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PubMed1998

Fracture toughness of hydroxyapatite/mica composite, packed hydroxyapatite, alumina ceramics, silicon nitride and -carbide.

By using the fracture toughness estimation method based on two-dimensional map, it was found that the ductility of the high porosity hydroxyapatite/mice composite was comparable with silicon carbide. It was measured to be higher than that of packed hydroxyapatite. Alumina ceramics with more than 96% aluminium oxide showed a higher fracture toughness than the composite material. When bending strength was compared, the strength of the composite was two or three times lower than that of packed hydroxyapatite and much lower than the other studied materials. The composite material showed high porosity, which in turn gives it a lower bending strength. However, the high porosity is more favourable for biocompatibility.

Aluminum↗
PubMed1997

In vitro characterization of a zinc based bioceramic.

Six different blends of zinc calcium phosphorous oxide ceramics (ZCAP) were prepared by mixing and calcining powders (ZnO:CaO:P2O5) of weight percent ratio: 50:30:20, 48:32:20, 44:20:26, 40:40:20, 30:40:30, and 30:30:40. ZCAP is a resorbable bioceramic and has been used to repair bone defects and deliver drugs in a continuous manner. The chemical composition, porosity, and elements released on exposure to buffered Tris HCl were measured for each blend of ZCAP. The products of mixing and thermal reaction were beta-Ca3(PO4)2, alpha-CaZn2(PO4)2, and 2CaO.P2O5. Free calcium and/or zinc oxide was present in several blends. The components of ZCAP and their volume percentages influenced the interconnected porosity of ZCAP bioceramics. The interconnected porosity for all blends of ZCAP ranged from 35 to 38%. Pore sizes from these six blends of ZCAP ranged from less 1 micron to greater than 100 microns. Results of the 12 hour dissolution study showed that more calcium was released than zinc or phosphorous from all blends of ZCAP. Zinc was released in trace amounts from all blends of ZCAP. Release of phosphorous from the different blends of ZCAP was not detected by the procedures used to detect phosphorous in this investigation. These blends of ZCAP have the potential to be used as bone substitutes and probably long term treatment of zinc deficiency in humans.

Biocompatible Materials↗
PubMedDate not supplied

In vivo performance of a modified CSTi dental implant coating.

Cylindrical dental implants coated with cancellous structured titanium (CSTi) were studied in a dog model. CSTi-2-coated and hydroxyapatite-coated (HA) implants were placed in 8 mongrel dogs. The porosity of the CSTi-2 coating was 9% less than that of the previously studied CSTi-1, resulting in greatly improved mechanical strength and cosmetic appearance. A slightly lower level of bone ingrowth was observed for CSTi-2 than for CSTi-1. However, the in vivo attachment strength of the CSTi-2 coating was comparable both to CSTi-1 and to an HA-coated control after 8 weeks. Measured porosity is technique dependent; digital analysis of in vitro samples yielded higher porosity values than in vivo histology cross sections.

Animals↗
PubMed1999

Age-related hypermineralization in the female proximal human femur.

Hip fracture incidence increases exponentially with age in virtually every human population that has been studied. In spite of this, relatively few studies have examined age-related changes in the metaphyseal cortex of the proximal femur. The present study investigates cortical aging changes in the female proximal femur, with particular reference to regions of hypermineralization. Thirty-three femora from Caucasian females were obtained at autopsy and analyzed using backscattered electron imaging. Variations in hypermineralized tissue area, cortical bone area, and porosity were quantified with standard stereological methods. Cortical width was quantified with digital calipers. Gender differences were examined by statistical comparison with previously published results. Hypermineralized tissue volume was significantly (P < 0.001) greater in elderly individuals. Hypermineralized tissue preferentially appeared near ligamentous or tendinous insertion sites, suggesting the hypermineralized tissue may be a calcified fibrocartilage. Cortical width significantly (P < 0.001) decreased with age and porosity significantly (P < 0.001) increased with age, however the changes were site-specific. The femoral neck and intertrochanteric cortices had a smaller change in cortical width and porosity with age than the diaphysis, but the femoral neck and intertrochanteric cortices had a larger increase in hypermineralized tissue. Comparison with previous data suggests that cortical aging in the proximal femur is similar between males and females and is unlikely to explain the higher incidence of fracture in females. However, the data strongly indicates that age-related changes in the femoral diaphysis cannot be directly extrapolated to either the femoral neck or intertrochanteric cortices.

Adolescent↗
PubMed1999

Bone turnover associated with antler growth in red deer (Cervus elaphus).

Although it is known that skeletal bone depletion occurs during antler growth in deer, it is not clear whether repletion of the skeleton takes place before or after completion of antler development. This study attempted to correlate repeated scanning electron microscopic measures of ilium and rib bone porosity from six approximately 2-monthly biopsy samples (using back-scattered imaging) and biochemical markers of bone turnover (serum hydroxyproline and osteocalcin concentrations) taken for 11 months with antler growth in six red deer stags. No changes were detected in ilium samples but changes in porosity of rib bones and an elevation of the biochemical markers indicated that skeletal depletion occurred during the antler growth period. However, the decrease in rib bone porosity and decline in markers of bone turnover took place before completion of antler growth, indicating that a considerable amount of skeletal repletion could have occurred whilst antlers were also undergoing bone accretion. This latter finding extends the current view of antler growth being accompanied by a form of reversible osteoporosis in the skeleton by showing that there is a period when the antlers and skeleton are both undergoing net bone formation.

Animals↗
PubMed1998

Release of bioactive human growth hormone from a biodegradable material: poly(epsilon-caprolactone).

We have characterized the biodegradable material poly(epsilon-caprolactone) (PCL) as a delivery system for recombinant human growth hormone (hGH). Two contrasting methods for the manufacture of the biomaterial were investigated: namely, solvent casting and solvent casting particulate leaching; the latter yielded porous PCL discs. The degree of porosity, which was assessed by scanning electron microscopy, could be controlled by incorporating selected concentrations of particulate sodium chloride during the manufacturing process. Bioactive hGH released from the PCL preparations was quantified with a highly sensitive and precise bioassay which was based upon hGH activation of rat lymphoma Nb2 cells. Eluates obtained from control discs of PCL which had not been loaded with hGH proved to be nontoxic when tested on these cells. The release of bioactive hGH from hormone-loaded nonporous discs of PCL was found to be a direct function of the initial hormone loading dose. Increased porosity of the discs manufactured by solvent casting particulate leaching increased the delivery of hGH from discs which had been immersion loaded. However, hGH release after surface loading was independent of porosity. Hormone concentrations were also assessed by immunoassay so that the ratios of bio- to immunoactivity (B:I ratio) of the hormone release could be determined. We found that the B:I ratio of the hormone after release from unstored discs was identical to that of the hormone prior to its incorporation into the PCL, demonstrating that the mild incorporation procedures utilized had not adversely affected the structural integrity of the hormone. However, if the hormone-loaded discs were stored at 37 degrees C prior to elution, the B:I ratios of the hGH released decreased indicating that this compromised the bioactive site.

Animals↗
PubMed1999

Glass-reinforced hydroxyapatite composites: secondary phase proportions and densification effects on biaxial bending strength.

CaO-P(2)O(5) glasses with additions of MgO and CaF(2) were used as a sintering aid of hydroxyapatite, and glass-reinforced hydroxyapatite composites obtained. Glasses promoted significant changes in the microstructure of the composites, namely with the formation of tricalcium phosphate secondary phases, beta and alpha-TCP. Quantitative phase analysis was performed by the Rietveld method using General Structure Analysis Software. Grain size measurements were carried out on SEM photomicrographs, using a planimetric procedure according to ASTM E 112-88. Flexural bending strength was determined from concentric ring-on-ring testing. Flexural bending strength (FBS) of glass-reinforced hydroxyapatite composites was found to be about twice or three times higher than that of unreinforced hydroxyapatite and tended to depend more on porosity and beta and alpha-TCP secondary phases, rather than on grain size. Traces of alpha-tricalcium phosphate significantly enhanced the strength of the composites. Using the rule of mixtures to estimate the zero porosity bending strength, the Duckworth-Knudsen model applied to the composites gave a porosity correction factor, b, with a value of 4.02. Weibull statistics were also used to analyze biaxial strength data and the level of reinforcement obtained by comparing failure probability for the composites and for the unreinforced hydroxyapatite. Lower activation energies for grain growth were observed for the composites compared to unreinforced hydroxyapatite, which should be attributed to the presence of a liquid glassy phase that promotes atomic diffusion during the sintering process.

Biocompatible Materials↗
PubMed2000

Osseointegration of composite calcium phosphate bioceramics.

The resistance of macroporous calcium phosphate ceramics to compressive strength generally is low and depends on, among other factors, porosity percentage and pore size. A compromise always is adopted between high porosity, required for a good integration, and mechanical strength, which increases with material density. We improved the strength of macroporous calcium phosphate ceramics of interconnected porosity by filling the pores with a highly soluble, self-setting calcium phosphate cement made of TCP and DCPD. Cylinders of the resulting material were implanted in sheep condyles and subjected to histological analysis after 20, 60, and 120 days. Microradiographs were made of the histological sections. The control material consisted of ceramic that had not been loaded with cement. Progressive ingrowth of bone into the ceramic pores occurred as the cement was degraded during the first implantation period. Marked degradation of the cement was apparent after 2 months, with fragmentation of the cement in most of the pores and the presence of bone tissue between the fragments. All the cement had been replaced by bone after 4 months. Some fragments of cement still were embedded in the newly formed bone. There was no significant difference between the integration of loaded and nonloaded ceramics. Filling the macroporous ceramic pores with a calcium phosphate cement significantly improved the mechanical strength of these ceramics without modifying their integration in the healing bone.

Animals↗
PubMed2000

Spherical crystal agglomeration of ibuprofen by the solvent-change technique in presence of methacrylic polymers.

The effects of Eudragit(R) nature on the formation and spherical agglomeration of ibuprofen microcrystals have been examined when solvent change (ethanol-water) technique is applied. Four methacrylic polymers (Eudragit(R) S100, L100, RS, and RL), with different solubility and solubilizing ability, were used. The extrapolated points of maximum temperature deviation rate in crystallization liquid that reflect the maximum crystallization rate and the corresponding water addition were determined, as well as crystal yielding and incorporation of drug and polymer in the agglomerates. The physicomechanical properties of the agglomerates, such as size, sphericity, surface roughness and porosity, as well as flow and packing or compression behavior during tableting, were evaluated for different drug/polymer ratios. It was found that crystal yield is greatly reduced in the presence of water-insoluble polymers and that formation of the microcrystals and incorporation of drug and polymer are affected by the polymer nature. Crystal formation changes are attributed to alterations in the metastable zone, whereas the changes in drug and polymer incorporation and crystal yield are caused by changes in the polymers' solubility and micellization. The size of agglomerates depends on the polymer nature and its interactions with the ibuprofen microcrystals formed. Sphericity, surface roughness, and intraparticle porosity of agglomerates increase, in general, with the presence of polymer owing to changes in habit and growth rate of the microcrystals and to their coating before binding into spherical agglomerates. The particle density or intraparticle porosity and size changes determine flow or packing behavior and densification of agglomerates at low compression. The incorporation and brittleness of the polymer determine the deformation under higher compression pressure, expressed as yield pressure, Py.

Acrylic Resins↗
PubMed2001

Fabrication of porous calcium polyphosphate implants by solid freeform fabrication: a study of processing parameters and in vitro degradation characteristics.

Solid freeform fabrication (SFF) involves the creation of a solid 3-D object of desired shape by successively adding raw materials in particles or layers. Its use in fabricating surgical implants is being explored. The objective of this study was to determine the feasibility of using SFF to build porous parts of calcium polyphosphate (CPP), a linear condensed phosphate that has been suggested as a material for forming bioresorbable skeletal replacement implants. CPP powders (<25 microm in particle size) were added to an UV curable monomer (SOMOS 6110) at a solids loading of 25 vol %, with the addition of a commercial dispersant to prevent particle agglomeration and settling. Viscosity and cure depth measurements were performed to insure that CPP suspension met the requirements deemed necessary for use in SFF. The CPP suspension was bulk cured and sintered in molds in order to assess binder removal and sintering parameters. Using a three-point bend test, the ultimate bending strength and energy-to-fracture of sintered CPP samples simulating parts to be formed by this strategy were characterized. In vitro degradation studies using 0.1M of tris-buffered solution were performed to assess the effect of aging on mechanical properties of the samples as a function of the processing route and resulting structures. The polymer binder successfully was removed from the cured ceramic suspension by developing a procedure that combined slow heating rates with low temperature dwells. Sintering CPP at 585 degrees C for 1 h produced amorphous material samples with average porosity of 27.7 +/- 2.0%. Sintering CPP at 600 degrees C for 1 h produced a crystalline material with samples having an average porosity of 22.9 +/- 1.3%. Crystalline CPP was found to exhibit superior bend strength and toughness compared with amorphous CPP. Both samples experienced a decline in mechanical properties during in vitro degradation; however, the effects were more pronounced with the amorphous CPP samples. Amorphous CPP was found to degrade four times faster than crystalline CPP, as shown by high levels of phosphate present in the degradation solution and a noticeable increase in the porosity of the samples. Crystalline CPP was more resistant to attack as dissolution was limited to surface features of the sintered particles.

Biocompatible Materials↗
PubMed2003

Towards on-line monitoring of cell growth in microporous scaffolds: Utilization and interpretation of complex permittivity measurements.

Here we demonstrate the ability to characterize microporous scaffolds and evaluate cell concentration variation via the utilization and interpretation of complex permittivity measurements (CP), a direct and nondestructive method. Polymer-based microporous scaffolds are of importance to tissue engineering, particularly in the promotion of cell adhesion, proliferation, and differentiation in predefined shapes. Chitosan gel scaffolds were seeded with increasing concentrations of macrophages to simulate cell growth. Complex permittivity measurements were performed using a dielectric probe and a vector network analyzer over a frequency ranging from 200 MHz to 2 GHz. An effective medium theory was applied to interpret the data obtained; respectively, Looyenga and Maxwell-Wagner-Hanai functions were used to retrieve the porosity and the variation of the cell concentration from the CP measurements. Calculated porosities were in agreement with experimental evaluation-porosity ranged from 81-96%. Changes in cell concentration inside the scaffolds upon injection of differing cell concentrations into the scaffold were detected distinguishably. Variations resulting from the cumulative injection of 400-1800 microL of 10(6) cells/mL solution into the scaffold were monitored. Results suggest that CP measurements in combination with an appropriate effective medium approximation can enable on-line monitoring of cell growth within scaffolds.

Algorithms↗
PubMed1995

Comparison of diametral shrinkage of centrifuged and uncentrifuged Simplex P bone cement.

Reducing the porosity of bone cement substantially strengthens the cement in fatigue. However, concern has been raised that reducing the porosity of the cement would increase the shrinkage of the cement and thus compromise the cement-bone interface. We measured diametral shrinkage of cement mantles prepared with and without centrifugation of the cement. Four cement preparations (centrifuged and uncentrifuged mixed with monomer at either room temperature or 0 degrees C) were used to form cement mantles of four different thicknesses (2, 4, 6, and 8 mm) around a stainless steel rod. We conclude that porosity reduction dramatically increases the fatigue strength of bone cement without substantially changing the diametral dimensions of the polymerized cement when studied in the shape and volume of a cement mantle that would be used for total hip replacement.

Biocompatible Materials↗
PubMed1987

A rapid in vitro test of the in vivo healing potential of vascular prostheses.

An in vitro method for comparing the penetration of bovine fibroblasts seeded on the external surface of porous vascular prostheses was devised. The effects of water porosity reduction and differing manufacturing constructions (warp-knit Dacron, woven Dacron and polytetrafluoroethylene) on the ability of the bovine fibroblasts to penetrate transmurally was investigated. Of the warp-knit external-veloured Dacron prostheses, the highest porosity 140-denier prototype had the highest luminal surface cell count and the lowest porosty 280-denier prototype the lowest luminal surface cell count. The intermediate prototypes had values between these two extremes. The woven Dacron prostheses, which were of even lower porosity but with a much thinner wall, had cell counts midway between the 140-denier and the 280-denier prototypes. The microporous polytetrafluoroethylene prostheses did not allow fibroblast penetration despite adherence of cells to the outer surface. These findings agree with in vivo healing studies of the same materials in the descending thoracic aorta of the dog, demonstrating that this rapid in vitro assay method can help predict the healing potential of a vascular prosthesis.

Animals↗
PubMed1988

Fabrication and characterization of small-diameter vascular prostheses.

We have developed a process to fabricate polyurethane vascular grafts of various dimensions and porosities in our laboratory. A primary feature of the presented fabrication technique is the ability to control surface porosity and roughness, and bulk mechanical properties. The method is based on the spray application of a fine mixture of polymer solution and nitrogen gas bubbles onto a lathe-mounted mandrel. The technique was successfully tested with Tecoflex, a linear segmented aliphatic polyurethane. Other urethane polymers can be used as well. Several polymer coats are applied in a semiautomated process, at the end of which the polymer coating is dried and the tube is slipped off the mandrel. It is the purpose of this paper to describe the fabrication process and present results of the evaluation of grafts. Wall structure was evaluated using scanning electron microscopy and compliance was measured in a specially designed testing apparatus. We developed methods to quantify kink resistance and suture retention capacity of the grafts. These characteristics were correlated with graft fabrication variables: mandrel rpm, horizontal speed of the spray nozzle, gas and polymer solution flow rates. We were able to routinely produce 3-6-mm-ID grafts with 0.5-1.2-mm wall thickness and average bulk pore sizes of 10-250 microns; the wall porosity could be varied between 30 and 70%. Compliance values of the grafts were comparable with corresponding values of carotid and femoral arteries of dogs.

Biocompatible Materials↗
PubMed1990

Effect of vacuum mixing on the mechanical properties of antibiotic-impregnated polymethylmethacrylate bone cement.

Polymethylmethacrylate bone cement, containing either no added antibiotic, 0.5 g of Vancomycin, 1.0 g of Vancomycin, or 1.0 g of Tobramycin, was mixed either in air or a vacuum chamber. Following storage in a water bath at 37 degrees C for 48 h, the specimens were tested in four-point bending. The porosity of the specimens was assessed radiographically, and their antibacterial activity was monitored for 21 days. The bending strength of the vacuum mixed specimens containing no antibiotic was 40% greater than that of similar air-mixed specimens. However, there were no significant differences in the bending strength of either the air- or vacuum-mixed specimens when any of the antibiotic dosages were added. The bending modulus of the vacuum-mixed specimens, containing no antibiotic, was significantly greater than the moduli of all the other specimen groups which did not differ from each other. Vacuum mixing reduced the apparent porosity of the specimens fivefold, and while the addition of antibiotic did not effect porosity of the air-mixed specimens, that of the vacuum-mixed specimens was doubled. Although initial rapid decreases were seen, leaching of antibiotic from the cement and antibacterial activity continued through the 21-day monitoring period.

Biomechanical Phenomena↗
PubMed2003

Performance of degradable composite bone repair products made via three-dimensional fabrication techniques.

This study analyzed the in vivo performance of composite degradable bone repair products fabricated using the TheriForm process, a solid freeform fabrication (SFF) technique, in a rabbit calvarial defect model at 8 weeks. Scaffolds were composed of polylactic-co-glycolic acid (PLGA) polymer with 20% w/w beta-tricalcium phosphate (beta-TCP) ceramic with engineered macroscopic channels, a controlled porosity gradient, and a controlled pore size for promotion of new bone ingrowth. Scaffolds with engineered macroscopic channels and a porosity gradient had higher percentages of new bone area compared to scaffolds without engineered channels. These scaffolds also had higher percentages of new bone area compared to unfilled control defects, suggesting that scaffold material and design combinations could be tailored to facilitate filling of bony defects. This proof-of-concept study demonstrated that channel size, porosity, and pore size can be controlled and used to influence new bone formation and calvarial defect healing.

Animals↗
PubMed2005

Antibody response to collagen after functional implantation of different polyester vascular prostheses in pigs.

Besides inflammation, specific immune responses are seen also after implantation of biomaterials. The aim was to investigate the humoral response to bovine collagen type I following implantation of various polyester (Dacron) prostheses into pigs. In 24 randomized pigs, the infrarenal aorta was replaced with a segment of collagen-impregnated, woven polyester prosthesis of low, medium, or high porosity. IgG antibodies were detected by immunoassay using native and denatured collagen type I as a target for blood samples taken on day 1 (implantation), 10, 17, 24, 62, and 116. As generally observed, antibodies to native and denatured collagen are of low titer and were significantly correlated with enhanced binding to the denatured form (p < 0.001). The highest overall antibody prevalence to native and denatured collagen was obtained on day 116 with 68% and on day 62 with 59%, respectively. Prostheses with high porosity induced an early immune response on day 10; those with low and medium porosity induced the highest antibody levels later after 2 months. Collagen antibodies neither correlated with serum IgG contents nor with antibodies to the prosthesis polyester matrix. Thus, humoral immune response against implant components may provide a further parameter in describing biocompatibility but also a potential marker that may facilitate monitoring of individual perigraft reaction.

Animals↗
PubMed2006

Dynamic mechanical properties of 3D fiber-deposited PEOT/PBT scaffolds: an experimental and numerical analysis.

Mechanical properties of three-dimensional (3D) scaffolds can be appropriately modulated through novel fabrication techniques like 3D fiber deposition (3DF), by varying scaffold's pore size and shape. Dynamic stiffness, in particular, can be considered as an important property to optimize the scaffold structure for its ultimate in vivo application to regenerate a natural tissue. Experimental data from dynamic mechanical analysis (DMA) reveal a dependence of the dynamic stiffness of the scaffold on the intrinsic mechanical and physicochemical properties of the material used, and on the overall porosity and architecture of the construct. The aim of this study was to assess the relationship between the aforementioned parameters, through a mathematical model, which was derived from the experimental mechanical data. As an example of how mechanical properties can be tailored to match the natural tissue to be replaced, articular bovine cartilage and porcine knee meniscus cartilage dynamic stiffness were measured and related to the modeled 3DF scaffolds dynamic stiffness. The dynamic stiffness of 3DF scaffolds from poly(ethylene oxide terephthalate)-poly(butylene terephthalate) (PEOT/PBT) copolymers was measured with DMA. With increasing porosity, the dynamic stiffness was found to decrease in an exponential manner. The influence of the scaffold architecture (or pore shape) and of the molecular network properties of the copolymers was expressed as a scaffold characteristic coefficient alpha, which modulates the porosity effect. This model was validated through an FEA numerical simulation performed on the structures that were experimentally tested. The relative deviation between the experimental and the finite element model was less than 15% for all of the constructs with a dynamic stiffness higher than 1 MPa. Therefore, we conclude that the mathematical model introduced can be used to predict the dynamic stiffness of a porous PEOT/PBT scaffold, and to choose the biomechanically optimal structure for tissue engineering applications.

Animals↗