Although most strains of escherichia coli (E. coli) are harmless, some serotypes can cause serious food poisoning in humans. It is very difficult to eliminate E. coli from our lives. Here we show that E. coli can be eliminated by hydroxyapatite (HAp). Because HAp has a positive charge, the material and E. coli are attracted through electrostatic interactions. Additionally, because the surface of HAp is porous, it enters the pores of the HAp surface removing them from the environment. The amount of adsorption was observed to increase over time, and the zeta potential value of the material tended to be similar to that of E. coli. This phenomenon is thought to have zeta potential similar to that of E. coli as it is adsorbed onto the HAp surface over time. E. coli stained with crystal violet was spread on a glass slide and HAp porous sol powder was dropped to remove the E. coli. We expect that this analysis will open a new direction for antibacterial materials.
The need for the development of sustainable, efficient, and green radioactive waste disposal methods is emerging with the saturation of spent nuclear waste storage facilities in the Republic of Korea. Conventional radioactive waste management methods like using cement or glass have drawbacks such as high porosity, less chemical stability, high energy consumption, carbon dioxide production, and the generation of secondary wastes, etc. To address this gigantic issue of the planet, we have designed a study to explore the potential of alternative materials having easy processability, low carbon emissions and more chemical stability such as ceramic (hydroxyapatite, HAP) and alkali-activated materials (geopolymers, GP) to capture the simulated radioactive cobalt ions from the contaminated water and directly solidify them at low temperatures. Physical and mechanical properties of HAP alone and 15wt% GP incorporated HAP (HAP-GP- 15) composite were studied and compared. The surface of both materials was fully sorbed with an excess amount of Co(II) ions in the aqueous system. Co(II) sorbed powders were separated from aqueous media using a centrifuge machine operating at 5,000 RPM for 10 minutes and dried at 100°C for 8 hours. The dried powders were then placed in stainless steel molds, and shaped into cylindrical pellets using a uniaxial press at a pressure of 1 metric ton for 1 minute. The pellets were sintered at 1,100°C for 2 hours at a heating rate of 10°C/min. Following this, the water absorption, density, porosity, and compressive strength of the polished pellets were measured using standard methods. Results showed that HAP has a greater potential for decontamination and solidification of Co(II) due to its higher density (2.65 g/cm3 > 1.90 g/cm3), less open porosity (16.2±2.9% < 42.4 ±0.9%) and high compressive strength (82.1±10.2 MPa > 6.9±0.8 MPa) values at 1,100°C compared to that of HAP-GP-15. Nevertheless, further study with different constituent ratio of HAP and GP at various temperatures is required to fully optimize the HAP-GP matrix for waste solidifications.
3Y-TZP (3 mol% yttria-stabilized tetragonal zirconia polycrystals) ceramics have excellent mechanical properties including high fracture toughness, good abrasion resistance as well as chemical and biological stability. As a result, they are widely used in mechanical and medical components such as bearings, grinding balls, and hip implants. In addition, they provide excellent light transmittance, biocompatibility, and can match tooth color when used as a dental implant. Recently, given the materials’ resemblance to human teeth, these ceramics have emerged as an alternative to titanium implants. Since the introduction of CAD/CAM in the manufacture of ceramic implants, they’ve been increasingly used for prosthetic restoration where aesthetics and strength are required. In this study, to improve the surface roughness of zirconia implants, we modified the 3YTZP surface with a biocomposite of hydroxyapatite and forsterite using room temperature spray coating methods, and investigated the mixed effect of the two powders on the evolution of surface microstructure, i.e., coating thickness and roughness, and biological interaction during the in vitro test in SBF solution. We compared improvement in bioactivity by observing dissolution and re-precipitation on the specimen surface. From the results of in vitro testing in SBF solution, we confirmed improvement in the bioactivity of the 3Y-TZP substrate after surface modification with a biocomposite of hydroxyapatite and forsterite. Surface dissolution of the coating layer and the precipitation of new hydroxyapatite particles was observed on the modified surface, indicating the improvement in bioactivity of the zirconia substrate.
In this study, Ti-Mo-EB composites are prepared by ball milling and spark plasma sintering (SPS) to obtain a low elastic modulus and high strength and to evaluate the microstructure and mechanical properties as a function of the process conditions. As the milling time and sintering temperature increased, Mo, as a β-Ti stabilizing element, diffused, and the microstructure of β-Ti increased. In addition, the size of the observed phase was small, so the modulus and hardness of α-Ti and β-Ti were measured using nanoindentation equipment. In both phases, as the milling time and sintering temperature increased, the modulus of elasticity decreased, and the hardness increased. After 12 h of milling, the specimen sintered at 1000oC showed the lowest values of modulus of elasticity of 117.52 and 101.46 GPa for α-Ti and β-Ti, respectively, confirming that the values are lower compared to the that in previously reported studies.
A powder mixture of 70 wt% Al2O3 and 30 wt% hydroxyapatite (HA) is sintered at 1300 ℃ or 1350 ℃ for 2 h at normal pressure. An MgF2-added composition to make HA into fluorapatite (FA) is also prepared for comparison. The samples without MgF2 show α & β-tricalcium phosphates (TCPs) and Al2O3 phases with no HA at either of the sintering temperatures. In the case of 1,350 ℃, a CaAl4O7 phase is also found. Densification values are 69 and 78 %, and strengths are 156 and 104MPa for 1,300 and 1,350 ℃, respectively. Because the decomposition of HA produces a H2O vapor, fewer large pores of 5-6 μm form at 1,300 ℃. The MgF2-added samples show FA and Al2O3 phases with no TCP. Densification values are 79 and 87%, and strengths are 104 and 143 MPa for 1,300 and 1,350 ℃, respectively. No large pores are observed, and the grain size of FA (1-2 μm) is bigger than that of TCP (0.7 μm ≥) in the samples without MgF2. The resulting TCP/Al2O3 and FA/Al2O3 composites fabricated in situ exhibit strengths 6-10 times higher than monolithic TCP and HA.
Plasma-sprayed HA coatings on metallic implants are widely used for clinical applications. However, typical lamellar structure along with plasma-sprayed coatings usually leads to weak inter-splat adhesion and impair their mechanical properties. In this research, graphene nanosheet (GNS) reinforced HA coatings were fabricated using plasma spray; these GNSs retained their original structure and distributed homogeneously in the as-sprayed coatings. On the basis of instrumented microindentation tests with and without multiple partial unloading, as compared with the monolithic HA coating, the inter-splat friction force increased by ~ 8.7% for the 1.0 wt% GNS/HA coating, and it slightly decreased to ~ 6.5% for the 2.0 wt% GNS/ HA coating due to GNS agglomeration. Meanwhile, the added GNSs contributed greatly to the indentation yield strength of the HA coatings. These results illustrated that these embedded GNSs at splat boundaries are potential in splat-boundary strengthening and resisting splat sliding.
수산화인회석은 생체적합성이 뛰어나기 때문에 생체재료로 사용되고 있다. 본 연구에서는 온도, 농도, pH를 조절하여 인산수소칼슘 중간체의 가수분해반응을 통해 c면이 배향된 수산화인회석을 합성하였다. 염기조건에서 전구체의 농도가 낮을 경우 막대 형태의 수산화인회석 결정이 모여 불규칙한 형태의 입자를 만들었고 농도가 높을 경우 수산화인회석결정의 c면이 노출된 판 형태의 입자를 만들었으며 이에 따라 입자의 제타전위 차가 3 mV가 되었다. 생성물의 물리화학적 특성은 XRD, SEM, FT-IR, 제타전위측정기를 통해 평가하였다.
One of the major sources causing eutrophication and algal blooms of lakes or streams is phosphorus which comes from point and nonpoint pollution sources. HAP (hydroxyapatite) crystallization using granular alkaline materials can achieve the decrease of phosphorus load from wastewater treatment plants and nonpoint pollution control facilities. In order to induce HAP crystal formation, continuous supply of calcium and hydroxyl ions is required. In this research, considering HAP crystallization, several types of lime-based granular alkaline materials were prepared, and the elution characteristics of calcium and hydroxyl ions of each were analyzed. Also, column tests were performed to verify phosphorus removal efficiencies of granular alkaline materials. Material_1 (gypsum+cement mixed material) achieved the highest pH values in the column tests consistently, also, Material_2 (gypsum+slag mixed material) and Material_3 (calcined limestone material) achieved over pH 9.0 for 240 hours (10 days) and proved the efficiencies of long-term ion supplier for HAP crystallization. In the column tests using Material_3, considerable pH increase and phosphorus removal were carried out according to each linear velocity and filtration depth. T-P removal efficiencies were 87.0, 84.0, 68.0% and those of PO4-P 100.0, 97.0, 80.0% for linear velocity of 1.0, 2.5, 5.0 m/hr respectively. Based on the column test results, the applicability of phosphorus removal processes for small-scale wastewater treatment plants and nonpoint pollution control facilities was found out.
Electrochemical synthesis was employed to prepare a novel hydroxyapatite/graphene (HAP/ Gr) composite powder suitable for medical applications as a hard tissue implant (scaffold). The synthesis was performed in a homogeneous dispersion containing Na2H2EDTA·2H2O, NaH2PO4 and CaCl2 with a Ca/EDTA/PO4 3− concentration ratio of 0.25/0.25/0.15M, along with 0.01 wt% added graphene nanosheets, at a current density of 137 mA cm−2 and pH value of 9.0. The field emission scanning electron microscopy and transmission electron microscopy observations of the composite HAP/Gr powder indicated that nanosized hydroxyapatite particles were uniformly placed in the graphene overlay. Raman spectroscopy, Fourier transform infrared spectroscopy and X-ray diffraction confirmed graphene incorporation in the HAP/Gr powder. The electrochemically prepared HAP/Gr composite powder exhibited slight antibacterial effect against the growth of the bacterial strain Staphylococcus aureus.
Hydroxyapatite (HA), which is an important calcium phosphate mineral, has been applied in orthopedics, dentistry, and many other fields depending upon its morphology. HA can be synthesized with different morphologies through controlling the synthesis method and several parameters. Here, we synthesize various morphologies of HA using two simple methods: hydrothermal combustion and solution combustion. The phase purity of the synthesized HA is confirmed using X-ray diffractometry. It demonstrates that pure phased hydroxyapatite can be synthesized using both methods. The morphology of the synthesized powder is examined using scanning electron microscopy. The effects of pH and temperature on the final powder are also investigated. At 140 oC, using the hydrothermal method, nano-micro HA rods with a hexagonal crystal structure can be synthesized, whereas using solution combustion method at 600 oC, a dense cubic morphology can be synthesized, which exhibits monoclinic crystal structures.
To increase the mechanical property of zirconia, we have investigated the phase change and the resulting hardness of zirconia ceramics by hydroxyapatite (HA) powder bed sintering. It was observed using X-ray diffraction that the cubic zirconia phase, which has a higher hardness value than that of the tetragonal phase, was obtained at the surface of 3 mol% Y2O3 doped tetragonal zirconia polycrystal (3Y-TZP) ceramics during the sintering process; in our experimental conditions, the phase change at the surface increased as the sintering time increased. We believe that the observed crystalline phase change originated from the decomposition of HA and the diffusion of CaO, as follows. CaO, which was derived from the decomposition of HA at high temperature (1400˚C), diffused into the surface of 3Y-TZP and acted as a stabilizer. As a result, the Vickers hardness value of the treated specimens was higher than that of the non-treated specimen due to the formation of the cubic phase on the surface of 3Y-TZP.
Nonthermal atmospheric pressure plasma has attracted great interest for biomedical applications. The plasma consists of charged particles, radicals, and a strong electric field as the fourth state of matter. This study evaluated the change in the surface roughness after tooth bleaching by plasma in combination with a low concentration (15%) of carbamide peroxide, specifically whether the application of plasma produced detriments, such as demineralization and structural change, with the goal of efficient and safe tooth bleaching. After being combined with plasma and 15% carbamide peroxide, the hydroxyapatite surface was significantly smoother with a low roughness average value. Tooth bleaching with 15% carbamide peroxide alone produced an irregular surface and increased the surface roughness with high roughness average value. Tooth bleaching with plasma resulted in no significant variations in hydroxyapatite in terms of change in surface roughness and surface topography. The application of tooth bleaching with plasma is not deleterious to dental hard tissue, implicating it as a safe tooth bleaching technique.
Spherical Ti-6Al-4V powders in the size range of 250 and 300 µm were uniformly doped with nano-sized hydroxyapatite (HAp) powders by Spex milling process. A single pulse of 0.75-2.0 kJ/0.7 g of the Ti-6Al-4V powders doped with HAp from 300 mF capacitor was applied to produce fully porous and porous-surfaced Ti-6Al-4V implant compact by electro-discharge-sintering (EDS). The solid core was automatically formed in the center of the compact after discharge and porous layer consisted of particles connected in three dimensions by necks. The solid core increased with an increase in input energy. The compressive yield strength was in a range of 41 to 215 MPa and significantly depended on input energy. X-ray photoelectron spectroscopy and energy dispersive x-ray spectrometer were used to investigate the surface characteristics of the Ti-6Al-4V compact. Ti and O were the main constituents, with smaller amount of Ca and P. It was thus concluded that the porous-surfaced Ti-6Al-4V implant compacts doped with HAp can be efficiently produced by manipulating the milling and electro-discharge-sintering processes.
The objective of this study was to compare peri-implant bone formation among uncoated (UC), hydroxyapatite (HA), collagen plus hydroxyapatite (CH), and silk plus hydroxyapatite (SH) implant groups. Surface coating was applied using the aerosol deposition method. The morphology of MG63 cells on the implant surfaces were examined by scanning electron microscopy (SEM) after 8 h cultures on the each of implant groups. After 48 h cultures, MTT assay was performed to compare cell viabilities of each group. Subsequently, a total of 20 implants from each group were installed in the tibia of the rabbits. The animals were sacrificed at 6 weeks after the implant installation. The peri-implant bone formation was evaluated from the histological sections. In the SEM images, SH coating implant showed better attachment of MG63 cells to the implant surface than the other groups. It also showed adequate cell viabilities and peri-implant bone formations compared with other implant groups. From these in vitro and vivo experiments, SH coating can be a possible candidate for the surface treatment of dental implant.
This study was supported by a grant from the Next-Generation BioGreen21 Program (Center for Nutraceutical & Pharmaceutical Materials no. PJ009013)
We define hydrogel as a polymer network containing a large amount of water or biological fluid in a 3-D structure. Because of the physical or chemical chains present in a hydrogel, it is stable in aqueous environment. Therefore, it has been used in diverse medical fields. In addition, by controlling the gelation degree of polymer solution (the state prior to hydrogel) hydrogels can be easily applied to damaged tissue area. This unique structure and properties of hydrogel shares a similarity with ECM (Extracellular matrix) in that it has a potential to be applied in tissue engineering field. Especially, the injectable property and ECM like structure can be applied to bone regeneration. Out of several polymers can be form hydrogels, silk fibroin (SF) has an excellent biocompatibility, biodegradability and it can be used to create bone regeneration scaffold in the form of hydrogel.
In this study, we fabricated a SF hydrogel containing hydroxyapatite nanoparticle (HAp). To improve the dispersibility of HAp in the SF aqueous solution, we chemically modified the surface of HAp particles using hyaluronic acid (HA) – dopamine (DA) conjugate. Since SF aqueous solution has a long term gelation time, we utilized ultra-sonication method to induce a rapid gelation. Stability of HAp in SF aqueous solution was measured by ELS and TGA. Finally, FT-IR and WAXD were used to evaluate the changes of secondary structure of silk hydrogel according to concentrations of hydroxyapatite nanoparticle concentration.
In this study, hydroxyapatite (HAp) was incorporated into toothpaste and its effect on the remineralization and restoration of dental enamel was evaluated. Different sets of toothpaste were incorporated with HAp levels of 0%, 5%, 10 %, and 15 %. The filler particles of the resulting toothpaste samples were observed via SEM and XRD and compared with compositions of several commercially available toothpastes, showing that the HAp was successfully incorporated into the toothpaste samples. Different sets of human enamel were inflicted with lesions and then treated with the different fabricated toothpaste samples for five minutes three times a day for seven days. During the treatment, the teeth were subjected to demineralization and remineralization cycles to simulate the effect of natural saliva. The surface of the enamel samples were observed using SEM before and after one week of treatment, showing the formation of HAp layers on the surfaces of the enamel samples. The effect of the toothpaste on the lesions was observed using an inverted light microscope and the lesion depth was found to decrease as the concentration of HAp in the toothpaste used increased. HAp was successfully incorporated in the toothpaste and its presence was found to lessen lesion depths and improve tooth remineralization.
Morphological control on hydroxyapatite crystals has attractive prospects in research to clarify the effects of crystal planes on biological performance. Hydrothermal processing is known as a typical type of processing for fabricating well-grown crystals with unique morphology. The purpose of the present study is to examine the feasibility of well-crystallized crystals with oriented structures through hydrothermal treatment of calcite. A single crystal of calcite was applied to hydrothermal treatment in a phosphate solution at 160˚C. Rod-shaped hydroxyapatite crystals with micrometer-size were formed on the 100 face of calcite after treatment, while nanometer-sized hydroxyapatite crystals were formed on the (111). The hydroxyapatite crystals formed on each plane were not morphologically changed with increasing treatment periods. An oriented structure of rod-shaped hydroxyapatite was constructed after hydrothermal treatment of 100 planes on the calcite single, while such orientation was not observed on the (111) plane after the treatment. The layer of hydroxyapatite formed on the 100 plane was thicker than that of the (111) plane. The 100 plane of calcite shows a higher reactivity than that of the (111) plane, which results in rapid crystal growth of hydroxyapatite. The difference in the morphology of the formed hydroxyapatite was governed by the reactivity of each crystal plane exposed to the surrounding solution.
Hydroxyapatite (HA) is well known as a biocompatible and bioactive material. HA has been practically applied as bone graft materials in a range of medical and dental fields. In this study, two types of dense hydroxyapatite ceramics were prepared from natural bones and synthetic materials. The biocompatibility of HA ceramics for supporting osteoblast cell growth and cytotoxicity using an in vitro MG-63 cell line model were respectively evaluated. Artificial hydroxyapatite shows relative density of 93% with 1-2 μm after sintering, but a hydroxyapatite compact derived from bovine bone has low sintered density of 85% with a small content of MgO. Irrespective of the starting raw materials, both types of sintered hydroxyapatite displayed similar biocompatibility in the tests. FE-SEM observations showed that most MG-63 cells had a stellar shape and formed an intercellular matrix containing fibers on sintered HA. The cells were well attached and grown over the HA surface, indicating that there was no toxicity.