requiring about 40 %v). It is also found that the inhomogeneous state of the CaSiO3 particles in the surface of the present composites strongly influences their biocompatibility. It will be necessary to improve the homogeneity of CaSiO3 dispersion in the surface of the composites to achieve a more uniform surface apatite layer.

Nanocrystalline bioactive apatite coatings

A study of carbonatehydroxyapatite coatings deposited by a sol–gel technique from different precursor-sols containing different water/ethanol content is performed. All the sols form uniform and homogeneous coatings with good adhesive strength values. The composition of sols determine both the aging time necessary to deposit monophasic apatite coatings as well as the time interval to deposit said coatings. The thickness, porosity and roughness of the coatings are also modified as a function of the precursor-sol. After the immersion into an acellular simulated body fluid solution, the coatings appeared to be constituted by two types of particles: nanoparticles smaller than 25 nm with a Ca/P molar ratio of 1.7, corresponding to the apatite sol–gel coating, and an other type of apatite particles with needle shape and Ca/P molar ratio of 1.4, corresponding to the mineralization process of the coatings. The results obtained indicate that a compromise among the aging time, coating roughness, porosity and thickness must be reached by using these precursor-sol for a technological development of the sol-gel technique.

Influência do estado de agregação da polpa na flotação de quartzo, apatita e calcita

Muitos estudos acadêmicos foram realizados nos Estados Unidos, durante as décadas de 30 e 40, motivados pela correlação entre o estado de agregação da polpa e a recuperação do processo de flotação, observada no dia-a-dia das usinas. O objetivo desse trabalho é contribuir para uma maior compreensão do fenômeno observado na prática, dentro da realidade brasileira. Ensaios de microflotação e grau de dispersão foram realizados com partículas de quartzo, apatita e calcita. Os resultados reforçam a afirmativa postulada por Taggart e colaboradores de que a agregação ocorre como efeito da ação de reagentes e não como a causa de uma boa flotabilidade.