Search

Nano-hydroxyapatite (nano-HA) coating has been proved to be effective to modify the titanium surface for better bone formation. A simple and economical nano-HA coating method that filling the nano-HA particles into the porous titanium substrate by using vacuum suction was introduced in this study. Two kinds of nano-HA modified titanium surfaces, nano-HA filled type (nHA-f) and nano-HA coated type (nHA-c), were prepared by a 2-step and 3-step protocol, respectively. Nano-HA modified titanium surfaces with and without thermal treatment were compared. The physicochemical properties including morphology, elemental composition, coating thickness, adhesion strength and in vitro mineralization ability were characterized. The SEM results showed that nano-HA particles were effectively filled into the porous titanium substrate under the function of vacuum suction in the nHA-f and nHA-f-heat groups. The thickness of the nano-HA layer was about 1 μm and 7-8 μm in the nano-HA filled type and nano-HA coating type, respectively. Localized separation between the nano-HA layer and the titanium substrate was observed in the thermal-treated groups, which may increase the risks of detachment. In the in vitro mineralization test, the unheated groups (nHA-f and nHA-c) showed promoted calcium phosphate compounds deposition than the heated groups (nHA-f-heated and nHA-c-heated) because of the active biological behavior of the amorphous nano-HA; the nHA-f group with a thin nano-HA layer showed no difference to the thick coating group (nHA-c) at the early stage, which was due to the effect of the porous structure as a cage to protect the nano-HA particles from fast dissolution. In conclusion, the vacuum spray method is effective to create a thin amorphous nano-HA layer with improved adhesion strength and sustained-release ability to induce mineralization by filling the nano-HA particles into the porous titanium substrate without thermal treatment., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2020 Elsevier B.V. All rights reserved.)

Hydroxyapatite (HA) thin films were coated on a polyetheretherketone (PEEK) substrate using a sputtering technique. A thin titanium (Ti) intermediate layer was formed between the HA and the PEEK surface to improve adhesion of the HA film to the PEEK substrate. The coated films were recrystallized using a hydrothermal treatment to reduce the dissolution of the HA film. The films were then characterized by X-ray diffractometry (XRD), scanning electron microscopy (SEM), and a UV-Vis spectrophotometer. A pull-out test was performed to measure the film-to-substrate adhesion strength, and an immersion test was performed in ultra-pure water. In the XRD patterns of the sputtered film with the Ti intermediate layer on the PEEK substrate, small HA peaks and large Ti peaks were observed. After the hydrothermal treatment, the intensity of the HA peaks increased. The transmittance of the HA films with 5 and 10nm Ti intermediate layers was >79% and 68%, respectively, in the visible light wavelength region (400-700nm) after the hydrothermal treatment. The adhesion strength of the hydrothermally treated HA films increased with decreasing thickness of the Ti intermediate layer, and the strength reached 2.7MPa with the 5-nm-thick Ti intermediate layer. In the immersion test, the HA film with a 5-nm-thick Ti intermediate layer without hydrothermal treatment exhibited a released Ti concentration of 42.0±2.4ppb. After hydrothermal treatment, the released Ti concentration decreased to 17.3±1.1ppb., (Copyright © 2016 Elsevier B.V. All rights reserved.)

Removal of radioactive substances, such as cesium (Cs) and strontium (Sr), has become an emerging issue after the Fukushima Daiichi Nuclear Power Plant Disaster. To assess the possibility that hydroxyapatite (HA) and zeolites can be used for removal of radioactive substances, the adsorption capacities of Cs and Sr on the HA and a zeolite were investigated. The influence of Fe ions on Cs and Sr adsorption on the HA and the zeolite was also evaluated, because Fe ions are the most effective inhibitor of Cs adsorption on the zeolite.In the Cs adsorption process on the HA and the zeolite, the zeolite showed a higher adsorption ratio than the HA, and the maximum sorption capacity of the zeolite was calculated as 196 mg/g, whereas the HA showed a higher Sr adsorption ratio than the zeolite. The maximum sorption capacity of Sr on the HA was 123 mg/g. Under coexistence with Fe, Cs adsorption on the zeolite decreased with increasing Fe concentration, reaching 2.0 ± 0.8% at 0.1 M Fe concentration. In contrast, Cs adsorption on the zeolite was improved by adding the HA. In the case of coexistence of the HA, the Cs adsorption on the mixture of the HA and the zeolite was 52.4% ± 3.6 % at 0.1 M Fe concentration, although Cs adsorption on the HA alone was quite low. In the Fe adsorption processes of the HA and the zeolite, the HA exhibited a maximum sorption capacity of 256 mg/g, which was much higher than that of the zeolite (111 mg/g). The high affinity of Fe on the HA contributes to the improvement of the deteriorated Cs adsorption on the zeolite due to Fe ions.

Hydroxyapatite (HA) was coated onto titanium substrates using radio frequency sputtering, and the sputtered films were crystallized using a hydrothermal treatment at 120°C and 170°C to evaluate the influence of the crystallinity of the HA film on its osteocompatibility. The crystallite size and surface morphology of the films were observed using X-ray diffraction (XRD) and scanning electron microscopy (SEM), respectively. The alkaline phosphatase (ALP) expression, osteocalin (OCN) expression and bone formation of osteoblast cells on the films were measured to evaluate the osteocompatibility of the film.The crystallite size increased as the hydrothermal temperature increased, and the crystallite sizes of the film treated at 120°C and 170°C were 82.2±12.3 nm and 124.7±13.3 nm, respectively. Globular particles were observed in the hydrothermally treated film using SEM. The size of the particles on the film increased as the hydrothermal temperature increased, and the width of the particles on the film treated at 120°C and 170°C were approximately 120-190 nm and 300-500 nm, respectively. In the osteoblast cell culture experiments, the ALP expression, OCN expression and bone formation area on the films treated at 120°C were higher than those treated for films treated at 170°C.

Hydroxyapatite (HA) thin films were prepared on a zirconia (ZrO2) substrate using a sputtering technique, and the film was also coated on a titanium (Ti) substrate for comparison. The coated films were recrystallised using a hydrothermal treatment to reduce film dissolution. The films were then characterised by X-ray diffractometry (XRD) and scanning electron microscopy (SEM). The osteocompatiblity of the films was evaluated by investigating the alkaline phosphatase (ALP) activity and the size of the bone formation area of osteoblast cells. In the XRD patterns of the as-sputtered films on the ZrO2 substrate, there are no peaks except for those from the ZrO2 substrate. After the hydrothermal treatment, HA peaks appeared in the patterns. Nanoparticles (less than 20 nm) were observed on the ZrO2 substrates in the SEM images of the as-sputtered films. After the hydrothermal treatment, particles of 20-40 nm were observed on the film, whereas the HA film on the Ti substrate was covered by a larger number of globular particles (20-60 nm). In the osteoblast cell cultures, the ALP activity and bone formation area on the HA films on both the ZrO2 and Ti substrates increased after the hydrothermal treatment of the films, and the values for the ZrO2 substrate were higher than those for the Ti substrate.

Sr-substituted hydroxyapatite thin films were prepared by sputtering technique from mixture targets of hydroxyapatite (HA) and strontium apatite (SrAp). The HA and SrAp powders were mixed at 0-100% Sr/(Sr+Ca) target ratios. The coated films were recrystallized by a hydrothermal treatment to reduce film dissolution. The films were then characterized by X-ray diffractometry (XRD), scanning electron microscopy (SEM) and inductively coupled plasma atomic emission spectrometry (ICP). The osteocompatiblity of the films was also evaluated by the size of the bone formation area in osteoblast cells.In the XRD patterns, peaks shifted to lower 2θ values with increasing Sr/(Sr+Ca) target ratios, which indicated Sr incorporation into the HA lattice. In the SEM observation of the hydrothermally treated films, the surface was covered with globular particles, and the size of the globular particles increased from Sr0 to Sr40, and then the size decreased from Sr60 to Sr100. The ICP analysis showed that the Sr/(Sr+Ca) film ratios were almost the same as the target ratios. In the cell culture, the bone formation area on the Sr-substituted HA films increased with increasing Sr concentration, and saturated at Sr60.

The adsorption behavior of albumin (BSA) and lysozyme (LSZ) on rod-shaped and plate-shaped hydroxyapatite (HA) was investigated to evaluate the influence of crystal orientation and morphology on the selective protein adsorption of HA. The rod-shaped HA was prepared by hydrothermal treatment from β-tricalcium phosphate (β-TCP) in H3PO4 solution (pH 2.0 and 4.0 for HA-pH 2.0 and HA-pH 4.0). The plate-shaped HA was synthesized by hydrolysis of CaHPO4-2H2O (DCPD) in NaOH solution at 40°C and 80°C (HA-40°C and HA-80°C). The synthesized HA was characterized using scanning electron microscopy (SEM) and X-ray diffractometry (XRD). HA-pH 2.0 and HA-pH 4.0 produced rod-shaped crystals that were highly oriented to the a-face plane, whereas HA-40°C and HA-80°C showed a plate-like shape and a c-face preferred orientation. The peak intensity ratio I(300)/I(002) (a/c intensity ratio) from the XRD patterns increased in the following order: HA-80°C, HA-40°C, HA-pH 2.0 and HA-pH 4.0. It also increased as the Ca/P ratio decreased. The amount of adsorbed BSA increased in the following order: HA-pH 4.0, HA-pH 2.0, HA-40°C and HA-80°C. The amount of adsorbed LSZ on HA increased in the following order--HA-pH 2.0, HA-pH 4.0, HA-40°C and HA-80°C--with a corresponding decrease in the a/c intensity ratio. The BSA/LSA adsorption ratio increased with the a/c intensity ratio in the range of 3.3-8.9, and the BSA and LSZ were selectively adsorbed on HA, depending on the crystal shape.

A sputtering technique followed by a low temperature hydrothermal treatment has been demonstrated to produce a dense-and-bioactive hydroxyapatite thin film coating. The purpose of the present study was to investigate osteoblast and osteoclast responses to the hydroxyapatite coated plates and titanium plates with similar roughness. Rat bone marrow stromal cells were cultured on these plates to induce osteoblasts. The cells showed a significantly enhanced proliferation on the hydroxyapatite surface, accompanied by increase of osteoblastic phenotypes. The co-cultured osteoclasts exhibited the significantly different cell number and morphology between the hydroxyapatite and the titanium surfaces. A series of osteoclast marker genes were more stimulated on the hydroxyapatite and thirty two percent of the hydroxyapatite surface area could be resorbed by osteoclasts. The thin film sputtered hydroxyapatite could provide a favorable surface for both osteoblast and osteoclast formation and their function, indicating its good osteoconductivity and biodegradability.

Hydroxyapatite (HA) was coated onto a titanium substrate using radio frequency magnetron sputtering. The sputtered film was crystallized using a hydrothermal treatment. The films were observed using X-ray diffractometry, field emission scanning electron microscopy (FE-SEM) and scanning transmission electron microscopy (STEM) equipped with energy dispersive X-ray spectroscopy (EDX).It was observed that the surface of the hydrothermally-treated film was covered with globular particles. The FE-SEM observations indicated that these particles were composed of columnar grains with a grain size of 20-50 nm. In the STEM cross-sectional observation of the HA-Ti interface, HA crystalline phase regions were observed, in part, in the non-crystalline phase layer of the as-sputtered film. After the hydrothermal treatment, the HA layer crystallized; the HA crystallization proceeded to a distance of 30 nm above the titanium surface. From an EDX line scan analysis, the titanium oxide layer was not observed at the HA-Ti interface of the as-sputtered film; however, in the hydrothermally-treated film, the titanium oxide layer, with a 15 nm thickness, was observed between the mixing layer and the titanium substrate. The formation of titanium oxide at the HA-Ti interface would contribute to the adhesion improvement of the sputtered film following the hydrothermal treatment.

This study describes the adsorptive property of vitamins on HA and the effect of the HA adsorbed vitamin on the alkaline phosphatase (ALP) activity for effective use as a bone graft substitute. The vitamins used were calciferol (D3), menaquirone (K2) and 25-hydroxycholecalciferol (25(OH)D3). These vitamins were adsorbed on HA at 4, 10, 20, 37 and 50 degrees C. The adsorption amount was constant below 20 degrees C, and decreased as the incubation temperature increased over 20 degrees C. The order of the adsorption amount was: 25(OH)D3 > K2 > D3. The HA adsorbed vitamins (HA/D3, HA/25(OH)D3 and HA/K2) were suspended in physiological saline for 48 h for the release test. The release ratio of all vitamins increased with incubation time. The order of the release ratio was: 25(OH)D3 > K2 > D3, which was proportional to that of the adsorption amount. The ALP activity of MC3T3-E1 osteoblast-like cells on HA, HA/D3, HA/25(OH)D3 and HA/K2 was also investigated. The ALP activity was higher on HA/25(OH)D3 than on any other samples. However, HA/K2 and HA/D3 showed similar ALP activity to HA.

The purpose of this study was to develop a new biodegradable bone substitute materials consisting of synthesized nano-size hydroxyapatite (nano-HAp) and Type I biodegradable honeycomb collagen sponge (HCS) composites. Bone defects in rabbit mandibles were prepared by a drill, and the composites were implanted into the bone defects. The HCS only and the HCS/calcined hydroxyapatite (HAp) composite were used as comparative materials. The bone tissues reaction at the early stage within 3 weeks after implantaion was investigated histologically. Amounts of new bone formation were determined by NIH-image analysis software using the histological sections. The amounts of the new bone formation were largest in the nano HAp/HCS compared to the comparative materials. Within 2 weeks after implantation, the nano-HAp/HCS composite was more rapidly exchanged by new bone than the comparative materials. From these results it was considered that the nano-HAp/HCS composites can be used as an effective biodegradable bone substitutive material.

Objective: To study the influence of a discrete nano-hydroxyapatite crystal (nano-HAp) on lymphatic leukemia P388 behavior by in vivo techniques., Methods: A nano-HAp was prepared by a neutralization reaction of 0.1 mol calcium hydroxide suspension and 0.06 mol phosphoric acid solutions at room temperature over pH7. The various doses of the nano-HAp only and the nano-HAp mixture with cyclophosphamide (CY) were injected into mice inoculated with solid tumor lymphatic leukemia P388 and dispersed into PRMI 1640 media harvested the leukemia P388 cells. Sixty P388 BALB/C mice were randomly grouped; 36 of them were used as nano-HAp treated groups and 24 mice as the control groups. The leukemia growth in the mice was examined morphologically, histopathologically and under a transmission electron microscope (TEM)., Results: The nano-HAp was identified as a hydroxyapatite by an X-ray diffractometry (XRD) and a Fourier transform infrared spectroscopy (FTIR). The morphology and sizes were observed under a TEM. The tissue growth inhibition ratio (weight%) of solid lymphatic leukemia P388 bearing mice treated with nano-HAp at doses 35 mg/kg, 53 mg/kg and nano-HAp (53 mg/kg) combined with CY (35 mg/kg) in 3 consecutive days via intraperitineal injections were 14.95%, 32.67% and 60.45% respectively. Apoptosis of P388 cell cocultured with nano-HAp was confirmed by TEM., Conclusions: The tissue growth restriction of solid tumor lymphatic leukemia P388 was greater after an injection of nano-HAp only or nano-HAp mixed with CY than that obtained after injection with physiological saline solution as a control (P < 0.01), and the tissue growth restriction of solid tumor after an injection of nano-HAp combined with CY was greater than that obtained after nano-HAp or CY injection only (P < 0.01).

Influence of a discrete nano-hydroxyapatite crystal (nano-HAp) on lymphatic leukemia P388 cell behavior was investigated by an in vitro technique using an MTT test and FITC analysis. The discrete nano-HAp was prepared by decanting upside clear layer of the nano-HAp suspension which was synthesized by a wet method using calcium hydroxide suspension and phosphoric acid solutions. The nano-HAp was identified as hydroxyapatite by the X-ray powder diffraction pattern and an infrared spectroscopy. The nano-HAp with concentrations of 8-40 microg/ml was dispersed into PRMI 1640 media with leukemia cells derived from BALB/C mice. The survival ratio of the cells decreased with the amounts of the nano-HAp increasing. Apoptosis rates of leukemia P388 cells on co-culturing with the nano-HAp of 35 microg/ml for 24, 48 h were 14.5% and 45.8%, respectively, and higher than those of 10.4% and 34% in controls. The G0/G1 peak values in leukemia P388 cell cycle were declined to reduce and the S peak values increased with extension time of co-culture. These results proved that the discrete nano-HAp can cause apoptosis of the leukemia P388 cells, and selectively act on G1 phase and arrest the G1 phase in cell cycle of the leukemia P388.

Hydroxyapatite (HA)/Hydrogen Peroxide (H(2)O(2)) solutions was prepared for a tooth whitening application. HA powder was immersed in the 100, 1000 and 10,000 ppm of the H(2)O(2) solutions. The HA/H(2)O(2), HA and H(2)O(2) solutions were applied to HA discs and extracted teeth for weight and whiteness change evaluation. After 24 hours, each HA disc was measured for the weight changes and each tooth was measured for the whitening changes (L(*)) using a Spectro Color Meter. The topology of the teeth surfaces were also observed using Scanning Electron Microscope (SEM). The weight of the HA disc applied with H(2)O(2) at all concentrations was lower than that applied with HA and HA/H(2)O(2) solutions. The whiteness of the teeth treated with HA/H(2)O(2) were higher than that treated with HA and H(2)O(2) only solutions. The whiteness change of the teeth treated with the HA/H(2)O(2) (10,000 ppm) showed the highest value in all solutions at L(*)=4.98+/-0.90 (p<0.05). In the SEM observation, the teeth surface treated with the H(2)O(2) showed rough and destructive holes on the enamel surface. However, the teeth surface treated with the HA/H(2)O(2) show smooth enamel surface due to covering of the destructive holes with HA powder.

Hydroxyapatite (HA) was coated onto titanium substrates using radio frequency sputtering. Some of the as-sputtered films were hydrothermally recrystallized at 110 degrees C. In immersion tests, the as-sputtered film completely dissolved after 2 days in a culture medium, whereas the thickness of hydrothermally treated films increased with an increase in immersion period, reaching a thickness of 127% after a period of 4 weeks. The proliferation and alkaline phosphatase (ALP) activity of MC3T3-E1 osteoblast-like cells on the as-sputtered and hydrothermally treated films were investigated, and the cell morphology was also observed using scanning electron microscopy. The proliferation of MC3T3-E1 cells on the as-sputtered films was suppressed, whereas proliferation on the hydrothermally treated films was comparable to that on control and titanium substrate. The suppression of cell proliferation is associated with an increase in pH of the culture medium caused by dissolution of the as-sputtered film. After a 96-h culture time, the ALP activity of the cells on the hydrothermally treated film was higher than that on the control, titanium substrate, and as-sputtered film samples. From scanning electron microscopic observations, it was found that the MC3T3-E1 cells on the hydrothermally treated films were elongated and had established more intricate filopodia networks with each other, which were also observed for MC3T3-E1 cells on the as-sputtered films after a period of 24 h., ((c) 2005 Wiley Periodicals, Inc.)

Hydroxyapatite (HA) was coated onto titanium implants using radio frequency magnetron sputtering. The HA films were crystallized in an autoclave tube using low temperature hydrothermal treatment. The average film thickness on the implant was 1.1 microm. HA-coated and pure-titanium implants were inserted into canine mandibles for up to 24 weeks. Forty-eight implants were placed in eight beagles. After 2, 4, 12 and 24 weeks, implants were retrieved and prepared for histological observation, and the HA film thickness was determined using energy-dispersive X-ray spectroscopy. Light microscopy revealed that, after two weeks, the bone response to the HA-coated implants was much better than to the pure titanium implants, and osteoblasts were observed at the bone-implant interface. After four weeks, the screw threads of the HA-coated implants were almost completely covered with bone. The HA film thickness rapidly decreased up to four weeks of implantation, then gently decreased, reaching 0.40+/-0.03 microm at the upper region of the implant after 12 weeks. That indicates that about 80% of the HA film had dissolved after 12 weeks of implantation. The rate of decrease in the HA film thickness was greater with increasing implant depth.

Three-dimensional finite element analysis was performed for thin hydroxyapatite (HA) coated and titanium dental implants to study the effects on stress/strain distribution in the mandible with application of axial and oblique loads. The implants were of screw and cylinder types. With an axial load, the maximum equivalent bone stresses in the titanium implants were 21.5 and 29.0 MPa for the cylinder and screw types respectively, and the stress and strain distributions differed. For the cylinder type, the highest stress was located at the implant base, and for the screw type, it was located at the top edge of the first thread within the cortical bone. For the HA-coated cylinder and screw implants, the maximum equivalent bone stresses were 7.1 and 7.2 MPa respectively. The stress and strain distributions were similar, and the highest stress was located on the upper side of the cortical bone around the implant neck for both implants. Of the implants examined, the screw type HA-coated implant had the most uniform stress distribution in bone.

To alleviate the effects of Ni allergy from NiTi alloy implants, hydroxyapatite (Ca10(PO4)6(OH)2; HA), alumina (Al2O3), or titanium (Ti) was coated onto NiTi alloy plates to form 1-microm thick films using radio frequency magnetron sputtering. The coatings on the plates were characterized using XRD. After the plates had been immersed in physiological saline for periods of one, four, or eight weeks, the concentration of Ni ions released in each solution was detected using a microwave induced plasma mass spectrometer. After eight weeks, the concentration of Ni ions released from the non-coated, the Ti-coated, the HA-coated, and the alumina-coated plates were 238, 19.7, 183, and 106 ppb, respectively. The bonding strength of the Ti film, the HA film, and the alumina film to the NiTi substrate were 3.8 +/- 1.2, 2.6 +/- 0.7, and 3.1 +/- 1.2 MPa, respectively. The non-coated, the HA-coated, the alumina-coated, and the Ti-coated plates were implanted into the femurs of a dog for four weeks for histological observation. In case of the non-coated plates, connective tissue more than 300 microm thick was observed, whereas for the coated plates the thickness of the connective tissue was around 100 microm.

Hydroxyapatite (HA) and other calcium phosphates were synthesized on titanium plates by a solid-gas state reaction of sputtered CaO and vaporized P(2)O(5). The calcium phosphates formed were HA, beta-tricalcium phosphate (beta-TCP; Ca(3)(PO(4))(2)), beta-calcium pyrophosphate (beta-PYR; Ca(2)P(2)O(7)), and beta-calcium metaphosphate (beta-MET; Ca(2)(PO(3))(2)). Their formation depended on the ratio of the sputtered CaO and the reacting P(2)O(5). For a mole ratio of CaO/P(2)O(5)=4 (Ca/P=2), an HA film was synthesized. The surface roughness increased by over seven times after the solid-gas state reaction from Ra = 0.16+/-0.02 microm (for the CaO film) to Ra = 1.15+/-0.25 microm (for the reacted film). The synthesized HA film-coated titanium plates and control non-coated titanium plates were implanted in the femora of two dogs for a period of two, four and 12 weeks, and observed using a soft X-ray radiograph and histological sections. New bone formation was observed without any connective tissue at four weeks around the HA film, whereas over the 12 week experimental period, there was no new bone formation around the control and connective tissue was observed over all periods, reaching a thickness of more than 200 microm at 12 weeks.

Hydroxyapatite (HA) was coated onto titanium substrates using radio frequency sputtering, and the coated HA films were crystallized in an autoclave at 110 degrees C using a low temperature hydrothermal method. The crystallite size, the Ca/P ratio, and the surface of the films were observed using XRD, EDS, and SEM, respectively. An immersion test was carried out in physiological saline solution, and the film-to-substrate adhesion strength was measured using a pull-out test. From the XRD patterns, a sputtered film subjected to the hydrothermal treatment had crystallized after 24 h, and the crystallite size increased from 38.0+/-8.7 to 81.4+/-19.1 nm. In immersion tests, an as-sputtered film completely dissolved after 1 d, whereas a sputtered film subjected to the hydrothermal treatment survived to 18.7+/-5.8% of the initial film thickness after four weeks. In pull-out tests, the adhesion strength of the sputtered film to the substrate increased from 1.9+/-0.2 to 5.3+/-1.6 MPa after the hydrothermal treatment. A sputtered film subjected to the hydrothermal treatment and a plasma-sprayed coating on titanium columns were implanted in the diaphysis of the femora of six adult dogs, and a pull-out test was carried out after two, four, and 12 weeks. The sputtered film showed higher bone bonding strength than the plasma-sprayed coating at any period.

Hydroxyapatite was coated with 1 microm thickness on titanium columns of a length of 10 mm, an outer diameter of 4.0 mm by radio frequency magnetron sputtering. The hydroxyapatite coating titanium columns were implanted in the diaphysis of femora of 3 adult dogs, and push-out test was carried out after 2, 4 and 12 weeks of implantation using a testing machine. The interface of bone/column was observed histologically after the test. At 12 weeks the push-out strengths of coating and non-coating columns were 3.5 and 1 MPa, respectively. Histological observation indicated a formation of thin connective tissue with 5-30 microm thickness at the interface of the bone/column. No inflammation was observed during the implantation periods.

Hydroxyapatite is widely utilized as a component in dental hygiene agents. The ability to adsorb and remove dental plaque adhering to tooth surfaces is recognized as an important property of hydroxyapatite particles. In this study, the adsorptive ability of hydroxyapatite was evaluated based on its adsorptive amount and adsorptive strength. The adsorptive amount was determined by measuring the weight of albumin, dextran and lipids adsorbing to hydroxyapatite. The adsorptive strength was determined by measuring the weights of albumin and dextran remaining adsorbed after rinsing. Similar procedures were performed in control experiments using calcium hydrogen phosphate dihydrate, alumina and sericite. The results showed that the weights of albumin and dextran adsorbed to hydroxyapatite were 1.4 +/- 0.13 and 1.6 +/- 0.30 times higher than that to calcium hydrogen phosphate dihydrate. The weight of lipids adsorbed to hydroxyapatite was much higher than that to alumina and sericite. The percentages of weight loss of albumin and dextran were 2.3 +/- 1.7% and 5.3 +/- 2.0% for hydroxyapatite and 27 +/- 6.8% and 19 +/- 11% for calcium hydrogen phosphate dihydrate after one rinse. It is concluded that hydroxyapatite is a better adsorbent than calcium hydrogen phosphate dihydrate, alumina and sericite with respect to adsorbing albumin, dextran and lipids.

Hydroxyapatite (HAP)-coated metal composites were made by the dipping method. The specimen substrates were Ti plates with a thickness of 2 mm. The HAP coating was carried out in HAP-sol for 1 min by the dipping method. The concentration of HAP-sol for the coating ranged from 3.28 to 9.99 wt%. Excellent coating was observed on Ti substrate dipped once in 9.99 wt% sol. A surface pretreated with a sandblasting provided a much better coating than a smooth surface. As the concentration of sol increased, the weight change and the coating thickness increased. Above 7 wt% sol, they increased sharply.

Hydroxyapatite-sol was prepared by dispersing hydroxyapatite microcrystals into saline. The hydroxyapatite microcrystals were synthesized by neutralization reaction of calcium hydroxide suspension and phosphoric acid solution. Sizes of the hydroxyapatite microcrystals were less than 0.1 microns, and the mean value was 0.05 microm. The 0.2 ml hydroxyapatite-sol with a concentration of 14.8 mg/ml was injected into medullary cavities of rat femurs. Both sintered hydroxyapatite powder suspension and saline as comparative materials were injected into the medullary cavities in the same way. Reaction of the hydroxyapatite-sol in the bone medullary cavities was investigated histologically using light and transmission electron microscopes. After 3 days, new bone formation was observed by injection of hydroxyapatite-sol, while no bone formation was observed by injection of sintered hydroxyapatite powder and saline. Osteoblasts were observed endocytosing the hydroxyapatite-sol in the medullary cavities of the rats. Macrophages and undifferentiated osteoblasts were found around the hydroxyapatite-sol aggregation by transmission electron microscope. After 5 days, amounts of new bone increased and matured, forming trabeculae. Many osteoblasts were observed in a line along the surface of the bone. On the other hand, 5 days after injection of sintered hydroxyapatite powder and saline to bone formation was observed while at 10 days after injection, some immature new bone formation started to be observed. New bone increased and matured at 15 days postoperatively. From these results, it was concluded that hydroxyapatite-sol only quickly promotes the formation of new bone in bone marrow and can be used as injection liquid of new biomaterials for bone formation.

The application of hydroxyapatite-sol as a drug carrier is being developed. Hydroxyapatite-sol which is a suspension consisting of hydroxyapatite nano-crystals, was synthesized using an ultrasonic homogenizer. The size of the crystals was 40 x 15 x 10 mm3 on average and their specific surface area was 100 m2/g. An amount of a glycoside antibiotics adsorbed onto hydroxyapatite nano-crystals was measured. The drug adsorbed 0.2 mg per 1 mg of hydroxyapatite. The affect of the drug adsorbed onto the hydroxyapatite was investigated using cancer cells. The drug, adsorbed onto the hydroxyapatite nano-crystals, inhibited cancer cell growth.